CN109437208A - The preparation facilities of disilane - Google Patents
The preparation facilities of disilane Download PDFInfo
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- CN109437208A CN109437208A CN201811594055.4A CN201811594055A CN109437208A CN 109437208 A CN109437208 A CN 109437208A CN 201811594055 A CN201811594055 A CN 201811594055A CN 109437208 A CN109437208 A CN 109437208A
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- C01B33/00—Silicon; Compounds thereof
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Abstract
The present invention provides a kind of preparation facilities of disilane.The disilane preparation facilities includes: filter element, rectification cell and reduction unit, and filter element is provided with polysilicon raffinate entrance and filtrate (liquid；Rectification cell is provided with filtrate inlet and the outlet of chloro disilane, and filtrate inlet is connected with filtrate inlet through filtrate transfer pipeline；Reduction unit is provided with feed opening, and feed opening is exported with chloro disilane to be connected through chloro disilane transfer pipeline, and feed opening is also used for that reducing agent is added.The preparation that chloro disilane can be saved using polysilicon raffinate as raw material, substantially reduces preparation cost.The solid impurity in polysilicon raffinate is removed by filter element, obtains filtrate；Then the organic impurities component in filtrate is removed by distillation unit, obtains chloro disilane；So that chloro disilane and reducing agent is carried out reduction reaction, obtains disilane.Preparing disilane using above-mentioned disilane preparation facilities has many advantages, such as at low cost, and process flow is short and disilane is with high purity.
Description
Technical field
The present invention relates to polysilicon preparation fields, in particular to a kind of preparation facilities of disilane.
Background technique
Disilane is mainly used for the side such as solar battery, photosensitive rotating cylinder, amorphous silicon film, epitaxial growth and chemical vapor deposition
Face.When sedimentary is silicon oxide or silicon nitride, compared with silane, disilane has deposition velocity faster as sedimentary origin, deposition
Temperature is lower, prevents from generating ball bumps in unformed silicon, and improve be deposited into homogeneity the advantages that.Disilane mainly uses
In 20 nanometers or less high-end chip manufacturing fields.In manufacture of solar cells, compared to silane, with disilane in amorphous silicon wafer
On deposition velocity it is faster, and temperature can reduce by 200~300 DEG C.In ion implantation process, after making ion source with disilane
Easy build-up of luminance, line are strong, and effect, which is significantly better than, makees ion source with other gases.In semiconductor processing, disilane can be used for outer
Prolong and diffusion technique, can be used for the photosensitive drums of solar battery and electrophotography.
The preparation of disilane at present mainly has chloro disilane reduction method and magnesium silicide-two kinds of sides of ammonium chloride reaction synthesis
Method.
Chloro disilane reduction method is using complex metal hydride (such as lithium aluminium hydride reduction or sodium aluminum hydride) deoxygenization chlorination
Disilane alkane prepares disilane.The disadvantage is that chloro disilane needs to carry out separately synthesized, but synthesize that difficulty is big and low yield.
Magnesium silicide is that magnesium silicide carries out reacting generation disilane with ammonium chloride with ammonium chloride reaction method.The disadvantage is that party's legal system
The product obtained is mainly silane, and disilane accounting 3% or so, is recycled as by-product.Which greatly limits adopt
With the feasibility of this method large scale preparation disilane.In addition, solid magnesium chloride hexammoniate can be generated in above-mentioned reaction process, in view of
The higher risk of disilane, the technological difficulties of this method are mainly: 1, how disilane and silane being separated；2, how
The separating-purifying disilane from the waste residue of silane reaction kettle.
Summary of the invention
The main purpose of the present invention is to provide a kind of preparation facilities of disilane, to solve to prepare second using existing method
There is a problem of that the purity of disilane is low and at high cost when silane.
To achieve the goals above, a kind of disilane preparation facilities is provided according to the present invention, the disilane preparation facilities
It include: filter element, rectification cell and reduction unit, filter element is provided with polysilicon raffinate entrance and filtrate (liquid；Rectifying
Unit is provided with filtrate inlet and the outlet of chloro disilane, and filtrate inlet is connected with filtrate inlet through filtrate transfer pipeline；Also
Former unit is provided with feed opening, and feed opening is exported with chloro disilane to be connected through chloro disilane transfer pipeline, feed opening
For reducing agent to be added.
Further, rectification cell includes: the first rectifier unit and the second rectifier unit, and the first rectifier unit is provided with filter
Liquid entrance and remove tiron entrance and the first overhead outlet；And second rectifier unit be provided with the first overhead product entrance and
The outlet of chloro disilane, the first overhead outlet are connected with the first overhead product entrance.
Further, rectification cell further includes except tiron feeding mechanism, except tiron feeding mechanism is used for the first essence
Distillation unit, which provides, removes tiron.
Further, filter element includes at least one filter device, and the quantity of filter device is denoted as N, works as N=1
When, filter device is provided with polysilicon raffinate entrance and filtrate (liquid, and as N > 1, N number of filter device is sequentially connected to, and presses object
The dynamic sequence of stream is provided with polysilicon raffinate entrance positioned at the 1st filter device, and the filter device of n-th is provided with filter
Liquid outlet.
Further, filter device is provided with filter hole, and the diameter in hole is 0.5~1 μm.
Further, reduction unit includes: reducing agent feeding mechanism, reduction apparatus and heating device, reducing agent supply dress
It installs and is equipped with reducing agent supply opening, reduction apparatus is provided with feed opening, and feed opening is connected with reducing agent supply opening, heating device
For controlling the reaction temperature in reduction apparatus.
Further, reduction unit further include: organic solvent feeding mechanism, protection gas feeding mechanism and catalyst supply dress
It sets.Organic solvent feeding mechanism is provided with organic solvent entrance, and organic solvent entrance is connected with feed opening；Protect gas supply dress
It installs and is equipped with protection gas supply opening, protection gas supply opening is connected with feed opening；Catalyst feeding mechanism is provided with catalyst confession
Mouth is answered to be connected with feed opening.
Further, reduction apparatus is micro passage reaction.
