CN214183129U - Equipment for preparing composite silicon adsorbent by using chlorosilane residual liquid and chitosan - Google Patents

Equipment for preparing composite silicon adsorbent by using chlorosilane residual liquid and chitosan Download PDF

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Publication number
CN214183129U
CN214183129U CN202022581082.7U CN202022581082U CN214183129U CN 214183129 U CN214183129 U CN 214183129U CN 202022581082 U CN202022581082 U CN 202022581082U CN 214183129 U CN214183129 U CN 214183129U
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chitosan
chlorosilane
adsorbent
residual liquid
unit
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CN202022581082.7U
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Chinese (zh)
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苏泽模
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Sichuan Guangyang Environmental Protection Technology Co ltd
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Sichuan Guangyang Environmental Protection Technology Co ltd
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Abstract

The utility model relates to a technical field that chlorosilane raffinate was handled and was retrieved, concretely relates to utilize equipment of chlorosilane raffinate and chitosan preparation composite silicon adsorbent, through adopting raw materials supply unit, reaction vessel, in and precipitation unit, drying unit, the equipment production line that waste gas treatment unit combination formed and was used for chlorosilane raffinate processing procedure, liquid in the processing procedure that makes the chlorosilane raffinate, gas all obtain effectively, safety, the processing of environmental protection, avoid chlorosilane raffinate processing procedure to cause secondary pollution, the economy of chlorosilane raffinate, the environmental protection utilization has been realized.

