CN113603091B - Resource utilization method of cold hydrogenation slag slurry dry powder - Google Patents
Resource utilization method of cold hydrogenation slag slurry dry powder Download PDFInfo
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- 239000002002 slurry Substances 0.000 title claims abstract description 58
- 238000005984 hydrogenation reaction Methods 0.000 title claims abstract description 55
- 239000000843 powder Substances 0.000 title claims abstract description 49
- 239000002893 slag Substances 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 34
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000007788 liquid Substances 0.000 claims abstract description 36
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 27
- 239000000413 hydrolysate Substances 0.000 claims abstract description 21
- 239000012629 purifying agent Substances 0.000 claims abstract description 21
- 239000000126 substance Substances 0.000 claims abstract description 21
- 238000001704 evaporation Methods 0.000 claims abstract description 17
- 230000008020 evaporation Effects 0.000 claims abstract description 17
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 16
- 238000000926 separation method Methods 0.000 claims abstract description 13
- 239000007787 solid Substances 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 7
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 30
- 229910001510 metal chloride Inorganic materials 0.000 claims description 18
- 238000006116 polymerization reaction Methods 0.000 claims description 18
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 14
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 14
- 229910052710 silicon Inorganic materials 0.000 claims description 13
- 239000010703 silicon Substances 0.000 claims description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 12
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 8
- 230000003301 hydrolyzing effect Effects 0.000 claims description 7
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 4
- 239000001110 calcium chloride Substances 0.000 claims description 4
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 4
- 229960002089 ferrous chloride Drugs 0.000 claims description 4
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 4
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 4
- 229910052755 nonmetal Inorganic materials 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000002351 wastewater Substances 0.000 abstract description 12
- 229910021420 polycrystalline silicon Inorganic materials 0.000 abstract description 10
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 abstract description 7
- 239000000047 product Substances 0.000 abstract description 5
- 238000011084 recovery Methods 0.000 abstract description 5
- 238000000746 purification Methods 0.000 abstract description 4
- 229920005591 polysilicon Polymers 0.000 abstract description 3
- 238000004065 wastewater treatment Methods 0.000 abstract description 3
- 239000005046 Chlorosilane Substances 0.000 description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 10
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical class Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 6
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 5
- 238000006460 hydrolysis reaction Methods 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 4
- 229960004887 ferric hydroxide Drugs 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000006386 neutralization reaction Methods 0.000 description 3
- 230000000379 polymerizing effect Effects 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 239000011555 saturated liquid Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 108010009736 Protein Hydrolysates Proteins 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- SLLGVCUQYRMELA-UHFFFAOYSA-N chlorosilicon Chemical compound Cl[Si] SLLGVCUQYRMELA-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 239000012263 liquid product Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/021—Preparation
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The invention relates to a resource utilization method of cold hydrogenation slag slurry dry powder, belonging to the technical field of cold hydrogenation treatment of polycrystalline silicon. The invention aims to provide a low-cost resource utilization method of cold hydrogenation slag slurry dry powder, which can realize zero discharge of waste water. Mixing cold hydrogenation slag slurry dry powder with water, and reacting at 40-110 ℃ to obtain a hydrolysate containing hydroxyl; heating the hydrolysate containing hydroxyl to 150-250 ℃ under pressurization, carrying out flash evaporation, and then carrying out solid-liquid separation to obtain solid silicon powder and liquid water purifying agent. The high-efficiency liquid water purifying agent and the silicon powder with the purity of more than 90 percent can be prepared by the method, and the high-efficiency liquid water purifying agent can be widely applied to the fields of power plant wastewater purification, chemical plant wastewater treatment and the like, can effectively remove suspended substances in water, and can reduce COD, BOD and ammonia nitrogen. The silicon powder can be directly sold as a product, so that zero discharge of the polysilicon slag slurry is realized, the dry powder recovery cost of the cold hydrogenation slag slurry is reduced, and the method is simple, low in cost and environment-friendly.
Description
Technical Field
The invention relates to a resource utilization method of cold hydrogenation slag slurry dry powder, belonging to the technical field of cold hydrogenation treatment of polycrystalline silicon.
Background
In the production of polycrystalline silicon, 1.05-1.07 tons of industrial silicon are generally consumed per ton of polycrystalline silicon. According to the principle of mass conservation, metal elements (mainly iron, aluminum and calcium) in the silicon powder are finally enriched in the cold hydrogenation slurry, and more than 4000 tons of metal chloride are generated per 10 ten thousand tons of polysilicon.