Further, reduction apparatus is additionally provided with the outlet of reduzate system, and disilane preparation facilities further includes that purification is single
Member, purifier units are provided with reduzate system entrance, and reduzate system entrance is connected with the outlet of reduzate system, use
It is purified in reduzate system.
Further, purifier units include: third rectifier unit and the 4th rectifier unit, and third rectifier unit is provided with also
Originate in objects system entrance, third distillation column top product exit；4th rectifier unit be provided with third distillation column top product inlet and
4th rectifying bottoms outlet, third distillation column top product inlet are connected with third distillation column top product exit.
Further, purifier units include the 5th rectifier unit, and the 5th rectifier unit is provided with the 4th rectifying tower bottom product
Entrance and the 5th rectifying bottoms outlet, the 4th rectifying tower bottom product entrance and the 4th rectifying bottoms outlet.
Further, purifier units further include the first adsorbent equipment, and the first adsorbent equipment is internally provided with active carbon layer,
And first adsorbent equipment be provided with the 5th rectifying tower bottom product entrance, the 5th rectifying tower bottom product entrance and the 5th rectifying column bottom
Product exit is connected, for removing the solid impurity in the 5th rectifying tower bottom product.
Further, activated carbon adsorption device is additionally provided with the outlet of the first purified product, and purifier units further include the second suction
Adsorption device, the inside of the second adsorbent equipment are mounted with molecular sieve, and the second adsorbent equipment is provided with the first purified product entrance, and first
Purified product entrance is connected with the outlet of the first purified product, for further removing the solid impurity in the first purified product.
It applies the technical scheme of the present invention, includes chloro disilane in polysilicon raffinate, using above-mentioned disilane device system
When standby disilane, it is to prepare raw material to save the preparation step of chloro disilane with polysilicon raffinate, substantially reduces disilane
Preparation cost.By setting filter element by polysilicon raffinate solid impurity (such as particulate material, metal-containing polymer,
Impurity containing amorphous silicon and metal) removal, obtain filtrate；Then the organic impurities in filtrate is removed by setting distillation unit
Component obtains chloro disilane；Finally in reduction unit, so that chloro disilane and reducing agent is carried out reduction reaction, obtain institute
The product disilane needed.Preparing disilane using above-mentioned disilane preparation facilities has at low cost, and process flow is short and disilane
The advantages that with high purity.
Detailed description of the invention
The accompanying drawings constituting a part of this application is used to provide further understanding of the present invention, and of the invention shows
Examples and descriptions thereof are used to explain the present invention for meaning property, does not constitute improper limitations of the present invention.In the accompanying drawings:
Fig. 1 shows the structural representation of the disilane preparation facilities provided according to a preferred embodiment of the present invention
Figure；And
Fig. 2 shows the process flows of the disilane preparation method provided according to a preferred embodiment of the present invention
Figure.
Wherein, the above drawings include the following reference numerals:
10, filter element；
20, rectification cell；21, the first rectifier unit；22, the second rectifier unit；23, tiron feeding mechanism is removed；
30, reduction unit；31, reducing agent feeding mechanism；32, reduction apparatus；33, organic solvent feeding mechanism；34, it protects
Gas feeding mechanism；35, catalyst feeding mechanism；
40, purifier units；41, third rectifier unit；42, the 4th rectifier unit；43, the 5th rectifier unit；44, first inhales
Adsorption device；45, the second adsorbent equipment；50, impurity collection device.
Specific embodiment
It should be noted that in the absence of conflict, the features in the embodiments and the embodiments of the present application can phase
Mutually combination.Below in conjunction with embodiment, the present invention will be described in detail.
As described in background technique, there are the purity of disilane is low and cost when preparing disilane using existing method
High problem.In order to solve the above-mentioned technical problem, this application provides a kind of disilane preparation facilities, as shown in Figure 1, the second silicon
Alkane preparation facilities includes: filter element 10, rectification cell 20 and reduction unit 30, and filter element 10 is provided with polysilicon raffinate and enters
Mouth and filtrate (liquid；Rectification cell 20 is provided with filtrate inlet and the outlet of chloro disilane, and filtrate inlet and filtrate inlet are through filtering
Liquid transfer pipeline is connected；Reduction unit 30 is provided with feed opening, and feed opening exports defeated through chloro disilane with chloro disilane
Pipeline is sent to be connected, feed opening is also used for that reducing agent is added.
It include chloro disilane in polysilicon raffinate, it is residual with polysilicon when preparing disilane using above-mentioned disilane device
Liquid is to prepare raw material to save the preparation step of chloro disilane, substantially reduces the preparation cost of disilane.By being arranged
Unit 10 is filtered by such as particulate material, metal-containing polymer, miscellaneous containing amorphous silicon and metal of the solid impurity in polysilicon raffinate
Matter removal, moral Austria filtrate；Then the organic impurities component in filtrate is removed by setting distillation unit, obtains chloro disilane；
Finally in reduction unit 30, so that chloro disilane and reducing agent is carried out reduction reaction, obtain required product disilane.Using
Above-mentioned disilane preparation facilities, which prepares disilane, to be had many advantages, such as at low cost, and process flow is short and disilane is with high purity.
In improved Siemens polysilicon production process, a small amount of chloro second silicon can be generated in reduction process and hydrogenation process
Alkane, chloro disilane are a silicon hexachloride, two silicon hexachlorides, trichloroethyl silane, four silicon hexachlorides, five silicon hexachlorides and hexachloroethanc
The mixture of silane, above-mentioned chloro disilane is enriched in polysilicon raffinate after concentration.Thus preferably, make in the application
The polysilicon raffinate that polysilicon raffinate is obtained by improved Siemens polysilicon production process.
