CN114409695A - Comprehensive utilization method of waste silicon powder in organic silicon monomer synthesis process - Google Patents
Comprehensive utilization method of waste silicon powder in organic silicon monomer synthesis process Download PDFInfo
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 172
- 239000011863 silicon-based powder Substances 0.000 title claims abstract description 165
- 239000002699 waste material Substances 0.000 title claims abstract description 109
- 238000000034 method Methods 0.000 title claims abstract description 59
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 43
- 239000010703 silicon Substances 0.000 title claims abstract description 43
- 239000000178 monomer Substances 0.000 title claims abstract description 40
- 230000008569 process Effects 0.000 title claims abstract description 37
- 230000015572 biosynthetic process Effects 0.000 title description 14
- 238000003786 synthesis reaction Methods 0.000 title description 14
- WCCJDBZJUYKDBF-UHFFFAOYSA-N copper silicon Chemical compound [Si].[Cu] WCCJDBZJUYKDBF-UHFFFAOYSA-N 0.000 claims abstract description 63
- 239000000463 material Substances 0.000 claims abstract description 54
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 claims abstract description 52
- 238000000926 separation method Methods 0.000 claims abstract description 52
- 239000002245 particle Substances 0.000 claims abstract description 50
- 230000003213 activating effect Effects 0.000 claims abstract description 43
- 238000006243 chemical reaction Methods 0.000 claims abstract description 37
- 239000000843 powder Substances 0.000 claims abstract description 36
- 238000003756 stirring Methods 0.000 claims abstract description 21
- 239000002253 acid Substances 0.000 claims abstract description 18
- 238000011084 recovery Methods 0.000 claims abstract description 16
- 238000002386 leaching Methods 0.000 claims abstract description 15
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 229910052751 metal Inorganic materials 0.000 claims abstract description 11
- 239000002184 metal Substances 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 9
- 239000011362 coarse particle Substances 0.000 claims abstract description 4
- 239000010949 copper Substances 0.000 claims description 39
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 38
- 230000004913 activation Effects 0.000 claims description 38
- 239000003795 chemical substances by application Substances 0.000 claims description 38
- 229910052802 copper Inorganic materials 0.000 claims description 38
- 239000000203 mixture Substances 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 23
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 21
- 238000006386 neutralization reaction Methods 0.000 claims description 21
- 239000011259 mixed solution Substances 0.000 claims description 20
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 17
- 229940050176 methyl chloride Drugs 0.000 claims description 17
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 16
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 16
- 238000003860 storage Methods 0.000 claims description 16
- 239000011701 zinc Substances 0.000 claims description 13
- 229910052725 zinc Inorganic materials 0.000 claims description 13
- YGZSVWMBUCGDCV-UHFFFAOYSA-N chloro(methyl)silane Chemical compound C[SiH2]Cl YGZSVWMBUCGDCV-UHFFFAOYSA-N 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 11
- 238000006073 displacement reaction Methods 0.000 claims description 10
- 239000003921 oil Substances 0.000 claims description 10
- 238000002791 soaking Methods 0.000 claims description 10
- 239000011882 ultra-fine particle Substances 0.000 claims description 10
- 239000011261 inert gas Substances 0.000 claims description 9
- 229910052718 tin Inorganic materials 0.000 claims description 9
- 239000011135 tin Substances 0.000 claims description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 8
- 239000001103 potassium chloride Substances 0.000 claims description 8
- 235000011164 potassium chloride Nutrition 0.000 claims description 8
- 239000011780 sodium chloride Substances 0.000 claims description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical group [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 2
- 239000003929 acidic solution Substances 0.000 claims 1
- 238000005243 fluidization Methods 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 6
- 238000010924 continuous production Methods 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 5
- 239000000428 dust Substances 0.000 abstract description 3
- 239000012190 activator Substances 0.000 abstract 1
- 230000003472 neutralizing effect Effects 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000000605 extraction Methods 0.000 description 4
- 229910021645 metal ion Inorganic materials 0.000 description 4
- 238000005554 pickling Methods 0.000 description 4
- 230000002035 prolonged effect Effects 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 230000036541 health Effects 0.000 description 3
- 238000004073 vulcanization Methods 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- NEHMKBQYUWJMIP-NJFSPNSNSA-N chloro(114C)methane Chemical compound [14CH3]Cl NEHMKBQYUWJMIP-NJFSPNSNSA-N 0.000 description 2
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/12—Organo silicon halides
- C07F7/16—Preparation thereof from silicon and halogenated hydrocarbons direct synthesis
