CN114524569A - Waste water treatment device and process for production of polysiloxane microspheres - Google Patents
Waste water treatment device and process for production of polysiloxane microspheres Download PDFInfo
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- CN114524569A CN114524569A CN202210214819.2A CN202210214819A CN114524569A CN 114524569 A CN114524569 A CN 114524569A CN 202210214819 A CN202210214819 A CN 202210214819A CN 114524569 A CN114524569 A CN 114524569A
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- metal salt
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- polyorganosiloxane
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000004005 microsphere Substances 0.000 title claims abstract description 27
- 238000004065 wastewater treatment Methods 0.000 title claims abstract description 18
- -1 polysiloxane Polymers 0.000 title abstract description 9
- 229920001296 polysiloxane Polymers 0.000 title abstract description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 90
- 239000002351 wastewater Substances 0.000 claims abstract description 69
- 229910052751 metal Inorganic materials 0.000 claims abstract description 46
- 239000002184 metal Substances 0.000 claims abstract description 46
- 150000003839 salts Chemical class 0.000 claims abstract description 45
- 238000004821 distillation Methods 0.000 claims abstract description 30
- 239000007788 liquid Substances 0.000 claims abstract description 22
- 238000004062 sedimentation Methods 0.000 claims abstract description 22
- 239000002244 precipitate Substances 0.000 claims abstract description 20
- 238000000926 separation method Methods 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000011259 mixed solution Substances 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 238000001556 precipitation Methods 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims description 26
- 238000003860 storage Methods 0.000 claims description 25
- 238000002156 mixing Methods 0.000 claims description 21
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical group [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 20
- 239000007787 solid Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 10
- 239000001110 calcium chloride Substances 0.000 claims description 10
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 10
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 10
- 230000035484 reaction time Effects 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 5
- 238000011084 recovery Methods 0.000 abstract description 7
- 238000000605 extraction Methods 0.000 abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052799 carbon Inorganic materials 0.000 abstract description 4
- 239000003814 drug Substances 0.000 abstract description 3
- 238000004064 recycling Methods 0.000 abstract description 3
- 125000004122 cyclic group Chemical group 0.000 abstract 1
- 230000001502 supplementing effect Effects 0.000 abstract 1
- 238000010668 complexation reaction Methods 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 4
- 238000010170 biological method Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C31/00—Saturated compounds having hydroxy or O-metal groups bound to acyclic carbon atoms
- C07C31/02—Monohydroxylic acyclic alcohols
- C07C31/04—Methanol
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/38—Treatment of water, waste water, or sewage by centrifugal separation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5281—Installations for water purification using chemical agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
- C02F2103/38—Polymers
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/30—Fuel from waste, e.g. synthetic alcohol or diesel
Abstract
The invention provides a waste water treatment device and a process for producing polysiloxane microspheres, wherein the process comprises the following steps: firstly, adding metal salt into production wastewater to prepare a mixed solution of the metal salt and the production wastewater; secondly, introducing the prepared mixed solution of the metal salt production wastewater into a sedimentation tank, and performing complex reaction on the metal salt and the methanol in the production wastewater to generate precipitate; after precipitation, carrying out solid-liquid separation on the production wastewater in the precipitation tank, separating the precipitate from water, and collecting the precipitate; fourthly, distilling the precipitate, recycling crude methanol from the top of the distillation tower, and recycling metal salt from the bottom of the distillation tower. The invention realizes the extraction and recovery of low-content methanol in the wastewater, so that the methanol and metal salt can be recycled, and the pollution discharge is low; the method has the advantages of short treatment period, no need of supplementing carbon source, cyclic utilization of the added medicament, small distillation treatment capacity and low cost; the treated water can be recycled for the production of the polysiloxane microspheres, so that the cost is reduced.
Description
Technical Field
The invention relates to a treatment process of methanol-containing wastewater; in particular to a waste water treatment device and a waste water treatment process for the production of polyorganosiloxane microspheres.
Background
In the production process of the polyorganosiloxane microspheres by using trialkoxysilane as a raw material, a small amount of methanol is generated as a byproduct during hydrolysis of trialkoxysilane. The residual production wastewater after the production process contains methanol, and if the methanol is directly recycled, the chemical reaction balance is influenced, so that the yield is reduced; if the waste water is directly discharged, the waste water causes environmental pollution and can be discharged after being treated.
Because the content of the methanol in the wastewater is low, if the conventional rectification method is adopted to recover the methanol, the water treatment amount is large, and the production cost is high; if the biological method is adopted, a carbon source needs to be additionally supplemented, so that the cost is increased, and the treatment period is longer.
