CN114262792A - Organic silicon slurry residue hydrolysis treatment process and resource recycling method - Google Patents

Organic silicon slurry residue hydrolysis treatment process and resource recycling method Download PDF

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Publication number
CN114262792A
CN114262792A CN202111455208.9A CN202111455208A CN114262792A CN 114262792 A CN114262792 A CN 114262792A CN 202111455208 A CN202111455208 A CN 202111455208A CN 114262792 A CN114262792 A CN 114262792A
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slurry
tank
residue
gas
slurry residue
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王长明
窦冰之
和德杰
张泽一
赵炳泉
刘万鹏
杨本超
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SILICON CHEMICAL BRANCH LUXI CHEMICAL GROUP CO Ltd
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SILICON CHEMICAL BRANCH LUXI CHEMICAL GROUP CO Ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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Abstract

The invention belongs to the field of organic silicon byproduct treatment and comprehensive utilization, and discloses an organic silicon slurry residue hydrolysis treatment process and a resource recycling method.

Description

Organic silicon slurry residue hydrolysis treatment process and resource recycling method
Technical Field
The invention belongs to the technical field of treatment and comprehensive utilization of organic silicon byproducts, and particularly relates to a treatment method of organic silicon slag slurry.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
The waste slag slurry produced in the process of synthesizing organosilicon monomer mainly comprises more high-boiling residues, a small amount of silicon powder brought out by a fluidized bed and a copper catalyst. The boiling point of the high-boiling substance is mainly disilane and siloxane (about 70-80 percent), and the solid content is mainly silicon powder and copper catalyst (about 20-30 percent). The slag slurry has the characteristics that high-boiling-point substances in the slag slurry are deliquesced when meeting air, cuprous ions are easy to cause combustion and explosion when meeting open fire and air due to strong reducibility, and strong acid mist and combustion are easy to cause if the slag slurry is exposed in the air, so that the slag slurry needs to be subjected to harmless treatment. At present, slag slurry is discharged into a water tank for hydrolysis by a plurality of organic silicon production enterprises, and the discharged hydrogen chloride is seriously polluted and causes serious potential safety hazard.
Disclosure of Invention
The invention aims to provide a method for treating organic silicon slurry slag, which can realize harmless treatment of slurry slag generated in the production process of organic silicon.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
in a first aspect of the present invention, there is provided an organosilicon slurry-residue treatment system, comprising: a slurry residue steaming and drying kettle 1, a condenser 2, a condensate tank 3, a tail gas washing tower 5, a slurry residue hydrolysis tank 6, a filter press 8 and a filtrate tank 9; the gas outlet of the slurry residue steaming and drying kettle 1 is connected with the gas inlet of a distillation kettle rectifying tower, the gas outlet of the distillation kettle rectifying tower is connected with the gas inlet of a condenser 2, the liquid outlet of the condenser 2 is respectively connected with the liquid inlet of a condensate tank 3 and the liquid inlet of a slurry residue hydrolysis tank 6, and the gas outlet of the condenser 2 is connected with the gas inlet of a tail gas washing tower 5; the discharge hole of the slurry residue steaming and drying kettle 1 is connected with the feed inlet of the slurry residue hydrolysis tank 6, the liquid outlet of the slurry residue hydrolysis tank 6 is connected with the liquid inlet of the filter press 8, and the liquid outlet of the filter press 8 is connected with the liquid inlet of the filtrate tank 9.
In a second aspect of the present invention, there is provided an organosilicon slurry-residue treatment method, comprising:
heating and evaporating slurry slag in the production process of organic silicon to generate gas and solid slag;
washing and condensing the gas to obtain synthetic high boiling point;
mixing the solid slag with acid liquor for hydrolysis, and performing filter pressing on the reacted slurry to obtain the acid liquor and hydrolyzed solid slag;
carrying out copper extraction treatment on the hydrolyzed solid slag
And (4) sending the acid liquor to a hydrochloric acid treatment unit, and mixing the acid liquor with water to be used as the slurry residue hydrolysate for recycling.