In a kind of preferred embodiment, it may include a filter device in above-mentioned filter element 10, be also possible to more
The filter device of platform series connection or more parallel runnings.In Partial filtration turnaround of unit, come into operation parallel filtering device, it is ensured that on
State disilane preparation facilities continuous operation.The quantity of filter device is denoted as N, as N=1, filter device is provided with polysilicon
Raffinate entrance and filtrate (liquid, as N > 1, and when N number of filter device is sequentially connected to, by Flow of Goods and Materials sequence positioned at the 1st
Filter device is provided with polysilicon raffinate entrance, and n-th filter device is provided with filtrate (liquid, is positioned at N number of filter device
When paired running, the connection type of filter device uses connection type commonly used in the art.
Above-mentioned filter device is provided with filter hole, in order to further decrease the content of solid impurity in filtrate, it is preferable that mistake
The diameter of filter opening is 0.5~1 μm.Filtering accuracy control can be removed farthest within the above range containing amorphous silicon and
The impurity of metal, filtering accuracy is too small, and filter is easy blocking to frequently overhaul, and the excessive then removal rate of filtering accuracy reduces.
Preferably, above-mentioned filter device is precise filtering device, and precise filtering device includes shell and is arranged in shell
The floral disc and filter core in portion, filter core are mounted on floral disc.It is highly preferred that above-mentioned filter core is more, can be determined according to filtration treatment amount
The particular number of filter core.It is highly preferred that filter core is metal filtering core, ceramic element or polytetrafluoroethylene (PTFE) filter core.
Disilane is prepared using above-mentioned preparation facilities and advantageously reduces preparation cost, while improving the purity of disilane.?
In a kind of preferred embodiment, as shown in Figure 1, rectification cell 20 includes the first rectifier unit 21 and the second rectifier unit 22, the
One rectifier unit 21 is provided with filtrate inlet and except tiron entrance and the first overhead outlet；And second rectifier unit 22 set
It is equipped with the first overhead product entrance and the outlet of chloro disilane, the first overhead outlet is connected with the first overhead product entrance
It is logical.
In polysilicon raffinate other than containing solid impurity, also contains some organic impurities, pass through 20 energy of rectification cell
Above-mentioned organic impurities is enough removed, and the composition of above-mentioned organic impurities is complex.When carrying out the first distillation process, to the first essence
It is added in distillation unit 21 and removes tiron, the titaniferous impurity in filtrate can be made with except complex reaction occurs for tiron, be changed into height
The substance of boiling point.This is conducive to improve in the first distillation process, the separation rate of chlorosilane and titaniferous impurity, and then is conducive to mention
The purity of high chlorosilane.It, can be by object low-boiling in filtrate by second of distillation process in the second rectification cell 20
Matter removal.
In order to improve the degree of automation of disilane preparation facilities, it is preferable that as shown in Figure 1, above-mentioned rectification cell 20 is also
Including removing tiron feeding mechanism 23, tiron is removed except tiron feeding mechanism 23 is used to provide to the first rectifier unit 21.
In reduction unit 30, chloro disilane and reducing agent occur reduction reaction and disilane are made.As long as can be realized
Above-mentioned function is specifically limited without the structure to reduction unit 30.
In a kind of preferred embodiment, as shown in Figure 1, reduction unit 30 include: reducing agent feeding mechanism 31, it is also original-pack
32 and heating device are set, reducing agent feeding mechanism 31 is provided with reducing agent supply opening；Reduction apparatus 32 is provided with feed opening, charging
Mouth is connected with reducing agent supply opening；Heating device is used to control the reaction temperature in reduction apparatus 32.In reduction unit 30
Heating device is set and is conducive to improve the reduction efficiency of chloro disilane in reduction process, and then improves the yield of disilane.
In a kind of preferred embodiment, as shown in Figure 1, reduction unit 30 further include: organic solvent feeding mechanism 33 is protected
Shield gas feeding mechanism 34 and catalyst feeding mechanism 35, organic solvent feeding mechanism 33 are provided with organic solvent entrance, You Jirong
Agent entrance is connected with feed opening；Protection gas feeding mechanism 34 is provided with protection gas supply opening, protects gas supply opening and feed opening
It is connected；Catalyst feeding mechanism 35 is provided with catalyst supply opening and is connected with feed opening.Organic solvent feeding mechanism is set
33, gas feeding mechanism 34 and catalyst feeding mechanism 35 are protected, and makes above three feedstock supply unit and protection gas supply opening
It is connected, this carries out reduction reaction under the action of organic solvent, protective gas and catalyst.It is advantageous that organic solvent is added
In the compatibility for improving reaction raw materials.Carry out advantageously reducing the several of reducing agent and air reaction under the atmosphere of protective gas
Rate improves the utilization rate of reducing agent.The reaction rate that catalyst is conducive to improve reduction reaction process is added.
Above-mentioned reduction apparatus 32 can select reaction unit commonly used in the art.In a kind of preferred embodiment, reduction
Device 32 is micro passage reaction.Micro passage reaction can continuous feeding and discharging, thus using its as reduction apparatus 32 favorably
In the yield of improving production efficiency and disilane, while the liquid holdup of the reactor is small, this is conducive to the safety of lifting device.
In order to further increase the yield of disilane, it is preferable that the diameter of the inner passage of micro passage reaction is 0.5~10 μm.It will
The diameter of the reaction channel of micro passage reaction limits the mass tranfer coefficient for being conducive to improve reaction within the above range, and then advantageous
In the yield for improving disilane.The material of above-mentioned micro passage reaction can use material commonly used in the art, such as metal, glass
Glass, silicon carbide etc..
Most of field just can satisfy to disilane using the purity of disilane made from above-mentioned disilane preparation facilities
Requirement.Semiconductor field is higher to the purity requirement of disilane, thus in order to further increase the purity of disilane, in one kind
In preferred embodiment, as shown in Figure 1, reduction apparatus 32 is additionally provided with the outlet of reduzate system, disilane preparation facilities is also
Including purifier units 40, purifier units 40 are provided with reduzate system entrance, reduzate system entrance and reduzate body
System outlet is connected, for purifying to reduzate system.
Those skilled in the art can improve the purity of disilane using conventional purifying plant.In a kind of preferred implementation
In example, as shown in Figure 1, above-mentioned purifier units 40 include: third rectifier unit 41 and the 4th rectifier unit 42, third rectifier unit
41 are provided with reduzate system entrance, third distillation column top product exit；4th rectifier unit 42 is provided with third distillation column
Push up product inlet and the 4th rectifying bottoms outlet, third distillation column top product inlet and third distillation column top product exit phase
Connection.