Disclosure of Invention
In order to solve the technical problem, the invention provides a waste water treatment device and a waste water treatment process for production of polyorganosiloxane microspheres.
The invention is realized by the following technical scheme.
The invention provides a waste water treatment device for production of polysiloxane microspheres, which comprises:
a waste water tank and a material storage tank;
the mixing kettle is used for mixing the materials from the waste water tank and the material storage tank, and conveying the mixed materials to the sedimentation tank;
the sedimentation tank is used for standing the mixed material from the mixing kettle;
the solid-liquid separation equipment is used for carrying out solid-liquid separation on the material from the sedimentation tank, the separated liquid part is conveyed to the water storage tank, and the solid-containing part is conveyed to the distillation tower;
the distillation tower is used for distilling the solid-containing part, and the material extracted from the top of the distillation tower is conveyed to a crude methanol storage tank.
And a metering pump is arranged between the waste water tank and the mixing kettle, and a powder metering pump is arranged between the storage tank and the mixing kettle.
The mixing kettle is arranged above the sedimentation tank.
And a pump is arranged between the sedimentation tank and the solid-liquid separation equipment.
The solid-liquid separation equipment is a screw centrifuge of the formula of \33253.
The method is characterized in that a pump is arranged between the formula screw centrifuge and the water storage tank, a slurry pump is arranged between the formula screw centrifuge and the distillation tower, and a 33253is arranged between the formula screw centrifuge and the distillation tower.
The bottom effluent of the distillation column is conveyed to a holding tank by a solids pump.
The invention provides a wastewater treatment process for production of polyorganosiloxane microspheres, which comprises the following steps:
firstly, adding metal salt into production wastewater to prepare a mixed solution of the metal salt and the production wastewater;
secondly, introducing the prepared mixed solution of the metal salt production wastewater into a sedimentation tank, and carrying out complex reaction on the metal salt and methanol in the production wastewater to generate precipitate;
after precipitation, carrying out solid-liquid separation on the production wastewater in the precipitation tank, separating the precipitate from water, and collecting the precipitate;
fourthly, distilling the precipitate, recovering crude methanol from the top of the distillation tower, and recovering metal salt from the bottom of the distillation tower.
The method comprises the following steps that (1-10) the mass ratio of metal salt to production wastewater is: 100.
and (3) preparing a mixed solution of the metal salt and the production wastewater, wherein the temperature is 5-35 ℃, the stirring speed is 50-300 rpm, and the stirring time is 5-30 min.
Preferably, the mass ratio of the metal salt to the production wastewater is (1-5): 100, preparing a mixed solution of the metal salt and the production wastewater, wherein the temperature is 15-25 ℃, the stirring speed is 50-100 rpm, and the stirring time is 5-10 min.
The metal salt is magnesium chloride or calcium chloride.
The magnesium chloride or the calcium chloride is in a solid powder state.
The mass percentage concentration of the magnesium chloride or the calcium chloride is 99-99.5%.
And step two, the temperature of the complexation reaction is 5-35 ℃, and the reaction time is 8-24 h.
Preferably, the temperature of the complexation reaction is 15-25 ℃, and the reaction time is 8-16 h.
And thirdly, performing solid-liquid separation on the production wastewater in the sedimentation tank, and using a 33253 ℃ spiral centrifuge.
The invention has the beneficial effects that:
the device is used for treating wastewater generated in the production of the polyorganosiloxane microspheres, realizes the extraction and recovery of low-content methanol in the wastewater, and has high recovery efficiency and short treatment period; the external material in the storage tank can be recycled, and the pollution emission is low; the distillation treatment capacity is small, and the energy consumption is low; the invention reduces the cost of wastewater treatment as a whole.
By adopting the process, the extraction and recovery of low-content methanol in the wastewater are realized, so that methanol and metal salt can be recycled, and the pollution emission is low; compared with a biological method, the treatment period is short, a carbon source does not need to be supplemented, an additional medicament can be recycled, and the cost is low; compared with a rectification method, the distillation treatment capacity is greatly reduced, and the energy consumption is low; the wastewater treatment cost is reduced as a whole. The treated water can be recycled for the production of the polysiloxane microspheres, thereby reducing the consumption of natural resources and lowering the cost.
Drawings
Fig. 1 is a schematic structural view of the present invention.
In the figure: 1-a wastewater tank; 2-a material storage tank; 3-mixing the mixture in a kettle; 4-a sedimentation tank; 5-solid-liquid separation equipment; 6-a water storage tank; 7-a distillation column; 8-crude methanol storage tank.
Detailed Description
The technical solution of the present invention is further described below, but the scope of the claimed invention is not limited to the described.