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0065—Leaching or slurrying
- C22B15/0067—Leaching or slurrying with acids or salts thereof
- C22B15/0069—Leaching or slurrying with acids or salts thereof containing halogen
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0084—Treating solutions
- C22B15/0089—Treating solutions by chemical methods
- C22B15/0091—Treating solutions by chemical methods by cementation
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/20—Obtaining zinc otherwise than by distilling
- C22B19/22—Obtaining zinc otherwise than by distilling with leaching with acids
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/20—Obtaining zinc otherwise than by distilling
- C22B19/26—Refining solutions containing zinc values, e.g. obtained by leaching zinc ores
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/30—Obtaining zinc or zinc oxide from metallic residues or scraps
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B25/00—Obtaining tin
- C22B25/04—Obtaining tin by wet processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B25/00—Obtaining tin
- C22B25/06—Obtaining tin from scrap, especially tin scrap
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a comprehensive utilization method of waste silicon powder in the synthetic process of an organic silicon monomer, which comprises the following steps: activating and stirring: preparing the waste silicon powder, the waste silicon-copper contact and an activator into a silicon-copper powder activating material; ② reaction in a bed: carrying out a fluidization reaction on the copper silicon powder activating material and chloromethane in a fluidized bed reactor; thirdly, separation treatment: carrying out primary separation on gas-material mixed particles discharged from the top of the fluidized bed reactor, introducing coarse particles obtained by the primary separation into the fluidized bed reactor for continuous fluidized reaction, carrying out secondary separation on gas-material mixed particles obtained by the primary separation, and conveying dust-containing gas obtained by the secondary separation into a washing tower; leaching silicon powder: carrying out acid leaching and filtering on superfine particles obtained by secondary separation to obtain a metal product and a silicon powder leaching solution; silicon powder recovery: and neutralizing, acid washing and filtering the silicon powder leaching solution to obtain a silicon powder product. The invention has the advantages of simple process technology, high conversion rate of waste silicon powder and continuous production.
Description
Technical Field
The invention belongs to the technical field of comprehensive utilization of waste resources, and particularly relates to a comprehensive utilization method of waste silicon powder in an organic silicon monomer synthesis process.
Background
At present, the synthesis of the organosilicon monomer mainly adopts a direct method, i.e. methyl chloride and industrial silicon react in a fluidized state in a fluidized bed under the action of a catalyst to obtain a crude monomer taking dimethyl dichlorosilane ((CH3)2SiCl2) as a main body, in the process of the fluidized reaction of the methyl chloride and the industrial silicon, the industrial silicon presents a certain particle size distribution after being ground by a grinding machine, when methyl chloride gas mixes and blows industrial silicon powder upwards from the bottom of the fluidized bed, larger silicon powder particles cannot be taken out from the top of the fluidized bed due to the action of gravity and continuously react in the fluidized bed, and finer silicon powder particles are taken out by unreacted methyl chloride gas and the crude monomer. In the prior art, in order to improve the utilization rate of silicon powder, a cyclone separator is generally installed at an outlet of a fluidized bed, unreacted methyl chloride, coarse monomers and finer silicon powder particles are separated through the centrifugal separation effect of the cyclone separator, but in the cyclone separation process, because the finer silicon powder particles have finer particle sizes, a large part of fine silicon powder is still discharged along with gas-phase coarse monomers and methyl chloride, which causes waste, so that most organosilicon monomer synthesis manufacturers design and use two-stage cyclone separation equipment at the reaction rear end of the fluidized bed, industrial silicon powder separated by the first-stage cyclone separation equipment often has larger particle sizes and can be directly returned to the bed for use, and finer silicon powder particles separated by the second cyclone separation equipment are unrealistic to be returned to the industrial fluidized bed or directly returned to the furnace for use in the industrial silicon production process, on one hand, the silicon dioxide is easily oxidized and changed into silicon dioxide due to the fine particle size, and on the other hand, the fine silicon powder can be taken away by high-speed airflow in an industrial fluidized bed and a smelting process, so that the recycling effect and the purpose can not be achieved. Therefore, the direct discharge of the fine silicon powder separated by the secondary cyclone separation equipment not only pollutes the environment and causes certain harm to human health, but also needs to further process the fine silicon powder to ensure the resource