High boiling substance in reduzate system can be removed by third rectifier unit 41, then pass through the 4th essence again
Distillation unit 42 removes the low-boiling point material in reduzate system, retains tower bottom product.
In order to further increase the removal rate of low boiling point organic impurities in reduzate system, in a kind of preferred embodiment
In, as shown in Figure 1, above-mentioned purifier units 40 include the 5th rectifier unit 43, the 5th rectifier unit 43 is provided with the 4th rectifying column
Bottom product entrance and the 5th rectifying bottoms outlet, the 4th rectifying tower bottom product entrance and the 4th rectifying bottoms outlet.
In a kind of preferred embodiment, as shown in Figure 1, above-mentioned purifier units 40 further include the first adsorbent equipment 44, the
One adsorbent equipment 44 is internally provided with active carbon layer, and the 5th rectifying tower bottom product that is provided with of the first adsorbent equipment 44 enters
Mouthful, the 5th rectifying tower bottom product entrance is connected with the 5th rectifying bottoms outlet, for removing the 5th rectifying tower bottom product
In solid impurity.In a kind of preferred embodiment, as shown in Figure 1, activated carbon adsorption device is additionally provided with the first purification production
Object outlet, purifier units 40 further include the second adsorbent equipment 45, and the inside of the second adsorbent equipment 45 is mounted with molecular sieve, and second inhales
Adsorption device 45 is provided with the first purified product entrance, and the first purified product entrance is connected with the outlet of the first purified product, is used for
The further solid impurity in the first purified product of removal.
Active carbon and molecular sieve all have porous structure, belong to good adsorbent, thus using active layer of charcoal
First adsorbent equipment 44 and the second adsorbent equipment 45 for being mounted with molecular sieve can further remove B, P in disilane, Al,
Fe, etc. metals and nonmetallic inclusion, improve the purity of disilane.
Preferably, as shown in Figure 1, above-mentioned disilane preparation facilities further includes impurity collection device 50, which collects dress
50 are set for recycling the impurity separated in rectification cell 20 and purifier units 40.
On the other hand the application also provides a kind of preparation method of disilane, as shown in Fig. 2, the preparation method includes:
Polysilicon raffinate is filtered, and obtains filtrate；Distillation process is carried out to filtrate, obtains chloro disilane；Make chloro disilane with
Reducing agent carries out reduction reaction, obtains disilane.
It include chloro disilane in polysilicon raffinate in the preparation method of disilane provided by the present application, it is residual with polysilicon
Liquid is to prepare raw material to save the preparation step of chloro disilane, substantially reduces the preparation cost of disilane.It is walked by filtering
Suddenly by the solid impurity (such as particulate material, metal-containing polymer, the impurity containing amorphous silicon and metal) in polysilicon raffinate
Removal.Then pass through distillation process, remove the organic impurities component in filtrate, obtain chloro disilane；Finally by chloro second silicon
Alkane and reducing agent carry out reduction reaction, obtain required product disilane.Above-mentioned preparation method have it is at low cost, process flow is short
And disilane it is with high purity the advantages that.
In order to further decrease the content of solid impurity in filtrate, filtrate purity is improved, it is preferable that control in filtration step
Filtering accuracy is 0.5~1 μm.Filtering accuracy control can farthest be removed containing amorphous silicon and gold within the above range
The impurity of category, filtering accuracy is too small, and filter is easy blocking to frequently overhaul, and the excessive then removal rate of filtering accuracy reduces.
Disilane is prepared using above-mentioned preparation method and advantageously reduces preparation cost, while improving the purity of disilane.?
In a kind of preferred embodiment, as shown in Fig. 2, above-mentioned distillation process include: by filtrate with except tiron carries out the first rectifying
Process obtains the first overhead product；And the first overhead product is subjected to the second distillation process, obtain chloro disilane.
It in the first distillation process, is added in filtrate and removes tiron, the titaniferous impurity in filtrate can be made to try with titanium is removed
Complex reaction occurs for agent, is changed into high boiling substance.This is conducive to improve in the first distillation process, and chlorosilane is miscellaneous with titaniferous
The separation rate of matter, and then be conducive to improve the purity of chlorosilane.
Used herein can occur complex reaction with above-mentioned titaniferous impurity except tiron can be in this field
Reagent.In a preferred embodiment, except tiron includes but is not limited to tetrahydrofuran, oxinane, in polyethylene glycol
It is one or more.Using above-mentioned several reagents as except tiron is conducive to further increase titaniferous impurity and removes tiron
Complexing degree, and then be conducive to further increase the purity of chlorosilane.
Preferably, except in the molal quantity of tiron and filtrate the ratio between molal quantity of titaniferous impurity be (1~10): 1.Except titanium tries
The ratio between molal quantity of titaniferous impurity includes but is not limited to above range in the molal quantity of agent and filtrate, and is limited to above-mentioned model
Be conducive to further increase the removal rate of titaniferous impurity in filtrate in enclosing.
Those skilled in the art can according to need the tower top pressure for adjusting above-mentioned first distillation process and the second distillation process
Power, tower top temperature and column plate series.In order to improve the separative efficiency of chloro disilane in the first distillation process, it is preferable that first
In distillation process, tower top pressure is 50~120KPa, and tower top temperature is 110~177 DEG C, and plate theory series is 60~120.For
The separative efficiency of chloro disilane in the first distillation process is further increased, it is highly preferred that in the first distillation process, tower top pressure
Power is 65~90KPa, and tower top temperature is 130~170 DEG C, plate theory series 80~110.
In order to further increase the removal rate of low boiling impurity in the second distillation process, in a kind of preferred embodiment
In, in the second distillation process, tower top pressure is 40~100KPa, and tower top temperature is 110~172 DEG C, tower theoretical stage 70~90.