As shown in fig. 1:
the invention provides a waste water treatment device for production of polysiloxane microspheres, which comprises:
a waste water tank 1 and a material storage tank 2;
the mixing kettle 3 is used for mixing the materials from the waste water tank 1 and the material storage tank 2, and conveying the mixed materials to the sedimentation tank 4;
the sedimentation tank 4 is used for standing the mixed material from the mixing kettle 3;
the solid-liquid separation equipment 5 is used for carrying out solid-liquid separation on the material from the sedimentation tank 4, the separated liquid part is conveyed to the water storage tank 6, and the solid-containing part is conveyed to the distillation tower 7;
the distillation tower 7 is used for distilling the solid-containing part, and the extracted material at the top of the distillation tower 7 is conveyed to a crude methanol storage tank 8.
The principle is as follows: the waste water tank 1 is used for storing waste water containing methanol, namely waste water produced by polysiloxane microspheres, and the storage tank 2 is used for storing metal salt, such as magnesium chloride or calcium chloride; the wastewater and metal salt are conveyed to a mixing kettle 3 together for mixing, and then conveyed to a sedimentation tank 4, the metal salt and methanol in the wastewater generate a complex reaction to generate a precipitate, a solid-liquid separator separates water from the precipitate, and the water is conveyed to a water outlet tank and can be directly recycled for production of polyorganosiloxane microspheres; the precipitate (i.e. the solid-containing part) is separated by a rectifying tower, the extract at the top of the rectifying tower is crude methanol, the effluent at the bottom of the rectifying tower is metal salt, and the metal salt can be conveyed to a storage tank 2 for recycling.
The method is used for treating wastewater generated in the production of the polyorganosiloxane microspheres, realizes the extraction and recovery of low-content methanol in the wastewater, and has high recovery efficiency and short treatment period; the external material in the material storage tank 2 can be recycled, and the pollution emission is low; the distillation treatment capacity is small, and the energy consumption is low; the invention reduces the cost of wastewater treatment as a whole.
A metering pump is arranged between the waste water tank 1 and the mixing kettle 3, and a powder metering pump is arranged between the storage tank 2 and the mixing kettle 3. The mixing proportion of the waste water and the metal salt is convenient to control, the chemical reaction efficiency is high, and the treatment time is short.
The mixing kettle 3 is arranged above the sedimentation tank 4. The mixture can conveniently flow into the sedimentation tank 4 by gravity, and the energy is saved.
A pump is arranged between the sedimentation tank 4 and the solid-liquid separation equipment 5. The material after being precipitated is conveniently conveyed to the solid-liquid separation equipment 5 for separation, and the automation degree is high.
The solid-liquid separation equipment 5 is a screw centrifuge of the type of \33253.
The method is characterized in that a pump is arranged between the formula screw centrifuge and the water storage tank 6, a slurry pump is arranged between the formula screw centrifuge and the distillation tower 7, and the 33253is arranged between the formula screw centrifuge and the distillation tower 7. Is convenient for conveying water to the water storage tank 6 and conveying the precipitate to the distillation tower 7, realizes continuous reaction and has high treatment efficiency.
The bottom discharge of the distillation column 7 is conveyed to the storage tank 2 by means of a solids pump. The metal salt is convenient to recycle.
The invention provides a wastewater treatment process for production of polyorganosiloxane microspheres, which comprises the following steps:
firstly, adding metal salt into production wastewater to prepare a mixed solution of the metal salt and the production wastewater;
secondly, introducing the prepared mixed solution of the metal salt production wastewater into a sedimentation tank 4, and carrying out complex reaction on the metal salt and methanol in the production wastewater to generate precipitate;
after precipitation, carrying out solid-liquid separation on the production wastewater in the precipitation tank 4, separating the precipitate from water, and collecting the precipitate;
fourthly, distilling the precipitate, recovering crude methanol from the top of the distillation tower 7, and recovering metal salt from the bottom of the distillation tower 7.
By adopting the process, the extraction and recovery of low-content methanol in the wastewater are realized, so that methanol and metal salt can be recycled, and the pollution emission is low; compared with a biological method, the treatment period is short, a carbon source does not need to be supplemented, an additional medicament can be recycled, and the cost is low; compared with a rectification method, the distillation treatment capacity is greatly reduced, and the energy consumption is low; the wastewater treatment cost is reduced as a whole.
The method comprises the following steps that (1-10) the mass ratio of metal salt to production wastewater is: 100. under the mass ratio, the content of methanol in wastewater generated in the production of the polyorganosiloxane microspheres is considered, the chemical reaction efficiency is high at a chemical equilibrium point, and the treated water can be recycled for the production of the polyorganosiloxane microspheres, so that the consumption of natural resources is reduced, and the cost is reduced.
