CN115970489A - Process for separating silicon powder by ceramic microfiltration membrane - Google Patents
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- CN115970489A CN115970489A CN202211628674.7A CN202211628674A CN115970489A CN 115970489 A CN115970489 A CN 115970489A CN 202211628674 A CN202211628674 A CN 202211628674A CN 115970489 A CN115970489 A CN 115970489A
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Abstract
The invention belongs to the technical field of membrane separation, and particularly relates to a process for separating silicon powder by using a ceramic microfiltration membrane. According to the invention, the ceramic microfiltration membrane is used for separating and recovering silicon powder in chlorosilane waste liquid, and the tubular ceramic membrane filter element is used as a core filter element, so that the influence on the filtering performance of the silicon powder caused by processes such as different pore structure ceramic filter elements, different operation time, different solid contents of liquid, different operation pressure, different feeding flow rate and the like is avoided; permeate flux and membrane rejection were analyzed. And cleaning the ceramic micro-filtration membrane by adopting a liquid forward cleaning mode to determine optimal process condition parameters. The high-efficiency recovery of silicon powder in the industrial production is realized. The invention has the advantages of high efficiency of separating silicon powder, simple operation, wide application range and the like; and the cleaning method is simple and easy to clean, the service life is prolonged, and the silicon powder separation cost is reduced.
Description
Technical Field
The invention belongs to the technical field of membrane separation, and particularly relates to a process for separating silicon powder by using a ceramic microfiltration membrane.
Background
Membrane technology is widely used, is an important method for separating, enriching and concentrating substances, and has a long development history. Microfiltration membranes were developed in the beginning of 1900 s abroad and used in industrial production and application. The ceramic membrane separation technology is developed quickly, has the advantages of high-efficiency separation performance, heat resistance, chemical corrosion resistance, high mechanical strength, easiness in cleaning, long service life and the like, is widely applied to the fields of chemical industry, food, medical treatment and the like, and forms a high-technology industry with potential development prospect.
At present, the production industry of polysilicon at home and abroad generates residual chlorosilane liquid in the manufacturing process. According to the measurement, about 0.45 ton of solid slag is generated for each 1 ton of polysilicon, the part of the by-product is called slag slurry or silicon slag, and the silicon slag mainly comprises various chlorosilane and silicon powder. The domestic treatment technology for chlorosilane residual liquid has a large promotion space, the direct discharge of the chlorosilane residual liquid can cause environmental pollution, and the extensive treatment or utilization also causes great waste of raw materials and has adverse effects on the environment. An ideal chlorosilane residual liquid treatment process is urgently needed.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a process for separating silicon powder by using a ceramic microfiltration membrane. The invention researches the ceramic micro-filtration membranes with different apertures, inspects the membrane separation process parameters and the membrane cleaning process conditions, develops the continuous solid-liquid separation process and recovers the silicon powder of the residual liquid in the industrial production.
In order to realize the purpose of the invention, the technical scheme of the invention is as follows:
the invention provides a process for separating silicon powder by using a ceramic microfiltration membrane, which comprises the following steps:
(1) Pouring the material liquid into a circulating tank, starting a circulating pump, and adjusting the operating pressure of the material liquid by adjusting a reflux valve;
(2) The feed liquid passes through the ceramic membrane component by the circulating pump, the permeate liquid is discharged from the permeate liquid port, the residual feed liquid enters the circulating tank again, the volume of the permeate liquid is measured, and the permeation flux is calculated.
Preferably, the solid content of the feed liquid in the step (1) is 0.1% (w/w) to 0.4% (w/w).
Preferably, the operating pressure in step (1) is between 0.8bar and 3.2bar.
Preferably, the ceramic membrane in step (2) has a pore size of 50nm to 800nm.
Preferably, the operation time of the process is 1min to 2.5min.
Preferably, the process further comprises cleaning the ceramic membrane module, specifically, after the operation is finished, discharging the concentrated solution from the discharge port, closing the discharge outlet valve, pouring deionized water into the circulation tank, and cleaning the ceramic membrane module.
Further, the cleaning is continuous cleaning, each cleaning time is 1min, and the cleaning is continuously repeated for 1-5 times.
The membrane rejection rate of the process reaches 100 percent, and the membrane permeation flux is 11-30L/m 2 ·min。
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the ceramic microfiltration membrane is used for separating and recovering silicon powder in chlorosilane waste liquid, and the tubular ceramic membrane filter element is used as a core filter element, so that the influence on the filtering performance of the silicon powder caused by processes such as different pore structure ceramic filter elements, different operation time, different solid contents of liquid, different operation pressure, different feeding flow rate and the like is avoided; permeate flux and membrane rejection were analyzed. And cleaning the ceramic micro-filtration membrane by adopting a liquid forward cleaning mode to determine optimal process condition parameters. The high-efficiency recovery of the silicon powder in the industrial production is realized. The invention has the advantages of high efficiency of separating the silicon powder, simple operation, wide application range and the like; and the cleaning method is simple and easy to clean, the service life is prolonged, and the silicon powder separation cost is reduced.
Drawings
FIG. 1 is a flow chart of a process for separating silicon powder by a ceramic microfiltration membrane.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a process for separating silicon powder by using a ceramic microfiltration membrane, which comprises the following steps:
(1) Pouring the material liquid to be separated into a circulating tank, starting a circulating pump, and adjusting the operating pressure of the material liquid by adjusting a reflux valve;
(2) The feed liquid passes through the ceramic membrane component by the circulating pump, the permeate liquid is discharged from the permeate liquid port, the residual feed liquid enters the circulating tank again, the volume of the permeate liquid is measured, and the permeation flux is calculated.