It is highly preferred that tower top pressure is 45~90KPa in the second distillation process, tower top temperature is 120~170 DEG C, and tower theoretical stage is
75~85.
High-boiling-point impurity in filtrate includes that methylchlorosilane, chloro disilane and the metal height in polysilicon raffinate are poly-
Object, low boiling impurity include the chlorosilanes such as low-boiling-point substance, such as trichlorosilane, silicon tetrachloride.It is walked by above-mentioned first distillation process
Suddenly the high-boiling-point impurity in filtrate can be removed, in order to remove the low boiling impurity in filtrate, above-mentioned distillation process further includes
Two distillation processes, second distillation process include that will carry out the second rectifying through the first overhead product that the first distillation process obtains
Journey collects tower bottom product, obtains chloro disilane.
Disilane can be converted by chloro disilane by reduction reaction, in order to improve the extent of reaction of reduction reaction and anti-
Answer rate, in a preferred embodiment, during reduction reaction, reaction temperature -20~20 DEG C, reaction pressure be 3~
4bar.Preferably, the weight ratio of reducing agent and chloro disilane is 1:(2~5).The weight ratio packet of reducing agent and chloro disilane
Above range is included but be not limited to, and reduces the reaction interval for limiting and being conducive to further increase chloro disilane within the above range
Degree, and then improve the yield of disilane.
In a preferred embodiment, reduction reaction includes that reducing agent is added in chloro disilane react
The step of to disilane.In above-mentioned reduction reaction, reducing agent can select type commonly used in the art, it is preferable that reducing agent is
One of complex metal hydride, more preferably lithium aluminium hydride reduction, the group of sodium aluminum hydride and diethylaluminum hydride composition are a variety of.
Specific reaction equation for example may is that LiAlH4+Si2HmCln→Si2H6+LiCl+AlCl3(m+n=6)
Wherein, by-product silane has been supervened in reaction process.
In a kind of preferred embodiment, the molal quantity of chloro disilane is the 1~5 of the molal quantity of complex metal hydride
Times, this is conducive to the conversion ratio for improving reduction reaction.
Above-mentioned reduction reaction can carry out under the action of organic solvent, protective gas and catalyst.
Above-mentioned organic solvent can select solvent commonly used in the art, in a kind of preferred embodiment, organic solvent packet
Ether and/or tetrahydrofuran are included but are not limited to, this is conducive to the compatibility for improving reaction raw materials, and then is conducive to improve reduction instead
The extent of reaction answered.It is highly preferred that 1~8 times for mole stating the molal quantity for complex metal hydride of organic solvent.
Above-mentioned protective gas can select inert gas or nitrogen commonly used in the art, in a kind of preferred embodiment,
Above-mentioned protective gas includes but is not limited to one of nitrogen, argon gas and helium or a variety of.
The progress that can promote the reduction reaction of chloro disilane by adding catalyst, improves reaction efficiency.A kind of excellent
In the embodiment of choosing, catalyst includes but is not limited to one of group of Pt, Pd, Ni and Co composition or a variety of.
In order to further increase the purity of disilane, the high-purity disilane for meeting semicon industry application requirement is obtained,
In a kind of preferred embodiment, as shown in Fig. 2, above-mentioned preparation method further includes purifying the product system of reduction reaction
The step of, the step of purification includes: that the product system of reduction reaction is carried out third distillation process, third overhead product is obtained,
To remove organic solvent, the tower top temperature of third distillation process is -10~10 DEG C；Third overhead product is set to carry out the 4th rectifying
Process, obtains the 4th overhead product and the 4th tower bottom product, and the tower top temperature of the 4th distillation process is -50~-30 DEG C；By the 4th
Tower bottom product carries out the 5th distillation process, obtains disilane, and the tower top temperature of the 5th distillation process is -20~-15 DEG C.
In order to further improve the purity of disilane, as shown in Fig. 2, in a preferred embodiment, purification
Step further include: the tower bottom product for obtaining the 5th distillation process carries out adsorption treatment, and the step of adsorption treatment includes: using living
Property charcoal adsorption treatment is carried out to the tower bottom product of the 5th distillation process, obtain the first purification object；It is purified using molecular sieve to first
Object carries out adsorption treatment, obtains disilane.Preferably, the temperature of adsorption treatment process is -35~20 DEG C.
Active carbon and molecular sieve can further remove B, P in disilane, Al, Fe, etc. metals and nonmetallic inclusion, produce
Product purity reaches 4N, O2≤ 1.0, N2≤ 2.0, H2O≤1.0, SiH4≤ 400, CO2≤ 1.0, CH4≤1.0(ppmv)。
Preferably, molecular sieve includes but is not limited to one of 4A molecular sieve, 4.5A molecular sieve and 5A molecular sieve or a variety of；
The shape of active carbon includes but is not limited to spherical or cylindrical, this kind of active carbon iodine sorption value with higher and specific surface area,
Be conducive to improve adsorption efficiency.It is highly preferred that the specific surface area of active carbon can be 400~800m2/ g, iodine sorption value >=
1100mg/g。
Preferably, the adsorption column that the adsorbent equipment used during above-mentioned adsorption treatment is ratio of height to diameter between 2~9, suction
The temperature of attached processing is -35~20 DEG C.It is highly preferred that doing electrobrightening processing to the inner wall of adsorption column.
The application is described in further detail below in conjunction with specific embodiment, these embodiments should not be understood as limitation originally
Apply for range claimed.
Embodiment 1
Polysilicon raffinate is filtered by 0.5 μm of filtering accuracy filter, obtains filtrate.
Tetrahydrofuran is reacted with the titanium impurity in filtrate, the additive amount of tetrahydrofuran and the mole ratio of titanium impurity are 4:
1, and the pressure of first rectifying column is 75KPa, the number of plates is 100 pieces, and tower top temperature is 145 DEG C, the first obtained overhead product
With tower reactor production.Tower reactor extraction material containing reagent is returned to reactive moieties to react again.
First overhead product is delivered to Second distillation column, and the pressure of Second distillation column is 70KPa, the number of plates 80
Block, tower top temperature are 130 DEG C, obtain tower bottom extraction material (chloro disilane).