And (3) preparing a mixed solution of the metal salt and the production wastewater, wherein the temperature is 5-35 ℃, the stirring speed is 50-300 rpm, and the stirring time is 5-30 min. Under the preparation condition, the chemical reaction efficiency is high, and the metal salt ions can fully react.
Preferably, the mass ratio of the metal salt to the production wastewater is (1-5): 100, preparing a mixed solution of the metal salt and the production wastewater, wherein the temperature is 15-25 ℃, the stirring speed is 50-100 rpm, and the stirring time is 5-10 min.
The metal salt is magnesium chloride or calcium chloride.
The magnesium chloride or the calcium chloride is in a solid powder state. The mixing is convenient and sufficient, and the mixing time is reduced.
The mass percentage concentration of the magnesium chloride or the calcium chloride is 99-99.5%.
And step two, the temperature of the complexation reaction is 5-35 ℃, and the reaction time is 8-24 h. The chemical reaction efficiency is high, and the precipitation is sufficient and the separation is convenient in the time.
Preferably, the temperature of the complexation reaction is 15-25 ℃, and the reaction time is 8-16 h.
And step three, carrying out solid-liquid separation on the production wastewater in the sedimentation tank 4, and using a 33253or a spiral centrifuge.
Claims (10)
1. The utility model provides a waste water treatment device of polyorganosiloxane microballon production which characterized in that: the method comprises the following steps:
a waste water tank (1) and a material storage tank (2);
the mixing kettle (3) is used for mixing the materials from the waste water tank (1) and the material storage tank (2) and conveying the mixed materials to the sedimentation tank (4);
the sedimentation tank (4) is used for standing the mixed materials from the mixing kettle (3);
the solid-liquid separation equipment (5) is used for carrying out solid-liquid separation on the material from the sedimentation tank (4), the separated liquid part is conveyed to the water storage tank (6), and the solid-containing part is conveyed to the distillation tower (7);
the distillation tower (7) is used for distilling the solid-containing part, and the extracted material at the top of the distillation tower (7) is conveyed to a crude methanol storage tank (8).
2. A waste water treatment process for production of polyorganosiloxane microspheres is characterized in that: comprises the following steps of (a) carrying out,
firstly, adding metal salt into production wastewater to prepare a mixed solution of the metal salt and the production wastewater;
secondly, introducing the prepared mixed solution of the metal salt production wastewater into a sedimentation tank (4), and carrying out complex reaction on the metal salt and methanol in the production wastewater to generate precipitate;
after precipitation, carrying out solid-liquid separation on the production wastewater in the precipitation tank (4), separating the precipitate from water, and collecting the precipitate;
fourthly, distilling the precipitate, recovering crude methanol from the top of the distillation tower (7), and recovering metal salt from the bottom of the distillation tower (7).
3. The process for treating wastewater from the production of polyorganosiloxane microspheres according to claim 2, wherein: the method comprises the following steps that (1-10) the mass ratio of metal salt to production wastewater is: 100.
4. the process for treating wastewater from the production of polyorganosiloxane microspheres according to claim 3, wherein: and (3) preparing a mixed solution of the metal salt and the production wastewater, wherein the temperature is 5-35 ℃, the stirring speed is 50-300 rpm, and the stirring time is 5-30 min.
5. The process for treating wastewater from the production of polyorganosiloxane microspheres according to claim 4, wherein: the mass ratio of the metal salt to the production wastewater is (1-5): 100, preparing a mixed solution of the metal salt and the production wastewater, wherein the temperature is 15-25 ℃, the stirring speed is 50-100 rpm, and the stirring time is 5-10 min.
6. The waste water treatment process for producing polyorganosiloxane microspheres according to any one of claims 2 to 5, wherein: the metal salt is magnesium chloride or calcium chloride.
7. The process for treating wastewater from the production of polyorganosiloxane microspheres according to claim 6, wherein: the magnesium chloride or the calcium chloride is in a solid powder state.
8. The process for treating wastewater from the production of polyorganosiloxane microspheres according to claim 7, wherein: the mass percentage concentration of the magnesium chloride or the calcium chloride is 99-99.5%.
9. The process for treating wastewater from the production of polyorganosiloxane microspheres according to claim 2, wherein: and step two, the temperature of the complex reaction is 5-35 ℃, and the reaction time is 8-24 h.
10. The process for treating wastewater from the production of polyorganosiloxane microspheres according to claim 9, wherein: the temperature of the complex reaction is 15-25 ℃, and the reaction time is 8-16 h.
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