The invention has the beneficial effects that:
(1) the method separates out pure high-boiling residues in the slurry residue, adopts a cracking method to carry out conversion treatment to obtain the organic silicon monomer, carries out hydrolysis treatment on the residual slurry residue to obtain hydrochloric acid serving as a calcium chloride production raw material, and carries out copper extraction treatment on the hydrolyzed solid residue, so that the organic silicon slurry residue is subjected to harmless and recycling treatment.
(2) The operation method is simple, low in cost, universal and easy for large-scale production.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a schematic view of the treatment of the organic silicon sludge of the present invention.
Wherein, the system comprises a slurry residue steaming and drying kettle 1, a heat exchanger 2, a condensate tank 3, a condensate pump 4, a tail gas washing tower 5, a slurry residue hydrolysis tank 6, a slurry pump 7, a filter press 8, a filtrate tank 9 and a filtrate pump 10.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
The organic silicon pulp residue treatment method comprises a pulp residue steaming and drying kettle, a cooler, a high-boiling storage tank, a pulp residue hydrolysis tank, a filter press, an acid storage tank and a tail gas washing tower, wherein the tops of the pulp residue steaming and drying kettle, the condenser and the tail gas washing tower are connected through pipelines, the bottom of the condenser is connected with the high-boiling storage tank, the pulp residue steaming and drying kettle is connected with the bottom of the pulp residue hydrolysis tank, stirring is arranged on the pulp residue hydrolysis tank, a bottom discharge port is connected with the filter press through a pulp pump, filtrate of the filter press is connected with a filtrate tank, the filtrate tank sends part of the filtrate out through a pump, and part of the filtrate returns to the hydrolysis tank.
And a process water continuous water replenishing pipe is arranged on the slurry residue hydrolysis tank.
The present invention is described in further detail below with reference to specific examples, which are intended to be illustrative of the invention and not limiting.
Example 1
As shown in figure 1, the method for treating the organic silicon pulp residue comprises a pulp residue steaming and drying kettle 1, a condenser 2, a high-boiling storage tank, a pulp residue hydrolysis tank 6, a filter press 8, an acid storage tank and a tail gas washing tower 5, wherein the tops of the pulp residue steaming and drying kettle 1, the condenser and the tail gas washing tower 5 are connected through pipelines, the bottom of the condenser is connected with the high-boiling storage tank, the pulp residue steaming and drying kettle 1 is connected with the bottom of the pulp residue hydrolysis tank 6, the pulp residue hydrolysis tank 6 is provided with a stirrer, a bottom discharge port is connected with the filter press 8 through a pulp pump, filtrate of the filter press 8 is connected with a filtrate tank 9, the filtrate tank 9 sends part of the filtrate out through a pump, and part of the filtrate returns to the pulp residue hydrolysis tank 6.
The invention mainly aims at the harmless treatment of the organic silicon slurry residue, the waste gas generated in the process is washed by water, the acid liquor in the hydrolysis process is recycled, and the solid residue is treated by copper extraction.
And (3) slurry and slag treatment: the method comprises the steps of heating and evaporating slurry residues in an organic silicon production process in a slurry residue steaming and drying kettle 1, controlling the evaporation temperature to be 200-300 ℃, washing a gas phase through a rectifying tower of the slurry residue steaming and drying kettle 1, condensing the gas phase through a condenser to obtain pure synthetic high-boiling liquid, washing the evaporated gas by using one part of the synthetic high-boiling liquid as reflux, using the other part of the synthetic high-boiling liquid as a high-boiling cracking raw material, pressurizing and conveying non-evaporated solid residues in the slurry residue steaming and drying kettle 1 into a slurry residue hydrolysis tank 6 through nitrogen, carrying out hydrolysis reaction on the slurry residue hydrolysis tank 6 and acid liquor, conveying the reacted slurry into a filter press 8 for filter pressing to obtain acid liquor and solid residues, conveying the solid residues into a slurry residue copper extraction unit for copper extraction treatment, conveying the acid liquor to a hydrochloric acid treatment unit, and mixing part of hydrochloric acid with fresh water to be used as slurry residue hydrolysate for recycling.