The cold hydrogenation slag slurry comprises the following main components: si, siCl 4 、SiHCl 3 、SiH 2 Cl 2 Polychlorosilanes, alCl 3 And other chlorides, of which silicon and chlorosilanes account for the most part. The cold hydrogenation slurry is used as an inevitable material flow in the production of the polycrystalline silicon, and because the cold hydrogenation slurry is harmful to the environment and the chlorosilane has a certain recovery value, the recycling of the cold hydrogenation slurry has important significance for the whole polycrystalline silicon production process.
The cold hydrogenation slag slurry treatment process completes the separation of chlorosilane and silicon powder to obtain dry silicon powder, namely the cold hydrogenation slag slurry dry powder has the total content of residual chlorosilane in the silicon powder not higher than 2.5 percent, the main component of the silicon powder is silicon, and simultaneously contains a large amount of acid metal chlorides, and the existence of the metal chlorides ensures that the dry powder cannot be directly utilized and needs further treatment.
The prior art generally uses lye to neutralize the part of the metal chloride-containing dry powder. For example, chinese patent application No. CN 201410199410.3 discloses a method and an apparatus for treating slurry in a cold hydrogenation process, in which solid and liquid in the slurry generated in the cold hydrogenation process are separated by preliminary evaporation, chlorosilane gas is separated, and the chlorosilane gas is condensed and recovered; and (3) performing hydrolysis neutralization reaction on the residual slurry after chlorosilane gas is separated by evaporation through alkali liquor, and discharging a solid-liquid mixture after the neutralization reaction. The treatment cost is high due to the adoption of alkali liquor neutralization, for example, according to the measurement of 10 ten thousand tons of capacity, 30 percent of alkali liquor is consumed for neutralizing the dry powder, more than 8000 tons of the dry powder are consumed, about 50000 tons of salt-containing wastewater is generated, about 5000 tons of waste residue is generated, and the treatment cost is more than 1000 ten thousand yuan.
Disclosure of Invention
Aiming at the defects, the invention provides a low-cost recycling method for cold hydrogenation slag slurry dry powder, which can realize recycling.
The resource utilization method of the cold hydrogenation slag slurry dry powder comprises the following steps:
a. and (3) hydrolytic polymerization: mixing the cold hydrogenation slag slurry dry powder with water, and reacting at 40-110 ℃ to obtain a hydrolysate containing hydroxyl;
b. flash polymerization: heating the hydrolysate containing hydroxyl to 150-250 ℃ under pressurization, and then carrying out flash evaporation to obtain a flash-evaporated substance;
c. solid-liquid separation: and (3) performing solid-liquid separation on the flash-evaporated substance to obtain solid silicon powder and liquid water purifying agent.
In one embodiment of the present invention, the composition of the cold hydrogenation slag slurry dry powder is: 1-94 wt% of silicon, and the balance of chloride, wherein the chloride comprises metal chloride and non-metal chloride.
In one embodiment of the present invention, the metal chloride includes at least one of aluminum chloride, ferrous chloride, ferric chloride, calcium chloride, and magnesium chloride.
In one embodiment of the invention, the non-metallic chloride comprises a polychlorosilane.
In one embodiment of the invention, the metal chloride comprises aluminum chloride and ferric chloride, and the total weight of the aluminum chloride and the ferric chloride is more than 80% of the total weight of the metal chloride.
In one embodiment of the invention, the content of the polychlorosilane is less than 2.5% of the dry powder weight of the cold hydrogenation slag slurry.
In one embodiment of the invention, in the step a, the mass volume ratio of the dry powder of the cold hydrogenation slag slurry to the water is 0.1-0.5 g/mL.
In one embodiment of the present invention, in step a, the reaction is carried out at 80 to 110 ℃.
In one embodiment of the invention, in the step b, the pressure after pressurization before flash evaporation is 0.1-5.0 MPa.
In one embodiment of the invention, in the step b, the pressure after pressurization before flash evaporation is 0.5 to 4.0MPa.
Compared with the prior art, the invention has the following beneficial effects:
the method of the invention utilizes the dry powder of the cold hydrogenation slag pulp to prepare the high-efficiency liquid water purifying agent and the silicon powder with the purity of more than 90 percent, and the high-efficiency liquid water purifying agent can be widely applied to the fields of power plant wastewater purification, chemical plant wastewater treatment and the like, can effectively remove suspended substances in water, and can reduce COD, BOD and ammonia nitrogen. The silicon powder can be directly sold as a product, so that zero discharge of the polysilicon slag slurry is realized, the dry powder recovery cost of the cold hydrogenation slag slurry is reduced, and the method is simple, low in cost and environment-friendly.