environment and the human health, at present, the fine silicon powder is treated by landfill storage, such as hydraulic transportation to a sludge pond or storage in an open air area, the silicon powder accumulated in large quantity can cause waste of land resources, the second method is to extract copper from waste silicon copper contact containing Cu by an acid leaching method, but the acid leaching can cause environmental pollution, in another treatment method, the fine silicon powder is used in the fields of concrete, cement, refractory materials and the like, but in practical application, the use amount of the fine silicon powder is low due to the fact that the fine silicon powder of various manufacturers has different quality. Therefore, it is objectively needed to develop a comprehensive utilization method of waste silicon powder in the synthetic process of the organic silicon monomer, which has reasonable process, can improve the recovery and utilization rate of the silicon powder and can realize continuous mass production.
Disclosure of Invention
In order to solve the problems in the background art, the invention aims to provide the comprehensive utilization method of the waste silicon powder in the synthetic process of the organic silicon monomer, which has reasonable process, can improve the recovery rate of the silicon powder and realize continuous large-scale production.
The comprehensive utilization method of waste silicon powder in the synthetic process of the organic silicon monomer comprises the following steps:
activating and stirring: adding waste silicon powder and waste silicon copper contacts generated in the synthetic process of industrial-grade production organic silicon monomers into an activation tank, stirring to prepare a copper-silicon powder mixture with the copper content of 1-20%, then adding an activating agent into the activation tank, adding the activating agent according to the proportion of adding 0.0001-100 g of the activating agent per kilogram of the copper-silicon powder mixture, stirring and activating the copper-silicon powder mixture and the activating agent in the activation tank to prepare a silicon-copper powder activation material, and then conveying the silicon-copper powder activation material into a conveying tank through a conveying pipe;
② reaction in a bed: replacing a return bed reactor and all pipelines communicated with the return bed reactor by inert gas, introducing heat conduction oil into a heat exchange pipe of the return bed reactor, controlling the temperature in the return bed reactor to be 260-320 ℃ by utilizing the heat conduction oil, conveying a silicon-copper powder activated material in a sending tank into a fluidized bed reactor through a feeding pipe by utilizing a feeding pump, introducing methyl chloride into the fluidized bed reactor from the bottom of the activated bed reactor by utilizing a guide pipe, performing a fluidized reaction on the copper-silicon powder activated material and the methyl chloride in the fluidized bed reactor, and discharging gas-material mixed particles produced by the fluidized reaction from the top of the fluidized bed reactor;
thirdly, separation treatment: conveying the gas-material mixed particles discharged from the top of the fluidized bed reactor into a primary cyclone separator through a discharge pipe for primary separation, discharging the coarse particles with the particle size larger than 400 meshes obtained by the primary separation from the bottom of the primary cyclone separator into a storage tank, introducing the coarse particles into the fluidized bed reactor through a material returning pump and a material returning pipe for continuous fluidized reaction, conveying the gas-material mixed particles obtained by the primary separation into a secondary cyclone separator through a communicating pipe for secondary separation, discharging the dust-containing gas obtained by the secondary separation from the top of the secondary cyclone separator and conveying the dust-containing gas into a washing tower, and discharging the ultrafine particles with the particle size smaller than 1000 meshes obtained by the secondary separation from the bottom of the secondary cyclone separator and conveying the ultrafine particles into a fine powder storage tank;
leaching silicon powder: adding an acid solution into a fine powder storage tank filled with superfine particles, stirring and soaking to obtain a mixed solution, wherein the solid-to-liquid ratio of the superfine silicon powder particles to the acid solution is 1: 5-10 mL/g, adding reduced iron powder with the mass of 0.1-100 times of that of the mixed solution into the mixed solution for a displacement reaction after the soaking reaction is completed, and filtering and separating the mixed solution to obtain a metal product and a silicon powder leaching solution after the displacement reaction is completed; the metal product contains elements such as copper, zinc, tin and the like;
silicon powder recovery: and (4) conveying the silicon powder leachate obtained by separation in the step (iv) to a neutralization tank, adding an alkaline agent into the neutralization tank to neutralize the silicon powder leachate in the neutralization tank, and after the neutralization reaction is finished, pickling and filtering the neutralized and leached solid silicon powder again to obtain a silicon powder product.