Because the slurry residue hydrolysis process is a heat release process, the heat exchanger is adopted to cool the circulating liquid, and the hydrolysis effect is improved.
By adopting the organic silicon slurry residue treatment method, after the cyclic treatment, the high-boiling condensate, the hydrochloric acid and the solid slurry residue are subjected to harmless and recycling treatment, in the prior art, the slag slurry is discharged into a water tank by a production enterprise for hydrolysis, and the discharged hydrogen chloride is seriously polluted and causes serious potential safety hazard.
Example 2
An organosilicon sludge treatment system, comprising: a slurry residue steaming and drying kettle 1, a condenser 2, a condensate tank 3, a tail gas washing tower 5, a slurry residue hydrolysis tank 6, a filter press 8 and a filtrate tank 9; the gas outlet of the slurry residue steaming and drying kettle 1 is connected with the gas inlet of a distillation kettle rectifying tower, the gas outlet of the distillation kettle rectifying tower is connected with the gas inlet of a condenser 2, the liquid outlet of the condenser 2 is respectively connected with the liquid inlet of a condensate tank 3 and the liquid inlet of a slurry residue hydrolysis tank 6, and the gas outlet of the condenser 2 is connected with the gas inlet of a tail gas washing tower 5; the discharge hole of the slurry residue steaming and drying kettle 1 is connected with the feed inlet of the slurry residue hydrolysis tank 6, the liquid outlet of the slurry residue hydrolysis tank 6 is connected with the liquid inlet of the filter press 8, and the liquid outlet of the filter press 8 is connected with the liquid inlet of the filtrate tank 9.
The operation was carried out in the same manner as in example 1.
Example 3
An organosilicon sludge treatment system, comprising: a slurry residue steaming and drying kettle 1, a condenser 2, a condensate tank 3, a tail gas washing tower 5, a slurry residue hydrolysis tank 6, a filter press 8 and a filtrate tank 9; the gas outlet of the slurry residue steaming and drying kettle 1 is connected with the gas inlet of a distillation kettle rectifying tower, the gas outlet of the distillation kettle rectifying tower is connected with the gas inlet of a condenser 2, the liquid outlet of the condenser 2 is respectively connected with the liquid inlet of a condensate tank 3 and the liquid inlet of a slurry residue hydrolysis tank 6, and the gas outlet of the condenser 2 is connected with the gas inlet of a tail gas washing tower 5; the discharge hole of the slurry residue steaming and drying kettle 1 is connected with the feed inlet of the slurry residue hydrolysis tank 6, the liquid outlet of the slurry residue hydrolysis tank 6 is connected with the liquid inlet of the filter press 8, and the liquid outlet of the filter press 8 is connected with the liquid inlet of the filtrate tank 9.
And a liquid outlet of the condensate tank 3 is connected with a liquid inlet of a distillation kettle rectifying tower.
The operation was carried out in the same manner as in example 1.
Example 4
An organosilicon sludge treatment system, comprising: a slurry residue steaming and drying kettle 1, a condenser 2, a condensate tank 3, a tail gas washing tower 5, a slurry residue hydrolysis tank 6, a filter press 8 and a filtrate tank 9; the gas outlet of the slurry residue steaming and drying kettle 1 is connected with the gas inlet of a distillation kettle rectifying tower, the gas outlet of the distillation kettle rectifying tower is connected with the gas inlet of a condenser 2, the liquid outlet of the condenser 2 is respectively connected with the liquid inlet of a condensate tank 3 and the liquid inlet of a slurry residue hydrolysis tank 6, and the gas outlet of the condenser 2 is connected with the gas inlet of a tail gas washing tower 5; the discharge hole of the slurry residue steaming and drying kettle 1 is connected with the feed inlet of the slurry residue hydrolysis tank 6, the liquid outlet of the slurry residue hydrolysis tank 6 is connected with the liquid inlet of the filter press 8, and the liquid outlet of the filter press 8 is connected with the liquid inlet of the filtrate tank 9.