Above-mentioned tower bottom extraction material is delivered in reduction apparatus (micro passage reaction) and carries out reduction reaction, reaction temperature
5 DEG C, pressure 350KPa, lithium aluminium hydride reduction is selected to be used as reducing agent, the molar ratio of reducing agent and chloro disilane is 1:4, selection Pt
As catalyst, ether obtains reduzate (thick disilane) as reaction dissolvent.
Above-mentioned reduzate is delivered in third distillation column and carries out rectifying, the pressure for controlling third distillation column is 40KPa,
The number of plates is 20 pieces, -5 DEG C of tower top temperature, obtains tower reactor extraction material containing reagent and overhead extraction material.Tower reactor extraction contains reagent
Material returns to reactive moieties and re-uses, and overhead extraction material is delivered to the 4th rectifying column and carries out rectifying, controls the 4th rectifying column
Pressure be -68KPa, the number of plates be 20 pieces, -40 DEG C of tower top temperature, obtain overhead extraction light component and tower bottom production.It will be upper
It states tower bottom production and is delivered in the 5th rectifying column and carry out rectifying, the pressure of the 5th rectifying column of control is -21KPa, and the number of plates is
20 pieces, tower top temperature is -20 DEG C, obtains tower bottom production.Above-mentioned tower bottom production is delivered in adsorbent equipment and is adsorbed
Processing, adsorbent are active carbon, and adsorption temp is -5 DEG C, and final products disilane is obtained after absorption.Product purity reaches 4N, O2
≤ 0.5, N2≤ 0.76, H2O≤0.62, SiH4≤ 198, CO2≤ 0.46, CH4≤0.57(ppmv)。
Embodiment 2
Polysilicon raffinate is filtered by 1 μm of filtering accuracy filter, obtains filtrate.
Polyethylene glycol is reacted with the titanium impurity in filtrate, the additive amount of polyethylene glycol and the mole ratio of titanium impurity are 3:
1, and the pressure of first rectifying column is 80KPa, the number of plates is 100 pieces, obtained the first overhead product and tower reactor production.By tower
Kettle extraction material containing reagent returns to reactive moieties and reacts again.
First overhead product is delivered to Second distillation column, and the pressure of Second distillation column is 70KPa, the number of plates 80
Block, tower top temperature are 130 DEG C, obtain tower bottom extraction material (chloro disilane).
Above-mentioned tower bottom extraction material is delivered in reduction apparatus (micro passage reaction) and is restored, reaction temperature -10
DEG C, pressure 300KPa selects diethyl aluminium oxide to be used as reducing agent, and the molar ratio of reducing agent and chloro disilane is 1:3, selection
Pd obtains reduzate (thick disilane) as reaction dissolvent as catalyst, ether.
Above-mentioned reduzate is delivered in third distillation column and carries out rectifying, the pressure for controlling third distillation column is 40KPa,
The number of plates is 20 pieces, -5 DEG C of tower top temperature, obtains tower reactor extraction material containing reagent and overhead extraction material.Tower reactor extraction contains reagent
Material returns to reactive moieties and re-uses, and overhead extraction material is delivered to the 4th rectifying column and carries out rectifying, controls the 4th rectifying column
Pressure be -68KPa, the number of plates be 20 pieces, -40 DEG C of tower top temperature, obtain overhead extraction light component and tower bottom production.It will be upper
It states tower bottom extraction material to be delivered in the 5th rectifying column and carry out rectifying, the pressure of the 5th rectifying column of control is -21KPa, the number of plates
It is 20 pieces, tower top temperature is -20 DEG C, obtained tower bottom extraction product object.Above-mentioned tower bottom production is delivered in adsorbent equipment
Adsorption treatment is carried out, adsorbent is molecular sieve, and adsorption temp is -20 DEG C, and final products disilane is obtained after absorption.Product purity
Reach 4N, O2≤ 0.7, N2≤ 0.81, H2O≤0.75, SiH4≤ 270, CO2≤ 0.77, CH4≤0.86(ppmv)。
Embodiment 3
Polysilicon raffinate is filtered by 0.5 μm of filtering accuracy filter, obtains filtrate.
Oxinane and polyethylene glycol are reacted with the titanium impurity in filtrate, the additive amount of tetrahydrofuran and rubbing for titanium impurity
Your amount is than being 5:1, and the pressure of first rectifying column is 80KPa, and the number of plates is 100 pieces, and tower top temperature is 155 DEG C, the obtained
One overhead product and tower reactor production.Tower reactor extraction material containing reagent is returned to reactive moieties to react again.
First overhead product is delivered to Second distillation column, and the pressure of Second distillation column is 70KPa, the number of plates 80
Block, tower top temperature are 130 DEG C, obtain tower bottom extraction material (chloro disilane).
Above-mentioned tower bottom extraction material is delivered in reduction apparatus (micro passage reaction) and carries out reduction reaction, reaction temperature
0 DEG C, pressure 350KPa, select lithium aluminium hydride reduction as reducing agent, reducing agent and chloro disilane molar ratio are 1:5, and Co is selected to make
For catalyst, ether obtains reduzate (thick disilane) as reaction dissolvent.
Above-mentioned reduzate is delivered in third distillation column and carries out rectifying, the pressure for controlling third distillation column is 67KPa,
The number of plates is 20 pieces, 0 DEG C of tower top temperature, obtains tower reactor extraction material containing reagent and overhead extraction material.Tower reactor extraction contains reagent
Material returns to reactive moieties and re-uses, and overhead extraction material is delivered to the 4th rectifying column and carries out rectifying, controls the 4th rectifying column
Pressure be -68KPa, the number of plates be 20 pieces, -40 DEG C of tower top temperature, obtain overhead extraction light component and tower bottom production.It will be upper
It states tower bottom production and is delivered in the 5th rectifying column and carry out rectifying, the pressure of the 5th rectifying column of control is -21KPa, and the number of plates is
20 pieces, -20 DEG C of tower top temperature, obtain tower bottom production.Above-mentioned tower bottom production is delivered in adsorbent equipment and is carried out at absorption
Reason, adsorbent are active carbon, and adsorption temp is -10 DEG C, and final products disilane is obtained after absorption.Product purity reaches 4N, O2
≤ 0.78, N2≤ 1.21, H2O≤0.49, SiH4≤ 190, CO2≤ 0.82, CH4≤0.78(ppmv)。
Embodiment 4
Polysilicon raffinate is filtered by 0.5 μm of filtering accuracy filter, obtains filtrate.