Description

Equipment for preparing composite silicon adsorbent by using chlorosilane residual liquid and chitosan
Technical Field
The utility model relates to a technical field that chlorosilane raffinate was handled and was retrieved, concretely relates to utilize equipment of chlorosilane raffinate and chitosan preparation composite silicon adsorbent.
Background
Most processes for domestic polycrystalline silicon production can generate chlorosilane residual liquid, and the main components of the process are as follows: silicon tetrachloride, dichlorosilane, trichlorosilane and the like are complex in components, and when meeting hydrogen in water, severe reaction can be generated and a large amount of hydrochloric acid and hydrogen are released, so that the silicon tetrachloride, the dichlorosilane, the trichlorosilane and the like are difficult to recycle, the environmental influence is large, and the scientific and effective cyclic utilization of chlorosilane residual liquid becomes a bottleneck of the development of the polycrystalline silicon industry due to the huge yield of chlorosilane residual liquid.
The patent with publication number CN108176366A discloses a method for preparing composite adsorbent by using chlorosilane raffinate and chitosan, a product and a use thereof, and provides a method with high practical value for recycling chlorosilane raffinate, which directly uses hydrochloric acid and silicic acid generated by chlorosilane hydrolysis, separates a certain amount of hydrochloric acid, and then adds chitosan, glutaraldehyde and the like to perform composite modification to obtain silicon dioxide-chitosan composite adsorbent with hydrophobic function, the whole treatment method has simple and environment-friendly process, the prepared composite adsorbent product can be widely applied to the field of industrial wastewater purification treatment, the practical value is high, however, the method for preparing the composite adsorbent by using chlorosilane raffinate and chitosan is only based on a laboratory manual operation stage, and because the chlorosilane raffinate and chitosan have complex components and great environmental hazard, at present, no industrial production equipment which can be applied to industrial production to prepare the composite adsorbent by using chlorosilane raffinate and chitosan is provided, the degree of automation is lower, directly adopts conventional chemical industry equipment to carry out the preparation of above-mentioned composite sorbent and causes secondary pollution easily, and the cost is higher, and it is unsatisfactory to make composite sorbent result of use, very big influence the recycle ratio of chlorosilane raffinate.
Therefore, a technical scheme is urgently needed at present to solve the technical problems that industrial production equipment which can be applied to industrial production to prepare the composite adsorbent from chlorosilane residual liquid and chitosan is unavailable, the treatment efficiency of chlorosilane residual liquid is low, the treatment effect is poor, and the recovery rate of chlorosilane residual liquid is influenced.
SUMMERY OF THE UTILITY MODEL
The utility model aims to provide a: aiming at the technical problems that no industrial production equipment which can be applied to industrial production to prepare the composite adsorbent from chlorosilane residual liquid and chitosan exists, the treatment efficiency of chlorosilane residual liquid is low, the treatment effect is poor, and the recycling rate of chlorosilane residual liquid is influenced, the equipment for preparing the composite silicon adsorbent from chlorosilane residual liquid and chitosan is provided.
In order to realize the purpose, the utility model discloses a technical scheme be:
the equipment for preparing the composite silicon adsorbent by using chlorosilane residual liquid and chitosan comprises a raw material supply unit, a reaction container, a neutralization and precipitation unit and a drying unit which are communicated through a pipeline, wherein the raw material supply unit comprises a chlorosilane residual liquid storage tank, a nitrogen storage tank, a compressed gas supply mechanism and a medicament premixing line, the medicament premixing line comprises a plurality of medicament barrels, a stirring chamber and a precipitation chamber are arranged in the reaction container, the reaction container and the neutralization and precipitation unit are connected with a waste gas treatment unit through an exhaust pipe, and the neutralization and precipitation unit is communicated with the reaction container through a liquid return pipeline.
The utility model discloses an utilize chlorosilane raffinate and chitosan preparation composite silicon adsorbent's equipment, through adopting raw materials supply unit, reaction vessel, neutralization and precipitation unit, drying unit, the equipment production line that the combination of exhaust-gas treatment unit formed and is used for chlorosilane raffinate processing procedure, liquid, gas in the processing procedure that makes the chlorosilane raffinate all obtain effective, safe, the processing of environmental protection, avoid chlorosilane raffinate processing procedure to cause secondary pollution, realized the economy of chlorosilane raffinate, environmental protection utilization.
As the preferred scheme of the utility model, the reaction vessel lateral wall is provided with the discharge gate, the discharge gate corresponds the inside overflow launder that is provided with of reaction vessel, the discharge gate is located the liquid level of mixing liquid in the reaction vessel above.