And a condensate pump 4 is also arranged between the condensate tank 3 and the distillation kettle rectifying tower.
The operation was carried out in the same manner as in example 1.
Example 5
An organosilicon sludge treatment system, comprising: a slurry residue steaming and drying kettle 1, a condenser 2, a condensate tank 3, a tail gas washing tower 5, a slurry residue hydrolysis tank 6, a filter press 8 and a filtrate tank 9; the gas outlet of the slurry residue steaming and drying kettle 1 is connected with the gas inlet of a distillation kettle rectifying tower, the gas outlet of the distillation kettle rectifying tower is connected with the gas inlet of a condenser 2, the liquid outlet of the condenser 2 is respectively connected with the liquid inlet of a condensate tank 3 and the liquid inlet of a slurry residue hydrolysis tank 6, and the gas outlet of the condenser 2 is connected with the gas inlet of a tail gas washing tower 5; the discharge hole of the slurry residue steaming and drying kettle 1 is connected with the feed inlet of the slurry residue hydrolysis tank 6, the liquid outlet of the slurry residue hydrolysis tank 6 is connected with the liquid inlet of the filter press 8, and the liquid outlet of the filter press 8 is connected with the liquid inlet of the filtrate tank 9.
And a discharge hole of the filter press 8 is connected with a copper extraction device.
The operation was carried out in the same manner as in example 1.
Example 6
An organosilicon sludge treatment system, comprising: a slurry residue steaming and drying kettle 1, a condenser 2, a condensate tank 3, a tail gas washing tower 5, a slurry residue hydrolysis tank 6, a filter press 8 and a filtrate tank 9; the gas outlet of the slurry residue steaming and drying kettle 1 is connected with the gas inlet of a distillation kettle rectifying tower, the gas outlet of the distillation kettle rectifying tower is connected with the gas inlet of a condenser 2, the liquid outlet of the condenser 2 is respectively connected with the liquid inlet of a condensate tank 3 and the liquid inlet of a slurry residue hydrolysis tank 6, and the gas outlet of the condenser 2 is connected with the gas inlet of a tail gas washing tower 5; the discharge hole of the slurry residue steaming and drying kettle 1 is connected with the feed inlet of the slurry residue hydrolysis tank 6, the liquid outlet of the slurry residue hydrolysis tank 6 is connected with the liquid inlet of the filter press 8, and the liquid outlet of the filter press 8 is connected with the liquid inlet of the filtrate tank 9.
The liquid outlet of the filtrate tank 9 is also connected with the liquid inlet of the slurry residue hydrolysis tank 6.
The operation was carried out in the same manner as in example 1.
Example 7
An organosilicon sludge treatment system, comprising: a slurry residue steaming and drying kettle 1, a condenser 2, a condensate tank 3, a tail gas washing tower 5, a slurry residue hydrolysis tank 6, a filter press 8 and a filtrate tank 9; the gas outlet of the slurry residue steaming and drying kettle 1 is connected with the gas inlet of a distillation kettle rectifying tower, the gas outlet of the distillation kettle rectifying tower is connected with the gas inlet of a condenser 2, the liquid outlet of the condenser 2 is respectively connected with the liquid inlet of a condensate tank 3 and the liquid inlet of a slurry residue hydrolysis tank 6, and the gas outlet of the condenser 2 is connected with the gas inlet of a tail gas washing tower 5; the discharge hole of the slurry residue steaming and drying kettle 1 is connected with the feed inlet of the slurry residue hydrolysis tank 6, the liquid outlet of the slurry residue hydrolysis tank 6 is connected with the liquid inlet of the filter press 8, and the liquid outlet of the filter press 8 is connected with the liquid inlet of the filtrate tank 9.