The invention has the following beneficial effects: firstly, the waste silicon powder and the waste copper contact generated in the organic silicon synthesis process are activated by an activating agent, then the activated waste silicon powder and the activated waste copper contact are sent into a fluidized bed reactor, and are subjected to a fluidized reaction again by using chloromethane, so that the conversion rate of the silicon powder can be effectively improved through a further fluidized reaction, the aim of reusing the silicon powder is fulfilled, the reuse of the waste silicon powder is reduced, and the yield of methyl chlorosilane is improved; secondly, the invention adopts a secondary cyclone separation mode to separate and treat the waste silicon powder and the waste copper which are not completely reacted, so that the utilization rate of the waste silicon powder is greatly improved, the generation of the waste silicon powder is further reduced, and the phenomena of environmental pollution and damage to human health are avoided; thirdly, the invention separates and recycles the waste silicon powder after the secondary cyclone separation, and the copper and the waste silicon powder are recycled separately, thereby generating better economic benefit. In conclusion, the process technology is simple, the operation cost is low, and by utilizing the waste silicon powder and the waste silicon copper contacts in a grading manner, on one hand, the waste silicon powder and the waste silicon copper contacts with relatively large particle sizes are activated to regenerate organic silicon methyl monomers, so that the pressure of the fine silicon powder with relatively low activity returning to the bed is reduced in the aspect of industrial organic silicon methyl monomer synthesis, the operation efficiency of the large bed is improved, the synthesis efficiency of the whole organic silicon methyl monomer is improved, the start cycle of the large bed is prolonged, good production benefits can be brought to enterprises, meanwhile, the continuous production of the waste silicon powder and the waste copper contacts can be realized, and the process has good popularization and utilization values; on the other hand, valuable metal ions in the fine waste silicon powder and the waste silicon copper contact are subjected to reduction extraction, so that the pollution of the fine silicon powder and the waste copper contact to the environment and the damage to a human body are avoided, the resource utilization of the waste silicon powder and the waste copper contact is realized, the recovery rate of the waste copper is over 85 percent, and the recovery rate of the waste zinc is over 80 percent.
Drawings
FIG. 1 is a schematic structural view of the present invention;
in the figure: 1-an activation tank, 2-a conveying pipe, 3-a sending tank, 4-a return bed reactor, 5-a feeding pump, 6-a feeding pipe, 7-a guide pipe, 8-a discharging pipe, 9-a primary cyclone separator, 10-a storage tank, 11-a return pump, 12-a return pipe, 13-a communicating pipe, 14-a secondary cyclone separator, 15-a washing tower, 16-a fine powder storage tank and 17-a neutralization tank.
Detailed Description
The invention is further illustrated by the following description of embodiments and the accompanying drawings, without in any way limiting the invention, and any alterations or substitutions made on the basis of the teachings of the invention shall fall within the scope of protection of the invention.