Oxinane is reacted with the titanium impurity in filtrate, the mole ratio of the additive amount and titanium impurity of tetrahydrofuran is
10:1, and the pressure of first rectifying column is 90KPa, the number of plates is 100 pieces, and tower top temperature is 170 DEG C, and the first obtained tower top produces
Object and tower reactor production.Tower reactor extraction material containing reagent is returned to reactive moieties to react again.
First overhead product is delivered to Second distillation column, and the pressure of Second distillation column is 90KPa, the number of plates 80
Block, tower top temperature are 170 DEG C, obtain tower bottom extraction material (chloro disilane).
Above-mentioned tower bottom extraction material is delivered in reduction apparatus (micro passage reaction) and carries out reduction reaction, reaction temperature
10 DEG C, pressure 400KPa, select sodium aluminum hydride as reducing agent, reducing agent and chloro disilane molar ratio are 1:5, and Pd is selected to make
For catalyst, tetrahydrofuran obtains reduzate (thick disilane) as reaction dissolvent.
Above-mentioned reduzate is delivered in third distillation column and carries out rectifying, the pressure for controlling third distillation column is 67KPa,
The number of plates is 20 pieces, 0 DEG C of tower top temperature, obtains tower reactor extraction material containing reagent and overhead extraction material.Tower reactor extraction contains reagent
Material returns to reactive moieties and re-uses, and overhead extraction material is delivered to the 4th rectifying column and carries out rectifying, controls the 4th rectifying column
Pressure be -49KPa, the number of plates be 20 pieces, -30 DEG C of tower top temperature, obtain overhead extraction light component and tower bottom production.It will be upper
It states tower bottom production and is delivered in the 5th rectifying column and carry out rectifying, the pressure of the 5th rectifying column of control is -4KPa, the number of plates 20
Block, obtains tower bottom production by -15 DEG C of tower top temperature.Above-mentioned tower bottom production is delivered in adsorbent equipment and carries out adsorption treatment,
Adsorbent is molecular sieve, and adsorption temp is -20 DEG C, and final products disilane is obtained after absorption.Product purity reaches 5N, O2≤
0.96, N2≤ 1.82, H2O≤0.74, SiH4≤ 320, CO2≤ 0.88, CH4≤0.89(ppmv)。
Embodiment 5
With the difference of embodiment 1 are as follows: except the ratio between molal quantity of titaniferous impurity is 0.5 in the molal quantity of tiron and filtrate:
1, other relevant parameters are consistent.
Product purity reaches 3.5N, O2≤ 0.77, N2≤ 1.21, H2O≤0.68, SiH4≤ 201, CO2≤ 0.53, CH4≤
0.58(ppmv)。
Embodiment 6
With the difference of embodiment 1 are as follows: in the first distillation process, tower top pressure 60KPa, tower top temperature is 120 DEG C, column plate
Theoretical stage 60, other relevant parameters are consistent.
Product purity reaches 3N, O2≤ 0.91, N2≤ 1.78, H2O≤0.94, SiH4≤ 341, CO2≤ 0.88, CH4≤1.1
(ppmv)。
Embodiment 7
With the difference of embodiment 1 are as follows: in the second distillation process, tower top pressure 100KPa, tower top temperature is 90 DEG C, tower reason
By series 70.Other relevant parameters are consistent.
Product purity reaches 3.5N, O2≤ 1.23, N2≤ 1.81, H2O≤0.74, SiH4≤ 317, CO2≤ 1.35, CH4≤
1.26(ppmv)。
Embodiment 8
With the difference of embodiment 1 are as follows: reaction temperature is 30 DEG C of KPa, reaction pressure 250KPa, reducing agent and chloro second silicon
The ratio between molal quantity of alkane is 1:1, and other relevant parameters are consistent.
Product purity reaches 3N, O2≤ 1.64, N2≤ 1.72, H2O≤0.64, SiH4≤ 365, CO2≤ 1.44, CH4≤
1.43(ppmv)。
Embodiment 9
With the difference of embodiment 1 are as follows: the temperature of adsorption treatment process is 30 DEG C, and other relevant parameters are consistent.
Product purity reaches 4N, O2≤ 0.62, N2≤ 0.79, H2O≤0.66, SiH4≤ 205, CO2≤ 0.64, CH4≤
0.61(ppmv)。
The performance of product obtained is shown in Table 1 in embodiment.
Table 1
It can be seen from the above description that the above embodiments of the present invention realized the following chievements:
By embodiment 1 to 9 it is found that being conducive to greatly promote disilane using the preparation method of disilane provided by the present application
Purity.
Comparing embodiment 1 and 5 except the ratio between the molal quantity of titaniferous impurity in the molal quantity of tiron and filtrate it is found that by limiting
Be conducive to improve the purity of disilane in the preferred range of the application.
Comparing embodiment 1 and 6 is it is found that be limited to this for pressure, temperature and the plate theory series in the first distillation process
Apply for the purity for being conducive to improve disilane in preferred range.
Comparing embodiment 1 and 7 is it is found that be limited to this for pressure, temperature and the plate theory series in the second distillation process
Apply for the purity for being conducive to improve disilane in preferred range.
Comparing embodiment 1 and 8 is it is found that by the reaction temperature of reduction reaction, reaction pressure and reducing agent and chloro second silicon
The ratio between molal quantity of alkane is limited to the purity for being conducive to improve disilane in the preferred range of the application.
