CN110526246A - A kind of synthetic method vulcanizing silicon powder - Google Patents
A kind of synthetic method vulcanizing silicon powder Download PDFInfo
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- CN110526246A CN110526246A CN201910791714.1A CN201910791714A CN110526246A CN 110526246 A CN110526246 A CN 110526246A CN 201910791714 A CN201910791714 A CN 201910791714A CN 110526246 A CN110526246 A CN 110526246A
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- silicon powder
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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Abstract
The invention discloses a kind of synthetic method for vulcanizing silicon powder, which includes the following steps: (1) under inert atmosphere protection, lithium sulfide is uniformly mixed with silicon tetrachloride, reactor is transferred to and seals；(2) the mixture heating and thermal insulation in reactor is reacted into certain time；(3) it is down to room temperature after reaction, recycles excessive silicon tetrachloride；(4) solid product is separated using solvent, vulcanization silicon powder can be obtained.It is of the present invention vulcanization silicon powder synthetic method have simple process, it is at low cost, be easy to industrialized productive prospecting.
Description
Technical field
The invention belongs to field of material synthesis technology, more particularly to a kind of synthetic method for vulcanizing silicon powder.
Background technique
Silicon sulfide is a kind of inorganic compound, chemical formula SiS2, belong to rectangle or tetragonal system, it is steady under normal temperature and pressure
It is fixed, it meets moisture and just resolves into SiO2And H2S.Currently, the synthetic method in relation to silicon sulfide is less.Japan Patent (publication number
JPS62252310A the method for the silicon dioxde reaction acquisition silicon sulfide of sulfur vapor or hydrogen sulfide gas and boiling) is disclosed.This
Kind method will be by high-temperature heating, and efficiency is lower, higher cost, it is difficult to realize industrialized production.Therefore develop a kind of novel, high
Effect, environmental-friendly silicon sulfide synthetic method are of great significance.
Summary of the invention
The invention aims to solve the deficiencies in the prior art, provide it is a kind of it is efficient, inexpensive, environmental-friendly, be easy to
The new method of the synthesis vulcanization silicon powder of industrialized production.
It is as follows that the technical scheme adopted by the invention to solve the technical problem:
Silicon sulfide synthesis method of the present invention realizes that synthetic method includes using the method for low-temperature heat
Following steps:
(1) under inert atmosphere protection, lithium sulfide is uniformly mixed with silicon tetrachloride, reactor is transferred to and seals；
(2) mixture in reactor is heated to certain temperature and insulation reaction certain time；
(3) it is down to room temperature after reaction, excessive silicon tetrachloride is recycled by distillating method；
(4) solid product in reactor is added in a certain amount of solvent, by being separated by solid-liquid separation, obtains sulfur-bearing SiClx
Solution, retort solution, and dry solid therein and vulcanization silicon powder can be obtained.
In the present invention, the purity of the lithium sulfide and silicon tetrachloride is not less than 90%.
In the present invention, the molar ratio of lithium sulfide and silicon tetrachloride is 2:(1-3 in the step (1)).
In the present invention, in the step (2), the heating rate of heating is 0.5-20 DEG C/min, and insulation reaction temperature is
100-300 DEG C, soaking time 1-100h.
In the present invention, in the step (3), the temperature for being distilled to recover excessive silicon tetrachloride is 60-100 DEG C.
In the present invention, in the step (4), solvent is benzene, and the additive amount of benzene is with the vulcanization in abundant dissolved solid product
Subject to silicon, the temperature of distillation removal benzene is 85-120 DEG C.
In the present invention, in the step (4), drying temperature is 90-100 DEG C.
In the present invention, inert atmosphere described in step (1) is the gas not reacted with reactant and product
Or their mixed gas, including argon gas and nitrogen.
In the present invention, " room temperature " is 0-40 DEG C.
Compared with prior art, the present invention its advantages are mainly reflected in:
Silicon sulfide is synthesized under heating using lithium sulfide and silicon tetrachloride in the present invention, is a kind of the green of resource rational utilization
Color synthetic method.This method is efficient, at low cost, environmental-friendly, and is easy to industrializing implementation.
Detailed description of the invention
Fig. 1 is the X-ray diffractogram of 1 reaction product of the embodiment of the present invention.
Specific implementation method
With reference to the accompanying drawing, technical solution of the present invention is described further with specific embodiment, but guarantor of the invention
It is without being limited thereto to protect range.
The purity of lithium sulfide and silicon tetrachloride that the embodiment of the present invention uses is not less than chemical pure (> 90%).
Embodiment 1
Under nitrogen atmosphere protection, lithium sulfide is uniformly mixed with silicon tetrachloride with molar ratio 2:1, is transferred to reactor simultaneously
Sealing.140 DEG C are heated to the heating rate of 2 DEG C/min, keeps the temperature 5h.It is down to room temperature after reaction, is distilled back by 100 DEG C
Receive excessive silicon tetrachloride.Solid product in reactor is added in benzene, by being separated by solid-liquid separation, obtains the benzene of sulfur-bearing SiClx
Solution is distilled to recover benzene at 120 DEG C, and dries solid therein at 100 DEG C and vulcanization silicon powder can be obtained.Fig. 1 is it
The diffraction pattern of the x-ray of product can only symbolize the X-ray map of lithium chloride, according to conservation of matter law, centainly have in product
Silicon sulfide.