Example 1
The method for comprehensively utilizing waste silicon powder in the synthetic process of the organic silicon monomer, which is described in the embodiment 1, comprises the following steps of:
activating and stirring: adding waste silicon powder and waste silicon copper contacts generated in the synthetic process of industrial-grade production organic silicon monomers into an activation tank 1, wherein a stirrer is arranged in the activation tank 1, stirring the waste silicon powder and the waste copper contacts by using the stirrer to prepare a copper-silicon powder mixture with the copper content of 1%, then adding an activating agent into the activation tank 1, and adding the activating agent according to the proportion of adding 0.0001g of the activating agent into each kilogram of the copper-silicon powder mixture, the activating agent is a mixture of tin powder, zinc powder, aluminum powder, sodium chloride and potassium chloride, the mass ratio of the tin powder to the zinc powder in the activating agent is 1:1, the content of the aluminum powder is less than 0.1wt.%, and the content of the sodium chloride and the potassium chloride is less than 50ppm, the activating agent is used for carrying out catalytic activation on the copper-silicon powder mixture, then stirring and activating the copper-silicon powder mixture and the activating agent in the activation tank 1 to prepare a silicon-copper powder activation material, and then conveying the silicon-copper powder activation material into a sending tank 3 through a conveying pipe 2;
② reaction in a bed: firstly replacing a return bed reactor 4 and all pipelines communicated with the return bed reactor 4 with inert gas, wherein the inert gas is argon, replacing the return bed reactor 4 and all pipelines with argon, so as to ensure the efficient contact of waste silicon powder in a fluidized bed reactor 4 and methyl chloride and improve the product quality of methyl chlorosilane, then introducing heat conduction oil into a heat exchange pipe of the return bed reactor 4, controlling the temperature in the return bed reactor 4 to be 260 ℃ by utilizing the heat conduction oil, controlling the reaction intensity of the waste silicon powder in the fluidized bed reactor 4 and the methyl chloride by controlling the temperature, further improving the utilization rate of the waste silicon powder while ensuring the product quality of the methyl chlorosilane, then conveying silicon-copper powder activated material in a sending tank 3 into the fluidized bed reactor 4 through a feeding pipe 6 by utilizing a feeding pump 5, and simultaneously introducing the methyl chloride into the fluidized bed reactor 4 from the bottom of an activated bed reactor 4 by utilizing a guide pipe 7 Carrying out a fluidization reaction on the copper silicon powder activation material and chloromethane in a fluidized bed reactor 4, wherein the feeding amount of the silicon copper powder activation material is controlled at 80kg/h, the feeding amount of the chloromethane is controlled at 320kg/h, gas-material mixed particles produced by the fluidization reaction are discharged from the top of the fluidized bed reactor 4, and the gas-material mixed particles contain methyl chlorosilane, silicon, copper, tin, zinc and other components;
thirdly, separation treatment: the gas-material mixed particles obtained by the first-stage separation are led into a second-stage cyclone separator 14 through a communicating pipe 13 for second-stage separation, the gas-material mixed particles obtained by the second-stage separation are discharged from the top of the second-stage cyclone separator 14 and are conveyed into a washing tower 15, and the ultrafine particles obtained by the second-stage separation and have the particle size of less than 1000 meshes are discharged from the bottom of the second-stage cyclone separator 14 and are conveyed into a fine powder storage tank 16, the performance of the superfine particle material can not meet the requirement of a vulcanization reaction, and the copper and the silicon powder are independently recovered through subsequent separation treatment;
leaching silicon powder: adding an acid solution into a fine powder storage tank 16 filled with ultrafine particles, stirring and soaking to obtain a mixed solution, wherein the acid solution is a hydrochloric acid solution with the concentration of 0.1-41 wt.%, the solid-to-liquid ratio of the ultrafine silicon powder particles to the acid solution is 1:5mL/g, adding reduced iron powder with the mass of 0.1 time of that of the mixed solution into the mixed solution for a displacement reaction after the soaking reaction is completed, and filtering and separating the mixed solution after the displacement reaction is completed to obtain a metal product and a silicon powder leaching solution; the metal product contains elements such as copper, zinc, tin and the like;
silicon powder recovery: and (4) conveying the silicon powder leachate obtained by separation in the step (iv) into a neutralization tank 17, adding an alkaline agent into the neutralization tank 17 to neutralize the silicon powder leachate in the neutralization tank 17, wherein the alkaline agent is sodium carbonate, and after the neutralization reaction is finished, pickling and filtering the neutralized and leached solid silicon powder again to obtain a silicon powder product.