As the preferred scheme of the utility model, be provided with the scraper in the reaction vessel and construct, the scraper constructs including power unit and doctor-bar, power unit drives the doctor-bar removes.
As the utility model discloses a preferred scheme, the drip chamber bottom with neutralization precipitation unit bottom all is provided with the groove that gathers materials, the groove that gathers materials is big-end-up's loudspeaker form, the groove that gathers materials through arrange the material pipe with drying unit intercommunication.
As the utility model discloses a preferred scheme, the neutralizing and precipitating unit connects the hold up tank, the hold up tank passes through back liquid pipe connection reaction vessel.
In conclusion, owing to adopted above-mentioned technical scheme, the utility model discloses an utilize equipment of chlorosilane raffinate and chitosan preparation composite silicon adsorbent's beneficial effect is:
the raw material supply unit, the reaction container, the neutralization and precipitation unit, the drying unit and the waste gas treatment unit are combined to form an equipment production line for the chlorosilane residual liquid treatment process, so that liquid and gas in the chlorosilane residual liquid treatment process are effectively, safely and environmentally treated, secondary pollution caused in the chlorosilane residual liquid treatment process is avoided, and economic and environmental-friendly utilization of the chlorosilane residual liquid is realized.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for preparing a composite silicon adsorbent from chlorosilane raffinate and chitosan according to the present invention;
FIG. 2 is a schematic view of the structure of the reaction vessel according to the present invention.
Icon: the method comprises the following steps of 1-a material gun, 2-a reaction container, 21-a stirring chamber, 22-a settling chamber, 23-a discharge port, 24-an overflow tank, 25-a material collecting tank, 3-a material scraping mechanism, a 4-chlorosilane residual liquid storage tank, 5-a nitrogen storage tank, 6-a compressed gas supply mechanism, 7-a neutralization and precipitation unit, 8-a drying unit, 9-a waste gas treatment unit, 10-a medicament barrel, 20-a storage tank, 30-a liquid return pipeline, 40-an exhaust pipe, 50-a discharge pipe and 60-a stirring mechanism.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings.
In order to make the objects, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the invention.
Example 1
As shown in fig. 1 and 2, the apparatus for preparing a composite silicon adsorbent by using chlorosilane residual liquid and chitosan according to the present embodiment includes a raw material supply unit, a reaction vessel 2, a neutralization and precipitation unit 7 and a drying unit 8, which are communicated with each other through a pipeline, wherein the raw material supply unit includes a chlorosilane residual liquid storage tank 4, a nitrogen storage tank 5, a compressed gas supply mechanism 6 and a reagent premixing line, the reagent premixing line includes a plurality of reagent barrels 10, the reaction vessel 2 and the neutralization and precipitation unit 7 are connected with a waste gas treatment unit 9 through an exhaust pipe 40, and the neutralization and precipitation unit 7 is communicated with the reaction vessel 2 through a liquid return pipeline 30.
According to the equipment for preparing the composite silicon adsorbent by using the chlorosilane residual liquid and the chitosan, a production line for the chlorosilane residual liquid treatment process is formed by combining the raw material supply unit, the reaction container 2, the neutralization and precipitation unit 7, the drying unit 8 and the waste gas treatment unit 9, so that liquid, gas and waste water in the chlorosilane residual liquid treatment process are effectively, safely and environmentally treated, secondary pollution caused in the chlorosilane residual liquid treatment process is avoided, and the economic and environmental-friendly utilization of the chlorosilane residual liquid is realized.
Specifically, each medicament barrel 10 of the medicament premixing line is correspondingly filled with a medicament, each medicament barrel 10 is internally provided with a stirring mechanism 60 and a mechanical diaphragm pump, and the plurality of medicament barrels 10 are respectively communicated with a tap water main pipe through pipelines, so that each medicament is respectively subjected to automatic concentration precise adjustment and then is provided with power by the mechanical diaphragm pump to be input into the reaction container 2 for use, the precision and the automation of the medicament filling process are realized, and the sequence of the medicament adding process can be controlled by a PLC (programmable logic controller) system in the prior art.
Preferably, a discharge hole 23 is formed in the side wall of the reaction container 2, an overflow groove 24 is formed in the reaction container 2 corresponding to the discharge hole 23, the discharge hole 23 is located above the liquid level of the mixed liquid in the reaction container 2, a material collecting groove 25 is formed in the bottom of the settling chamber 22 and the bottom of the neutralization and precipitation unit 7, the material collecting groove 25 is in a horn shape with a large top and a small bottom, and the material collecting groove 25 is communicated with the drying unit 8 through a discharge pipe 50.