And a filtrate pump 10 is arranged between the liquid outlet of the filtrate tank 9 and the liquid inlet of the slurry residue hydrolysis tank 6.
The operation was carried out in the same manner as in example 1.
Example 8
An organosilicon sludge treatment system, comprising: a slurry residue steaming and drying kettle 1, a condenser 2, a condensate tank 3, a tail gas washing tower 5, a slurry residue hydrolysis tank 6, a filter press 8 and a filtrate tank 9; the gas outlet of the slurry residue steaming and drying kettle 1 is connected with the gas inlet of a distillation kettle rectifying tower, the gas outlet of the distillation kettle rectifying tower is connected with the gas inlet of a condenser 2, the liquid outlet of the condenser 2 is respectively connected with the liquid inlet of a condensate tank 3 and the liquid inlet of a slurry residue hydrolysis tank 6, and the gas outlet of the condenser 2 is connected with the gas inlet of a tail gas washing tower 5; the discharge hole of the slurry residue steaming and drying kettle 1 is connected with the feed inlet of the slurry residue hydrolysis tank 6, the liquid outlet of the slurry residue hydrolysis tank 6 is connected with the liquid inlet of the filter press 8, and the liquid outlet of the filter press 8 is connected with the liquid inlet of the filtrate tank 9.
A slurry pump 7 is arranged between the liquid outlet of the slurry-residue hydrolysis tank 6 and the liquid inlet of the filter press 8.
The operation was carried out in the same manner as in example 1.
It should be noted that the above-mentioned embodiments are only preferred embodiments of the present invention, and the present invention is not limited thereto, and although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications and equivalents can be made in the technical solutions described in the foregoing embodiments, or equivalents thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. An organosilicon thick liquid sediment processing system which characterized in that includes: a pulp residue steaming and drying kettle (1), a condenser (2), a condensate tank (3), a tail gas washing tower (5), a pulp residue hydrolysis tank (6), a filter press (8) and a filtrate tank (9); the gas outlet of the slurry residue steaming and drying kettle (1) is connected with the gas inlet of a distillation kettle rectifying tower, the gas outlet of the distillation kettle rectifying tower is connected with the gas inlet of a condenser (2), the liquid outlet of the condenser (2) is respectively connected with the liquid inlet of a condensate tank (3) and the liquid inlet of a slurry residue hydrolysis tank (6), and the gas outlet of the condenser (2) is connected with the gas inlet of a tail gas washing tower (5); the discharge hole of the slurry residue steaming and drying kettle (1) is connected with the feed inlet of the slurry residue hydrolysis tank (6), the liquid outlet of the slurry residue hydrolysis tank (6) is connected with the liquid inlet of the filter press (8), and the liquid outlet of the filter press (8) is connected with the liquid inlet of the filtrate tank (9).
2. The organosilicon slurry residue processing system according to claim 1, wherein the liquid outlet of the condensate tank (3) is connected with the liquid inlet of the distillation still rectifying tower.
3. The organosilicon slurry residue processing system according to claim 1, wherein a condensate pump (4) is further arranged between the condensate tank (3) and the distillation still rectifying tower.
4. The organosilicon slurry residue treatment system according to claim 1, wherein the discharge port of the filter press (8) is connected to a copper extraction device.
5. The organosilicon slurry slag treatment system according to claim 1, wherein the liquid outlet of the filtrate tank (9) is further connected with the liquid inlet of the slurry slag hydrolysis tank (6).
6. The organosilicon slurry slag treatment system according to claim 5, wherein a filtrate pump (10) is further arranged between the liquid outlet of the filtrate tank (9) and the liquid inlet of the slurry slag hydrolysis tank (6).