The process of the embodiment 1 is simple in technology and low in operation cost, and by utilizing the waste silicon powder and the waste silicon copper contacts in a grading manner, on one hand, the waste silicon powder and the waste silicon copper contacts with relatively large particle sizes are activated to regenerate organic silicon methyl monomers, so that the bed returning pressure of the fine silicon powder with relatively low activity is reduced in the aspect of industrial-grade organic silicon methyl monomer synthesis, the operation efficiency of a large bed is improved, the whole organic silicon methyl monomer synthesis efficiency is improved, the start cycle of the large bed is prolonged, good production benefits can be brought to enterprises, meanwhile, the continuous production of the waste silicon powder and the waste silicon copper contacts can be realized, and the process has good popularization and utilization values; on the other hand, valuable metal ions in the fine waste silicon powder and the contact body are subjected to reduction extraction, so that the pollution of the fine silicon powder and the waste copper contact body to the environment and the damage to a human body are avoided, the resource utilization of the waste silicon powder and the waste copper contact body is realized, the recovery rate of the waste copper reaches 88.5.6%, and the recovery rate of the waste zinc reaches 82.7%.
Example 2
The method for comprehensively utilizing waste silicon powder in the synthetic process of the organic silicon monomer, which is described in the embodiment 2, comprises the following steps:
activating and stirring: adding waste silicon powder and waste silicon copper contacts generated in the synthetic process of industrial-grade production organic silicon monomers into an activation tank 1, wherein a stirrer is arranged in the activation tank 1, stirring the waste silicon powder and the waste copper contacts by using the stirrer to prepare a copper-silicon powder mixture with the copper content of 15%, then adding an activating agent into the activation tank 1, wherein the activating agent is added according to the proportion of adding 50g of the copper-silicon powder mixture per kilogram, the activating agent is a mixture of tin powder, zinc powder, aluminum powder, sodium chloride and potassium chloride, the mass ratio of the tin powder to the zinc powder in the activating agent is 1:1.5, the content of the aluminum powder is less than 0.1wt.%, and the content of the sodium chloride and the potassium chloride is less than 50ppm, the activating agent is used for carrying out catalytic activation on the copper-silicon powder mixture, then stirring and activating the copper-silicon powder mixture and the activating agent in the activation tank 1 to prepare a silicon-copper powder activation material, and then conveying the silicon-copper powder activation material into a sending tank 3 through a conveying pipe 2;
② reaction in a bed: firstly replacing a return bed reactor 4 and all pipelines communicated with the return bed reactor 4 with inert gas, wherein the inert gas is nitrogen, the return bed reactor 4 and all pipelines are replaced by using the nitrogen, in order to ensure that waste silicon powder in the fluidized bed reactor 4 is efficiently contacted with methyl chloride and improve the product quality of methyl chlorosilane, then introducing heat conduction oil into a heat exchange pipe of the return bed reactor 4, controlling the temperature in the return bed reactor 4 to be 300 ℃ by using the heat conduction oil, controlling the reaction intensity of the waste silicon powder in the fluidized bed reactor 4 and the methyl chloride by controlling the temperature, further improving the utilization rate of the waste silicon powder while ensuring the product quality of the methyl chlorosilane, then conveying silicon-copper powder activated material in a sending tank 3 into the fluidized bed reactor 4 through a feeding pipe 6 by using a feeding pump 5, and simultaneously introducing the methyl chloride into the fluidized bed reactor 4 from the bottom of the activated bed reactor 4 by using a guide pipe 7 Carrying out a fluidization reaction on the copper silicon powder activation material and chloromethane in a fluidized bed reactor 4, wherein the feeding amount of the silicon copper powder activation material is controlled at 300kg/h, the feeding amount of the chloromethane is controlled at 1200kg/h, gas-material mixed particles produced by the fluidization reaction are discharged from the top of the fluidized bed reactor 4, and the gas-material mixed particles contain methyl chlorosilane, silicon, copper, tin, zinc and other components;