Specifically, a stirring chamber 21 and a settling chamber 22 which are communicated with each other and are close to the top of the reaction vessel 2 are formed in the reaction vessel 2 by a partition board which is obliquely arranged, a chlorosilane residual liquid storage tank 4 inputs chlorosilane residual liquid into the stirring chamber 21 through a material gun 1, a nitrogen storage tank 5 inputs nitrogen into the material gun, so that the chlorosilane residual liquid and the nitrogen are mixed and flow into the stirring chamber 21 to fully react with other reaction agents added into the stirring chamber 21, then generated adsorbent enters the settling chamber 22 in an overflow mode under the disturbance of compressed air input by a compressed air supply mechanism 6, an overflow groove 24 is arranged on the inner side wall of the settling chamber 22, a collecting groove 25 is arranged at the bottom, the adsorbent floating on the liquid surface in the settling chamber 22 enters the overflow groove 24 in an overflow mode and is output from a discharge hole 23, the precipitated adsorbent enters the collecting groove 25 to be collected and then is output from a discharge pipe 50 at the bottom, the liquid in the settling chamber 22 from which the adsorbent is separated is fed via a pipe to the neutralization and settling unit 7 for further treatment.
Preferably, a scraping mechanism 3 is arranged in the reaction container 2, the scraping mechanism 3 comprises a power mechanism and a scraping blade, and the power mechanism drives the scraping blade to move. Preferably, the power mechanism is a rotating structure composed of a fluted disc and a chain, drives the scraping blade arranged on the chain to move, pushes the suspended adsorbent to enter the settling chamber 22 from the stirring chamber 21 and then enter the overflow tank 24, and promotes the separation of the adsorbent.
Specifically, the neutralization and precipitation unit 7 includes the box and sets up a plurality of baffles in the box, adjacent baffle dislocation set forms overflow channel, set up the filtration filler that is used for hindering the adsorbent to pass through in the overflow channel, make the adsorbent sediment to the collecting tank 25 of bottom after being hindered, and simultaneously, set up the baffle and separate overflow channel input one side for a plurality of cavities, adjacent cavity top and bottom intercommunication, correspond in every cavity and set up rabbling mechanism 60 through a pipe connection medicament bucket 10, in order to promote going on of reaction, realize the make full use of chlorosilane raffinate, and avoid the secondary pollution that reaction waste water caused.
Specifically, overflow passageway output one side is provided with the level gauge for liquid level in detecting and the precipitation unit 7, when liquid level is too high or liquid concentration is less than 20% in the reaction vessel, introduces waste water into reaction vessel 2 through returning liquid pipeline 30 and recycles, avoids the waste water overflow that the liquid level was too high to guarantee going on smoothly of reaction process, realize chlorosilane raffinate treatment process's feature of environmental protection.
Further, the adsorbent output from the reaction vessel 2 and the neutralization precipitation unit 7 is uniformly input into a drying unit 8 for drying treatment to prepare the composite silicon adsorbent with extremely fine particles, extremely large specific surface area and good use effect, and preferably, the drying unit is a spray drying system, namely, the water-containing adsorbent is sprayed into the drying unit 8 in a spraying state through a spray head for drying and filter pressing, so that the drying efficiency and the product quality of the prepared adsorbent are improved.
Specifically, the adsorbent after drying is separated from hot air through the cyclone dust collector, so that the efficient separation of the adsorbent is realized, the concentrated collection and treatment of waste gas are facilitated, the residual quantity of the adsorbent in the waste gas is reduced, the adsorption efficiency is improved, and the risk of secondary pollution is reduced.
Specifically, the preparation method of the apparatus for preparing the composite silicon adsorbent by using chlorosilane residual liquid and chitosan in the embodiment relates to: chlorosilane residual liquid and nitrogen gas are mixed and flow into a stirring chamber 21 of a reaction container 2 along the same material gun 1 to be stirred and react, each reaction medicament is independently stirred and then quantitatively injected into the stirring chamber 21, compressed air is introduced into the stirring chamber 21 towards an opening of the material gun 1 in a hedging mode, the gas is wrapped and carried to react to generate an adsorbent, the adsorbent enters a settling chamber 22 of the reaction container 2 in an overflowing mode, and the adsorbent in a floating state in the settling chamber 22 is input into a drying unit 8 from a discharge port 23 on the side wall of the reaction container 2 in the overflowing mode. According to the reaction principle, the characteristic that chlorosilane raffinate is subjected to hydrolysis equilibrium reaction to generate silicon dioxide is utilized, the prior art that chitosan and glutaraldehyde carry out polymerization reaction on hydrolyzed silicon dioxide is combined to modify the silicon dioxide into a modified silicon dioxide adsorbent product with good hydrophobicity is utilized to prepare a silicon dioxide-chitosan composite silicon adsorbent product, the whole preparation process is combined with each other, reaction heat release and chemical equilibrium are effectively utilized to promote efficient, energy-saving and environment-friendly preparation of the silicon dioxide-chitosan composite silicon adsorbent product, the chlorosilane raffinate is fully recycled, specific equipment is arranged in a