Detailed Description
The invention relates to a resource utilization method of cold hydrogenation slag slurry dry powder, which comprises the following steps:
a. and (3) hydrolytic polymerization: mixing the cold hydrogenation slag slurry dry powder with water, and reacting at 40-110 ℃ to obtain a hydrolysate containing hydroxyl;
b. flash polymerization: heating the hydrolysate containing hydroxyl to 150-250 ℃ under pressurization, and then carrying out flash evaporation to remove part of hydrogen chloride to obtain a flash-evaporated substance;
c. solid-liquid separation: and (3) performing solid-liquid separation on the flash-evaporated substance to obtain solid silicon powder and liquid water purifying agent.
The resource utilization method of the cold hydrogenation slag slurry dry powder does not need to add a large amount of medicament, and has lower cost. The dry powder obtained by dry recovery is utilized to prepare the high-efficiency liquid water purifying agent, and the agent can be widely applied to the fields of power plant wastewater purification, chemical plant wastewater treatment and the like, can effectively remove suspended substances in water, and can reduce COD, BOD and ammonia nitrogen. The product quality reaches or even exceeds the national standard. In addition, the purity of the silicon powder recovered by the method reaches over 90 percent, and the silicon powder can be directly sold as a product, so that the green environmental protection and the best use of the materials are realized in the true sense, and the global zero discharge process of the polycrystalline silicon slag slurry is initiated.
The dry powder of the cold hydrogenation slag slurry is obtained by recovering chlorosilane from the cold hydrogenation slag slurry. Recovery methods commonly used in the art are suitable for use in the present invention. In one embodiment of the present invention, the composition of the cold hydrogenation slag slurry dry powder is: 1-94 wt% of silicon, and the balance of chloride, wherein the chloride comprises metal chloride and non-metal chloride.
In one embodiment of the present invention, the metal chloride includes at least one of aluminum chloride, ferrous chloride, ferric chloride, calcium chloride, and magnesium chloride.
In one embodiment of the invention, the non-metallic chloride comprises a polychlorosilane.
In one embodiment of the invention, the metal chloride comprises aluminum chloride and ferric chloride, and the total weight of the aluminum chloride and the ferric chloride is greater than 80% of the total weight of the metal chloride.
In one embodiment of the invention, the content of the polychlorosilane accounts for less than 2.5 percent of the weight of the cold hydrogenation slag slurry dry powder.
In the method, the step a is mainly hydrolytic polymerization, and the step a is mainly hydrolysis reaction of aluminum chloride, ferric chloride and polychlorosilane to obtain hydrolysate containing hydroxyl.
The amount of water added may be any amount conventionally used in the art. In one embodiment of the invention, in the step a, the mass volume ratio of the dry powder of the cold hydrogenation slag slurry to the water is 0.1-0.5 g/mL.
In one embodiment of the present invention, in step a, the reaction is carried out at 80 to 110 ℃.
And b, performing flash polymerization, namely performing flash evaporation after pressurizing and heating the hydrolysate, and removing part of hydrogen chloride, wherein the hydrolysate is further polymerized, and the polymerization reaction mainly occurs among ferric hydroxide, aluminum hydroxide and orthosilicic acid to form a multi-element polymer containing iron, aluminum and silicon.
After the saturated liquid that has flashed to high pressure enters the relatively low pressure vessel, the saturated liquid becomes a part of the saturated vapor and saturated liquid at the vessel pressure due to the sudden drop in pressure. The flash evaporation aims at removing hydrogen chloride, and a flash evaporator can be adopted, and the hydrolysate can be directly pressurized and heated and then added into the flash evaporator for flash evaporation. The flash evaporator may employ a flash evaporation apparatus commonly used in the art.
In one embodiment of the invention, in step b, the pressure after pressurization before flash evaporation is 0.1-5.0 MPa. Namely, the hydrolysate containing hydroxyl is heated to 150 to 250 ℃ under the pressure of 0.1 to 5.0MPa.
In one embodiment of the invention, in the step b, the pressure after pressurization before flash evaporation is 0.5 to 4.0MPa.
And c, performing solid-liquid separation, wherein the obtained solid is silicon powder, and the obtained liquid is a liquid water purifying agent. The solid-liquid separation method commonly used in the invention is applicable to the invention, such as filtration, centrifugation and the like.