thirdly, separation treatment: the gas-material mixed particles obtained by the first-stage separation are led into a second-stage cyclone separator 14 through a communicating pipe 13 for second-stage separation, the gas-material mixed particles obtained by the second-stage separation are discharged from the top of the second-stage cyclone separator 14 and are conveyed into a washing tower 15, and the ultrafine particles obtained by the second-stage separation and have the particle size of less than 1000 meshes are discharged from the bottom of the second-stage cyclone separator 14 and are conveyed into a fine powder storage tank 16, the performance of the superfine particle material can not meet the requirement of a vulcanization reaction, and the copper and the silicon powder are independently recovered through subsequent separation treatment;
leaching silicon powder: adding an acid solution into a fine powder storage tank 16 filled with ultrafine particles, stirring and soaking to obtain a mixed solution, wherein the acid solution is a sulfuric acid solution with the concentration of 0.1-41 wt.%, and the solid-to-liquid ratio of the ultrafine silicon powder particles to the acid solution is 1:8mL/g, adding reduced iron powder with the mass 60 times that of the mixed solution into the mixed solution for a displacement reaction after the soaking reaction is completed, and filtering and separating the mixed solution after the displacement reaction is completed to obtain a metal product and a silicon powder leaching solution; the metal product contains elements such as copper, zinc, tin and the like;
silicon powder recovery: and (4) conveying the silicon powder leachate obtained by separation in the step (iv) into a neutralization tank 17, adding an alkaline agent into the neutralization tank 17 to neutralize the silicon powder leachate in the neutralization tank 17, wherein the alkaline agent is caustic soda, and after the neutralization reaction is finished, pickling and filtering the neutralized and leached solid silicon powder again to obtain a silicon powder product.
The process of the embodiment 2 is simple in technology and low in operation cost, and by utilizing the waste silicon powder and the waste silicon copper contacts in a grading manner, on one hand, the waste silicon powder and the waste silicon copper contacts with relatively large particle sizes are activated to regenerate organic silicon methyl monomers, so that the bed returning pressure of the fine silicon powder with relatively low activity is reduced in the aspect of industrial-grade organic silicon methyl monomer synthesis, the operation efficiency of a large bed is improved, the whole organic silicon methyl monomer synthesis efficiency is improved, the start cycle of the large bed is prolonged, good production benefits can be brought to enterprises, meanwhile, the continuous production of the waste silicon powder and the waste silicon copper contacts can be realized, and the process has good popularization and utilization values; on the other hand, valuable metal ions in the fine waste silicon powder and the contact body are subjected to reduction extraction, so that the pollution of the fine silicon powder and the waste copper contact body to the environment and the damage to a human body are avoided, the resource utilization of the waste silicon powder and the waste copper contact body is realized, the recovery rate of the waste copper reaches 87.6%, and the recovery rate of the waste zinc reaches 83.5%.