Embodiment 2
Under argon atmosphere protection, lithium sulfide is uniformly mixed with silicon tetrachloride with molar ratio 1:1, is transferred to reactor simultaneously
Sealing.100 DEG C are heated to the heating rate of 0.5 DEG C/min, keeps the temperature 100h.It is down to room temperature after reaction, is steamed by 60 DEG C
Evaporate the excessive silicon tetrachloride of recycling.Solid product in reactor is added in benzene, by being separated by solid-liquid separation, obtains sulfur-bearing SiClx
Benzole soln, benzene is distilled to recover at 85 DEG C, and dry solid therein at 100 DEG C and vulcanization silicon powder can be obtained.
Embodiment 3
Under nitrogen atmosphere protection, lithium sulfide is uniformly mixed with silicon tetrachloride with molar ratio 2:3, is transferred to reactor simultaneously
Sealing.300 DEG C are heated to the heating rate of 20 DEG C/min, keeps the temperature 1h.It is down to room temperature after reaction, is distilled back by 80 DEG C
Receive excessive silicon tetrachloride.Solid product in reactor is added in benzene, by being separated by solid-liquid separation, obtains the benzene of sulfur-bearing SiClx
Solution is distilled to recover benzene at 90 DEG C, and dries solid therein at 100 DEG C and vulcanization silicon powder can be obtained.
Embodiment 4
Under nitrogen and the protection of argon gas mixed atmosphere, lithium sulfide is uniformly mixed with silicon tetrachloride with molar ratio 2:1, is shifted
To reactor and seal.200 DEG C are heated to the heating rate of 10 DEG C/min, heat preservation is for 24 hours.It is down to room temperature after reaction, leads to
It crosses 90 DEG C and is distilled to recover excessive silicon tetrachloride.Solid product in reactor is added in benzene, by being separated by solid-liquid separation, is obtained
The benzole soln of sulfur-bearing SiClx is distilled to recover benzene at 100 DEG C, and dries solid therein at 100 DEG C and silicon sulfide can be obtained
Powder.
Above-mentioned embodiment is only a preferred solution of the present invention, not the present invention is made in any form
Limitation, there are also other variations and modifications on the premise of not exceeding the technical scheme recorded in the claims.
Claims (8)
1. a kind of synthetic method for vulcanizing silicon powder, which comprises the steps of:
(1) under inert atmosphere protection, lithium sulfide is uniformly mixed with silicon tetrachloride, reactor is transferred to and seals；
(2) mixture in reactor is heated to certain temperature and insulation reaction certain time；
(3) it is down to room temperature after reaction, excessive silicon tetrachloride is recovered by distillation；
(4) solid product in reactor is added in a certain amount of solvent, after separation of solid and liquid, obtains the solution of sulfur-bearing SiClx,
Retort solution, and dry solid therein and vulcanization silicon powder can be obtained.
2. a kind of synthetic method for vulcanizing silicon powder as described in claim 1, which is characterized in that the lithium sulfide and four chlorinations
The purity of silicon is not less than 90%.
3. as described in claim 1 it is a kind of vulcanize silicon powder synthetic method, be characterized in that, in the step (1), lithium sulfide with
The molar ratio of silicon tetrachloride is 2:(1-3).
4. a kind of synthetic method for vulcanizing silicon powder as described in claim 1, which is characterized in that in the step (2), heating
Heating rate is 0.5-20 DEG C/min, and insulation reaction temperature is 100-300 DEG C, soaking time 1-100h.
5. a kind of synthetic method for vulcanizing silicon powder as described in claim 1, which is characterized in that in the step (3), distill back
The temperature for receiving excessive silicon tetrachloride is 60-100 DEG C.
6. a kind of synthetic method for vulcanizing silicon powder as described in claim 1, which is characterized in that in the step (4), solvent is
Benzene, the additive amount of benzene are subject to the silicon sulfide in abundant dissolved solid product, and the temperature of distillation removal benzene is 85-120 DEG C.
7. a kind of synthetic method for vulcanizing silicon powder as described in claim 1, which is characterized in that in the step (4), drying temperature
Degree is 90-100 DEG C.
8. a kind of synthetic method for vulcanizing silicon powder as described in claim 1, which is characterized in that inertia described in step (1)
Atmosphere is the gas not reacted with reactant and product or their mixed gas, including argon gas and nitrogen.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910791714.1A CN110526246A (en) | 2019-08-26 | 2019-08-26 | A kind of synthetic method vulcanizing silicon powder |
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| CN201910791714.1A CN110526246A (en) | 2019-08-26 | 2019-08-26 | A kind of synthetic method vulcanizing silicon powder |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113461014A (en) * | 2021-07-30 | 2021-10-01 | 江西科泰新材料有限公司 | Double-temperature-zone gas-solid synthesis process of silicon disulfide |
-
2019
- 2019-08-26 CN CN201910791714.1A patent/CN110526246A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113461014A (en) * | 2021-07-30 | 2021-10-01 | 江西科泰新材料有限公司 | Double-temperature-zone gas-solid synthesis process of silicon disulfide |
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Application publication date: 20191203 |