material filling process, a conveying process and a separating process in a targeted manner by combining an equipment structure from the aspect of the preparation method, wherein in the filling process, raw materials are filled in a chlorosilane raffinate and nitrogen mixed flow manner, the feeding process can not block the material gun 1, the accuracy of the feeding amount is ensured, the disturbance of mixed liquid consisting of chlorosilane residual liquid and various reaction reagents in the reaction container 2 is facilitated, the reaction is promoted to be carried out, the reaction time is reduced, the particle uniformity of the prepared adsorbent is increased, the using effect of the adsorbent is improved, meanwhile, compressed air is introduced in a mode of oppositely flushing raw materials and compressed air airflow by the material gun 1, the mixed liquid is further disturbed by the compressed air, the phenomenon that the adsorbent generated by the reaction of the chlorosilane residual liquid and the various reaction reagents blocks the material gun 1 is avoided, the reaction time is further reduced, the granularity of the adsorbent is smaller under the action of airflow impact, the using effect of the adsorbent is improved, in the conveying process, more bubbles are formed in the mixed liquid due to the introduction of nitrogen and the compressed air, the adsorbent generated by the wrapping reaction floats to the surface of the mixed liquid, so that in the separation process, the prepared adsorbent is conveniently separated in advance in an overflow mode, so that the reaction efficiency is further improved, and the use effect is improved.
Further, a plurality of stirring mechanisms 60 are arranged in the stirring chamber 21 of the reaction container 2, each stirring mechanism 60 comprises a motor, a rotating rod and blades arranged on the rotating rod, mixed raw materials input by the gun 1 and composed of chlorosilane residual liquid and nitrogen enter the stirring chamber 21 and then are fully mixed and stirred by the stirring mechanisms 60, the mixed raw materials are fully reacted with each reaction medicament added into the stirring chamber 21, and under the disturbance of the nitrogen and compressed air, the prepared adsorbent is wrapped by bubbles and easily floats to the surface of a mixed liquid, so that the mixed liquid is conveniently input into the settling chamber 22 of the reaction container 2 from the stirring chamber 21 of the reaction container 2 in an overflow mode.
Further, the adsorbent in a floating state in the settling chamber 22 enters the overflow groove 24 in the settling chamber 22 in an overflow manner and then is output from the discharge hole 23, the adsorbent is input into the settling chamber 22 from the stirring chamber 21 of the reaction vessel 2 to complete the first overflow treatment, and the adsorbent is input into the overflow groove 24 from the settling chamber 22 to complete the second overflow treatment, so that the two overflow treatments of the adsorbent are realized, the treatment time and resource consumption for separating the adsorbent from the mixed liquid are reduced, the separation efficiency of the adsorbent in the preparation process is improved, and the treatment efficiency of chlorosilane residual liquid is improved.
Further, the mixed liquid in the settling chamber 22 passes through the neutralization and precipitation unit 7 and then is input into the drying unit 8, and the neutralization and precipitation unit 7 is used for introducing a neutralization agent to react with the mixed liquid.
Specifically, the waste water after chlorosilane residual liquid reacts with chitosan to generate the adsorbent also contains more unseparated adsorbent, and the waste water is directly discharged to cause environmental pollution, the waste water after twice overflow treatment in the reaction container 2 is input into the neutralization precipitation unit 7, alkali liquor and PAM are introduced, the waste water is treated, the generation of the adsorbent is further promoted, the chlorosilane residual liquid is fully recycled, the chlorosilane residual liquid treatment process is safer and more environment-friendly, and secondary pollution is avoided.
Preferably, the wastewater output by the neutralization and precipitation unit 7 is input into a storage tank 20 for temporary storage and is introduced into the reaction vessel 2 through a liquid return pipeline 30 for recycling.
Specifically, the wastewater treated by the neutralization and precipitation unit 7 flows back into the reaction vessel 2, so that on one hand, chlorosilane residual liquid continuously reacts with medicaments such as chitosan and the like to realize the full recovery of the chlorosilane residual liquid, on the other hand, the wastewater treatment device is also favorable for avoiding secondary pollution caused by wastewater discharge, reducing the filling of water in the reaction process and saving resources.
Preferably, the gas in the reaction vessel 2 and the neutralization precipitation unit 7 is introduced into the exhaust gas treatment unit 9 through the exhaust pipe 40.
Specifically, the waste gas treatment unit 9 is a conventional tail gas treatment device such as a spray tower and the like, so as to ensure the environmental protection of the chlorosilane residual liquid treatment process to the maximum extent.
The above description is only exemplary of the present invention and should not be taken as limiting the scope of the present invention, as any modifications, equivalents, improvements and the like made within the spirit and principles of the present invention are intended to be included within the scope of the present invention.