7. The organosilicon slurry slag treatment system according to claim 5, wherein a slurry pump (7) is arranged between the liquid outlet of the slurry slag hydrolysis tank (6) and the liquid inlet of the filter press (8).
8. The method for treating the organic silicon slurry slag is characterized by comprising the following steps:
heating and evaporating slurry slag in the production process of organic silicon to generate gas and solid slag;
washing and condensing the gas to obtain synthetic high boiling point;
mixing the solid slag with acid liquor for hydrolysis, and performing filter pressing on the reacted slurry to obtain the acid liquor and hydrolyzed solid slag;
carrying out copper extraction treatment on the hydrolyzed solid slag
And (4) sending the acid liquor to a hydrochloric acid treatment unit, and mixing the acid liquor with water to be used as the slurry residue hydrolysate for recycling.
9. The method of treating organosilicon sludge according to claim 8, wherein a part of the synthesized high-boiling fraction is used as reflux to wash the boil-off gas, and the other part is used as a high-boiling cracking raw material.
10. The method for treating organosilicon residues according to claim 8, wherein the evaporation temperature is controlled at 200-300 ℃.
CN202111455208.9A 2021-12-01 2021-12-01 Organic silicon slurry residue hydrolysis treatment process and resource recycling method Pending CN114262792A (en)

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008533293A (en) * 2005-03-22 2008-08-21 アングロ オペレーションズ リミティッド Leaching method in the presence of hydrochloric acid to recover valuable metals from ora
DE102010003108A1 (en) * 2010-03-22 2011-09-22 Wacker Chemie Ag Silaoxacyclen
CN105037414A (en) * 2015-07-29 2015-11-11 湖北兴瑞化工有限公司 Method and device for recovering efficient high-boiling substance from organic silicon residue slurry
CN106220666A (en) * 2016-07-18 2016-12-14 聊城市鲁西化工工程设计有限责任公司 The processing system of a kind of organic silicon slurry slag and processing method
CN108558928A (en) * 2018-05-09 2018-09-21 成都斯力康科技股份有限公司 A kind of method and apparatus of organosilicon slag slurry synthetical recovery processing
CN109897058A (en) * 2019-02-28 2019-06-18 天津大学 A kind of organic silicon slurry slag processing system and treatment process
CN210701661U (en) * 2019-10-08 2020-06-09 内蒙古鄂尔多斯多晶硅业有限公司 Cold hydrogenation slag slurry treatment system
CN112321626A (en) * 2020-11-10 2021-02-05 云南能投硅材科技发展有限公司 Method for treating organic silicon slag slurry

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008533293A (en) * 2005-03-22 2008-08-21 アングロ オペレーションズ リミティッド Leaching method in the presence of hydrochloric acid to recover valuable metals from ora
DE102010003108A1 (en) * 2010-03-22 2011-09-22 Wacker Chemie Ag Silaoxacyclen
CN105037414A (en) * 2015-07-29 2015-11-11 湖北兴瑞化工有限公司 Method and device for recovering efficient high-boiling substance from organic silicon residue slurry
CN106220666A (en) * 2016-07-18 2016-12-14 聊城市鲁西化工工程设计有限责任公司 The processing system of a kind of organic silicon slurry slag and processing method
CN108558928A (en) * 2018-05-09 2018-09-21 成都斯力康科技股份有限公司 A kind of method and apparatus of organosilicon slag slurry synthetical recovery processing
CN109897058A (en) * 2019-02-28 2019-06-18 天津大学 A kind of organic silicon slurry slag processing system and treatment process
CN210701661U (en) * 2019-10-08 2020-06-09 内蒙古鄂尔多斯多晶硅业有限公司 Cold hydrogenation slag slurry treatment system
CN112321626A (en) * 2020-11-10 2021-02-05 云南能投硅材科技发展有限公司 Method for treating organic silicon slag slurry

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