The purity of the obtained silicon powder is higher than 90%, and the silicon powder can be directly sold as a product. The liquid water purifying agent can be used for purifying power plant wastewater, treating chemical plant wastewater and the like, removing suspended substances in water, and reducing COD, BOD and ammonia nitrogen.
The following examples are provided to further illustrate the embodiments of the present invention and are not intended to limit the scope of the present invention. The cold hydrogenation slag slurry dry powder in the embodiment is prepared by the following method: and (3) primarily separating the slurry from the cold hydrogenation section by using a stirring kettle to obtain concentrated silicon slurry, drying the silicon slurry in a dryer, recovering chlorosilane in the silicon powder in the drying process, and finally controlling the chlorosilane in the silicon powder to be below 2.5%.
The dry powder components are detected, wherein the silicon content is 70%, the polychlorosilane is 0.5%, and the rest is metal chlorides such as aluminum chloride, ferrous chloride, calcium chloride, magnesium chloride and the like, wherein the aluminum chloride and the ferric chloride account for 80% of the total content of the metal chlorides.
Example 1
The resource utilization method of the cold hydrogenation slag slurry dry powder comprises the following steps:
a. and (3) hydrolytic polymerization: mixing 500g of cold hydrogenation slag slurry dry powder with 1000mL of water, reacting at 100 ℃, and carrying out hydrolysis reaction on aluminum chloride, ferric chloride and polychlorosilane to obtain a hydrolysate containing hydroxyl;
b. flash polymerization: heating the hydrolysate containing hydroxyl to 150 ℃ under pressurization (pressure of 0.5 MPa), then entering a flash evaporator, removing part of hydrogen chloride in the flash evaporator, and further polymerizing the hydrolysate to obtain a flash evaporated substance; the polymerization occurs among ferric hydroxide, aluminum hydroxide and orthosilicic acid to form a multi-polymer containing iron, aluminum and silicon;
c. and (3) filtering and separating: and (4) carrying out solid-liquid separation on the flash-evaporated substance to obtain 400g of solid silicon powder and 750mL of liquid water purifying agent.
The purity of the silicon powder was measured and found to be 92.5%.
Example 2
The resource utilization method of the cold hydrogenation slurry dry powder comprises the following steps:
a. hydrolytic polymerization: mixing 500g of cold hydrogenation slag slurry dry powder with 1500mL of water, reacting at 80 ℃, and carrying out hydrolysis reaction on aluminum chloride, ferric chloride and polychlorosilane to obtain a hydrolysate containing hydroxyl;
b. flash polymerization: heating the hydrolysate containing hydroxyl to 200 ℃ under pressurization (pressure of 1.5 MPa), then entering a flash evaporator, removing part of hydrogen chloride in the flash evaporator, and further polymerizing the hydrolysate to obtain a flash evaporated substance; the polymerization occurs among ferric hydroxide, aluminum hydroxide and orthosilicic acid to form a multi-polymer containing iron, aluminum and silicon;
c. and (3) filtering and separating: and performing solid-liquid separation on the substance after flash evaporation to obtain 395g of solid silicon powder and 850mL of liquid water purifying agent.
The purity of the silicon powder was measured and found to be 93.6%.
Example 3
The resource utilization method of the cold hydrogenation slurry dry powder comprises the following steps:
a. hydrolytic polymerization: mixing 500g of cold hydrogenation slag slurry dry powder with 2000mL of water, reacting at 110 ℃, and carrying out hydrolysis reaction on aluminum chloride, ferric chloride and polychlorosilane to obtain a hydrolysate containing hydroxyl;
b. flash polymerization: heating the hydrolysate containing hydroxyl to 250 ℃ under pressurization (pressure of 4 MPa), then entering a flash evaporator, removing part of hydrogen chloride in the flash evaporator, and further polymerizing the hydrolysate to obtain a flash evaporated substance; the polymerization is carried out among ferric hydroxide, aluminum hydroxide and orthosilicic acid to form a multi-component polymer containing iron, aluminum and silicon;
c. filtering and separating: and (4) carrying out solid-liquid separation on the flash-evaporated substance to obtain 405g of solid silicon powder and 900mL of liquid water purifying agent.
The purity of the silicon powder was measured and found to be 92.3%.
The liquid water purifying agents of the embodiments 1 to 3 are adopted to treat the wastewater of the power plant, the water quality before treatment is 10000mg/L of COD, 9500mg/L of BOD, 2000mg/L of ammonia nitrogen and 30000mg/L of suspended matters, and the details are shown in the table 1.