Comparing embodiment 1 and 9 is it is found that the limit temperature of adsorption treatment process is conducive in the preferred range of the application
Improve the purity of disilane.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (13)
1. a kind of disilane preparation facilities, which is characterized in that the disilane preparation facilities includes:
Filter element (10), the filter element (10) are provided with polysilicon raffinate entrance and filtrate (liquid；
Rectification cell (20), the rectification cell (20) are provided with filtrate inlet and the outlet of chloro disilane, the filtrate inlet
It is connected with the filtrate inlet through filtrate transfer pipeline；
Reduction unit (30), the reduction unit (30) are provided with feed opening, and the feed opening and the chloro disilane export
It is connected through chloro disilane transfer pipeline, the feed opening is also used for that reducing agent is added.
2. disilane preparation facilities according to claim 1, which is characterized in that the rectification cell (20) includes:
First rectifier unit (21), first rectifier unit (21) are provided with the filtrate inlet and except tiron entrance and the
One overhead outlet；And
Second rectifier unit (22), second rectifier unit (22) are provided with the first overhead product entrance and the chloro second silicon
Alkane outlet, first overhead outlet are connected with the first overhead product entrance.
3. disilane preparation facilities according to claim 2, which is characterized in that the rectification cell (20) further includes except titanium
Agent delivery device (23), it is described to be provided to first rectifier unit (21) except titanium tries except tiron feeding mechanism (23) are used for
Agent.
4. disilane preparation facilities according to any one of claim 1 to 3, which is characterized in that the filter element
It (10) include at least one filter device, and the quantity of the filter device is denoted as N, as N=1, the filter device is set
It is equipped with the polysilicon raffinate entrance and the filtrate (liquid, as N > 1, N number of filter device is sequentially connected to, and presses object
The dynamic sequence of stream is provided with the polysilicon raffinate entrance positioned at the 1st filter device, positioned at the filtering of n-th
Device is provided with the filtrate (liquid.
5. disilane preparation facilities according to claim 4, which is characterized in that the filter device is provided with filter hole,
The diameter in the hole is 0.5~1 μm.
6. disilane preparation facilities according to claim 1, which is characterized in that the reduction unit (30) includes:
Reducing agent feeding mechanism (31), the reducing agent feeding mechanism (31) are provided with reducing agent supply opening；
Reduction apparatus (32), the reduction apparatus (32) are provided with the feed opening, and the feed opening and the reducing agent are supplied
Mouth is connected；
Heating device, the heating device are used to control the reaction temperature in the reduction apparatus (32).
7. disilane preparation facilities according to claim 6, which is characterized in that the reduction unit (30) further include:
Organic solvent feeding mechanism (33), the organic solvent feeding mechanism (33) is provided with organic solvent entrance, described organic
Colvent inlet is connected with the feed opening；
It protects gas feeding mechanism (34), the protection gas feeding mechanism (34) is provided with protection gas supply opening, and the protection gas supplies
Mouth is answered to be connected with the feed opening；
Catalyst feeding mechanism (35), the catalyst feeding mechanism (35) are provided with catalyst supply opening and the feed opening phase
Connection.
8. disilane preparation facilities according to claim 6 or 7, which is characterized in that the reduction apparatus (32) is micro- logical
Road reactor.
9. disilane preparation facilities according to claim 6 or 7, which is characterized in that the reduction apparatus (32) also sets up
There is the outlet of reduzate system, the disilane preparation facilities further includes purifier units (40), purifier units (40) setting
There is reduzate system entrance, the reduzate system entrance is connected with reduzate system outlet, for also
Original objects system is purified.
10. disilane preparation facilities according to claim 9, which is characterized in that the purifier units (40) include:
Third rectifier unit (41), the third rectifier unit (41) are provided with the reduzate system entrance, third rectifying
Overhead outlet；
4th rectifier unit (42), the 4th rectifier unit (42) are provided with third distillation column top product inlet and the 4th
Rectifying bottoms outlet, third distillation column top product inlet are connected with third distillation column top product exit.
11. disilane preparation facilities according to claim 10, which is characterized in that the purifier units (40) include the 5th
Rectifier unit (43), the 5th rectifier unit (43) are provided with the 4th rectifying tower bottom product entrance and the 5th rectifying tower bottom product
Outlet, the 4th rectifying tower bottom product entrance and the 4th rectifying bottoms outlet.
12. disilane preparation facilities according to claim 11, which is characterized in that the purifier units (40) further include
One adsorbent equipment (44), first adsorbent equipment (44) are internally provided with active carbon layer, and first adsorbent equipment
(44) be provided with the 5th rectifying tower bottom product entrance, the 5th rectifying tower bottom product entrance and the 5th rectifying column bottom produce
Object outlet is connected, for removing the solid impurity in the 5th rectifying tower bottom product.
13. disilane preparation facilities according to claim 12, which is characterized in that the activated carbon adsorption device is also set up
There is the outlet of the first purified product, the purifier units (40) further include the second adsorbent equipment (45), second adsorbent equipment
(45) inside is mounted with molecular sieve, and second adsorbent equipment (45) is provided with the first purified product entrance, and described first is net
Change product inlet to be connected with first purified product outlet, it is miscellaneous for further removing the solid in the first purified product
Matter.
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| CN102171143A (en) * | 2008-10-17 | 2011-08-31 | 瓦克化学股份公司 | Method for removing titanium from hexachlorodisilane |
| CN106946261A (en) * | 2017-04-06 | 2017-07-14 | 洛阳中硅高科技有限公司 | The retracting device of disilicone hexachloride |
| CN108862282A (en) * | 2018-08-09 | 2018-11-23 | 洛阳中硅高科技有限公司 | The preparation method of disilane |
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| WO2008058549A2 (en) * | 2006-11-13 | 2008-05-22 | Ahmed Elsadany Hassan | A new way to manufacture of silica fumed sio2 |
| CN102171143A (en) * | 2008-10-17 | 2011-08-31 | 瓦克化学股份公司 | Method for removing titanium from hexachlorodisilane |
| CN106946261A (en) * | 2017-04-06 | 2017-07-14 | 洛阳中硅高科技有限公司 | The retracting device of disilicone hexachloride |
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