Preferably, the solid content of the feed liquid in the step (1) is 0.1% (w/w) to 0.4% (w/w).
Preferably, the operating pressure in step (1) is between 0.8bar and 3.2bar.
Preferably, the ceramic membrane in step (2) has a pore size of 50nm to 800nm.
Preferably, the operation time of the process is 1min to 2.5min.
Preferably, the process further comprises cleaning the ceramic membrane module, specifically, after the operation is finished, discharging the concentrated solution from the discharge port, closing the discharge outlet valve, pouring deionized water into the circulation tank, and cleaning the ceramic membrane module.
Further, the cleaning is continuous cleaning, each cleaning time is 1min, and the cleaning is continuously repeated for 1-5 times.
Through calculation, the membrane rejection rate of the process for separating silicon powder by using the ceramic microfiltration membrane provided by the invention reaches 100%, and the membrane permeation flux is 11-30L/m 2 ·min。
Example 1
Pouring 8L of feed liquid (silicon powder solution) with the solid content of 0.1% (w/w) into a circulation tank, starting a circulating pump, adjusting the operating pressure of the feed liquid to be 1bar by adjusting a reflux valve, allowing the feed liquid with the volume of the permeate liquid under the operation time of 1min to enter a membrane component with the aperture of a ceramic membrane of 800nm through the circulating pump, discharging the permeate liquid from a permeate liquid port, and allowing the rest feed liquid to enter the circulation tank again; after the operation is finished, concentrated solution can be discharged from the discharge port, the discharge outlet valve is closed, 8L of deionized water is poured into the circulating tank, the ceramic membrane component is cleaned, the cleaning is carried out for 5 times, and the membrane permeation flux can be restored to the initial value. The permeation flux and the retention rate are calculated according to the following formula:
permeation flux:
vp- -volume or mass m of the permeate 3 Or Kg, am- -effective area m of the membrane 2 T-time h;
membrane rejection: r = (1-C1/C0). Times.100%
R-retention, C1-permeate concentration, C0-feed concentration.
Calculated, the membrane retention rate reaches 100 percent, and the membrane flux reaches 13L/m 2 ·min。
Example 2
The embodiment provides a process for separating silicon powder by using a ceramic microfiltration membrane, which is different from the process of the embodiment 1 in that the operation time is 2.5min. The calculated results show that the membrane retention rate reaches 100 percent and the membrane flux reaches 20L/m 2 ·min。
Example 3
This example provides a process for separating silicon powder with ceramic microfiltration membrane, which is different from example 1 in that the solid content of the feed liquid is 0.4% (w/w). Calculated, the membrane retention rate reaches 100 percent, and the membrane flux reaches 30L/m 2 ·min。
Example 4
This example provides a process for separating silicon powder with ceramic microfiltration membrane, which differs from example 1 in that the operating pressure is 2.5bar. The calculated results show that the membrane retention rate reaches 100 percent and the membrane flux reaches 25L/m 2 ·min。
Example 5
This example provides a comparative process for separating silicon powder with ceramic microfiltration membrane, which is different from example 1 in that the membrane module has a 50nm pore diameter. Calculated, the membrane retention rate reaches 100 percent, and the membrane flux reaches 11L/m 2 ·min。
Based on the above, the process for separating the silicon powder by using the ceramic microfiltration membrane provided by the invention has the advantages of good separation efficiency, simple operation and wide application range; and the cleaning method is simple and easy to clean, the service life is prolonged, and the separation cost is reduced.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (8)
1. The process for separating silicon powder by using the ceramic microfiltration membrane is characterized by comprising the following steps of:
(1) Pouring the material liquid into a circulating tank, starting a circulating pump, and adjusting the operating pressure of the material liquid by adjusting a reflux valve;
(2) The feed liquid passes through the ceramic membrane component by the circulating pump, the permeate liquid is discharged from the permeate liquid port, the residual feed liquid enters the circulating tank again, the volume of the permeate liquid is measured, and the permeation flux is calculated.
2. The process according to claim 1, wherein the solid content of the feed liquid in the step (1) is 0.1-0.4% (w/w).
3. The process according to claim 1, wherein the operating pressure in step (1) is between 0.8bar and 3.2bar.
4. The process according to claim 1, wherein the ceramic membrane in step (2) has a pore size of 50nm to 800nm.
5. The process according to claim 1, wherein the process is carried out for a period of time of 1 to 2.5min.
6. The process according to claim 1, further comprising cleaning the ceramic membrane module by discharging the concentrated solution from the discharge port after the operation is completed, closing the discharge outlet valve, pouring deionized water into the circulation tank, and cleaning the ceramic membrane module.
7. The process according to claim 6, wherein the washing is continuous washing, each washing is for 1min, and the washing is continuously repeated for 1-5 times.
8. The process according to claim 1, wherein the process has a membrane rejection rate of 100% and a membrane permeation flux of 11-30L/m 2 ·min。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211628674.7A CN115970489A (en) | 2022-12-18 | 2022-12-18 | Process for separating silicon powder by ceramic microfiltration membrane |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211628674.7A CN115970489A (en) | 2022-12-18 | 2022-12-18 | Process for separating silicon powder by ceramic microfiltration membrane |
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| CN115970489A true CN115970489A (en) | 2023-04-18 |
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| CN202211628674.7A Pending CN115970489A (en) | 2022-12-18 | 2022-12-18 | Process for separating silicon powder by ceramic microfiltration membrane |
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