The treatment method comprises the following steps: taking 1500mL of wastewater, adding liquid water purifying agent with the addition of 6.5 ten-thousandth of the volume of the wastewater, namely 0.975mL, stirring for 10 minutes, and standing.
The water quality after the purification treatment is shown in Table 1.
TABLE 1
| Numbering | COD(mg/L) | Ammonia nitrogen (mg/L) | Suspended substance (mg/L) |
| Quality of wastewater before treatment | 10000 | 2000 | 30000 |
| Example 1 Water quality after treatment with liquid Water purifying agent | 500 | 50 | 2 |
| Example 2 Water quality after treatment with liquid Water purifying agent | 650 | 55 | 3.1 |
| Example 3 Water quality after treatment with liquid Water purifying agent | 350 | 45 | 2.9 |
Therefore, the method can successfully obtain the silicon powder with higher purity and the liquid product which can be used as the purifying agent, and the liquid purifying agent can greatly reduce the content of COD, ammonia nitrogen and suspended matters in the wastewater.
Claims (9)
1. The resource utilization method of the cold hydrogenation slag slurry dry powder is characterized by comprising the following steps:
a. and (3) hydrolytic polymerization: mixing the cold hydrogenation slag slurry dry powder with water, and reacting at 40-110 ℃ to obtain a hydrolysate containing hydroxyl;
b. flash polymerization: heating the hydrolysate containing hydroxyl to 150-250 ℃ under pressurization, and then carrying out flash evaporation to obtain a flash-evaporated substance;
c. solid-liquid separation: and (3) performing solid-liquid separation on the flash-evaporated substance, wherein the obtained solid is silicon powder, and the obtained liquid is a liquid water purifying agent.
2. The resource utilization method of the cold hydrogenation slag slurry dry powder according to claim 1, characterized in that: the cold hydrogenation slag slurry dry powder comprises the following components: 1-94 wt% of silicon and the balance of chloride, wherein the chloride comprises metal chloride and non-metal chloride.
3. The resource utilization method of the cold hydrogenation slag slurry dry powder according to claim 2, characterized in that: the metal chloride comprises at least one of aluminum chloride, ferrous chloride, ferric chloride, calcium chloride and magnesium chloride; the non-metal chloride comprises a polychlorosilane.
4. The resource utilization method of the cold hydrogenation slag slurry dry powder according to claim 3, characterized in that: the metal chloride comprises aluminum chloride and ferric chloride, and the total weight of the aluminum chloride and the ferric chloride accounts for more than 80% of the total weight of the metal chloride.
5. The resource utilization method of the cold hydrogenation slag slurry dry powder according to claim 3, characterized in that: the content of the polychlorosilane accounts for less than 2.5 percent of the weight of the dry powder of the cold hydrogenation slag slurry.
6. The resource utilization method of the cold hydrogenation slag slurry dry powder according to claim 1, characterized in that: in the step a, the mass volume ratio of the dry powder of the cold hydrogenation slag slurry to the water is 0.1-0.5 g/mL.
7. The resource utilization method of the cold hydrogenation slag slurry dry powder according to claim 1, characterized in that: in the step a, the reaction is carried out at the temperature of 80-110 ℃.
8. The resource utilization method of the cold hydrogenation slag slurry dry powder according to claim 1, characterized in that: in the step b, the pressure intensity after pressurization before flash evaporation is 0.1-5.0 MPa.
9. The resource utilization method of the cold hydrogenation slag slurry dry powder according to claim 8, characterized in that: in the step b, the pressure intensity after pressurization before flash evaporation is 0.5-4.0 MPa.
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| CN110950342A (en) * | 2019-11-29 | 2020-04-03 | 天华化工机械及自动化研究设计院有限公司 | Polysilicon slag slurry non-hydration treatment process |
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| US6916943B2 (en) * | 2002-12-16 | 2005-07-12 | Corning Incorporated | Supported metal catalysts |
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| CN103408023A (en) * | 2013-07-19 | 2013-11-27 | 中国恩菲工程技术有限公司 | Method and equipment for treatment of chlorosilane-containing waste liquid |
| CN106623370A (en) * | 2017-01-18 | 2017-05-10 | 山东省环境保护科学研究设计院 | Treatment process and system for organic silica mud |
| CN107628623A (en) * | 2017-09-29 | 2018-01-26 | 四川绿源聚能环保科技有限责任公司 | A kind of method for handling chlorosilane slurry raffinate |
| CN110950342A (en) * | 2019-11-29 | 2020-04-03 | 天华化工机械及自动化研究设计院有限公司 | Polysilicon slag slurry non-hydration treatment process |
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