Claims (8)

1. The equipment for preparing the composite silicon adsorbent by using chlorosilane raffinate and chitosan is characterized by comprising a raw material supply unit, a reaction container (2), a neutralization and precipitation unit (7) and a drying unit (8) which are communicated through pipelines, wherein the raw material supply unit comprises a chlorosilane raffinate storage tank (4), a nitrogen storage tank (5), a compressed gas supply mechanism (6) and a medicament premixing line, the medicament premixing line comprises a plurality of medicament barrels (10), a stirring chamber (21) and a precipitation chamber (22) are arranged in the reaction container (2), the reaction container (2) and the neutralization and precipitation unit (7) are connected with a waste gas treatment unit (9) through an exhaust pipe (40), and the neutralization and precipitation unit (7) is communicated with the reaction container (2) through a liquid return pipeline (30).
2. The equipment for preparing the composite silicon adsorbent by using the chlorosilane residual liquid and the chitosan as claimed in claim 1, wherein a discharge hole (23) is formed in the side wall of the reaction vessel (2), an overflow groove (24) is formed in the reaction vessel (2) corresponding to the discharge hole (23), and the discharge hole (23) is positioned above the liquid level of the mixed liquid in the reaction vessel (2).
3. The apparatus for preparing the composite silicon adsorbent by using the chlorosilane residual liquid and the chitosan as claimed in claim 2, wherein a scraping mechanism (3) is arranged in the reaction vessel (2), the scraping mechanism (3) comprises a power mechanism and a scraping blade, and the power mechanism drives the scraping blade to move.
4. The apparatus for preparing the composite silicon adsorbent by using chlorosilane residual liquid and chitosan as claimed in claim 3, wherein the bottom of the settling chamber (22) and the bottom of the neutralization and precipitation unit (7) are both provided with a material collecting groove (25), the material collecting groove (25) is in a horn shape with a large top and a small bottom, and the material collecting groove (25) is communicated with the drying unit (8) through a material discharging pipe (50).
5. The apparatus for preparing the composite silicon adsorbent by using the chlorosilane residual liquid and the chitosan as claimed in claim 1, wherein the neutralization and precipitation unit (7) comprises a box body and a plurality of partition plates arranged in the box body, adjacent partition plates are arranged in a staggered manner to form an overflow channel, and a filter filler for blocking the passage of the adsorbent is arranged in the overflow channel.
6. The apparatus for preparing the composite silicon adsorbent by using chlorosilane residual liquid and chitosan as claimed in claim 5, wherein a liquid level meter is arranged at the output side of the overflow channel and is used for detecting the liquid level in the neutralization precipitation unit (7).
7. The apparatus for producing a composite silicon adsorbent using chlorosilane residual liquid and chitosan according to any one of claims 1 to 6, wherein a plurality of stirring mechanisms (60) are provided in the stirring chamber (21).
8. The apparatus for preparing the composite silicon adsorbent by using chlorosilane residual liquid and chitosan as claimed in claim 7, wherein the neutralization and precipitation unit (7) is connected with a storage tank (20), and the storage tank (20) is connected with the reaction vessel (2) through a liquid return pipeline (30).
CN202022581082.7U 2020-11-10 2020-11-10 Equipment for preparing composite silicon adsorbent by using chlorosilane residual liquid and chitosan Withdrawn - After Issue CN214183129U (en)

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CN202022581082.7U CN214183129U (en) 2020-11-10 2020-11-10 Equipment for preparing composite silicon adsorbent by using chlorosilane residual liquid and chitosan

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112452304A (en) * 2020-11-10 2021-03-09 四川广阳环保科技有限公司 Method and equipment for preparing composite silicon adsorbent by using chlorosilane residual liquid and chitosan

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112452304A (en) * 2020-11-10 2021-03-09 四川广阳环保科技有限公司 Method and equipment for preparing composite silicon adsorbent by using chlorosilane residual liquid and chitosan
CN112452304B (en) * 2020-11-10 2024-04-09 四川广阳环保科技有限公司 Method and equipment for preparing composite silicon adsorbent by utilizing chlorosilane raffinate and chitosan

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