Example 3
The method for comprehensively utilizing waste silicon powder in the synthetic process of the organic silicon monomer, which is described in the embodiment 3, comprises the following steps:
activating and stirring: adding waste silicon powder and waste silicon copper contacts generated in the synthetic process of industrial-grade production organic silicon monomers into an activation tank 1, wherein a stirrer is arranged in the activation tank 1, stirring the waste silicon powder and the waste copper contacts by using the stirrer to prepare a copper-silicon powder mixture with the copper content of 20%, then adding an activating agent into the activation tank 1, wherein the activating agent is added according to the proportion of adding 100g of the copper-silicon powder mixture per kilogram, the activating agent is a mixture of tin powder, zinc powder, aluminum powder, sodium chloride and potassium chloride, the mass ratio of the tin powder to the zinc powder in the activating agent is 1:2, the content of the aluminum powder is less than 0.1wt.%, and the content of the sodium chloride and the potassium chloride is less than 50ppm, the activating agent is used for carrying out catalytic activation on the copper-silicon powder mixture, then stirring and activating the copper-silicon powder mixture and the activating agent in the activation tank 1 to prepare a silicon-copper powder activation material, and then conveying the silicon-copper powder activation material into a sending tank 3 through a conveying pipe 2;
② reaction in a bed: firstly replacing a return bed reactor 4 and all pipelines communicated with the return bed reactor 4 with inert gas, wherein the inert gas is helium, replacing the return bed reactor 4 and all pipelines with helium, so as to ensure that waste silicon powder in a fluidized bed reactor 4 is efficiently contacted with methyl chloride and improve the product quality of methyl chlorosilane, then introducing heat conduction oil into a heat exchange pipe of the return bed reactor 4, controlling the temperature in the return bed reactor 4 to be 320 ℃ by utilizing the heat conduction oil, controlling the reaction intensity of the waste silicon powder in the fluidized bed reactor 4 and the methyl chloride by controlling the temperature, further improving the utilization rate of the waste silicon powder while ensuring the product quality of the methyl chlorosilane, then conveying silicon-copper powder activated material in a sending tank 3 into the fluidized bed reactor 4 through a feeding pipe 6 by utilizing a feeding pump 5, and simultaneously introducing the methyl chloride into the fluidized bed reactor 4 from the bottom of an activated bed reactor 4 by utilizing a guide pipe 7 Carrying out a fluidization reaction on the copper silicon powder activation material and chloromethane in a fluidized bed reactor 4, wherein the feeding amount of the silicon copper powder activation material is controlled at 500kg/h, the feeding amount of the chloromethane is controlled at 2000kg/h, gas-material mixed particles produced by the fluidization reaction are discharged from the top of the fluidized bed reactor 4, and the gas-material mixed particles contain methyl chlorosilane, silicon, copper, tin, zinc and other components;
thirdly, separation treatment: the gas-material mixed particles obtained by the first-stage separation are led into a second-stage cyclone separator 14 through a communicating pipe 13 for second-stage separation, the gas-material mixed particles obtained by the second-stage separation are discharged from the top of the second-stage cyclone separator 14 and are conveyed into a washing tower 15, and the ultrafine particles obtained by the second-stage separation and have the particle size of less than 1000 meshes are discharged from the bottom of the second-stage cyclone separator 14 and are conveyed into a fine powder storage tank 16, the performance of the superfine particle material can not meet the requirement of a vulcanization reaction, and the copper and the silicon powder are independently recovered through subsequent separation treatment;
leaching silicon powder: adding an acid solution into a fine powder storage tank 16 filled with ultrafine particles, stirring and soaking to obtain a mixed solution, wherein the acid solution is a mixture of a hydrochloric acid solution with the concentration of 0.1-41 wt.% and a sulfuric acid solution with the concentration of 0.1-41 wt.%, the solid-to-liquid ratio of the ultrafine silicon powder particles to the acid solution is 1:10mL/g, adding reduced iron powder with the mass of 100 times that of the mixed solution into the mixed solution for a displacement reaction after the soaking reaction is completed, and filtering and separating the mixed solution after the displacement reaction is completed to obtain a metal product and a silicon powder leachate; the metal product contains elements such as copper, zinc, tin and the like;
silicon powder recovery: and (4) conveying the silicon powder leachate obtained by separation in the step (iv) into a neutralization tank 17, adding an alkaline agent into the neutralization tank 17 to neutralize the silicon powder leachate in the neutralization tank 17, wherein the alkaline agent is sodium carbonate, and after the neutralization reaction is finished, pickling and filtering the neutralized and leached solid silicon powder again to obtain a silicon powder product.
The process of the embodiment 3 is simple in technology and low in operation cost, and by utilizing the waste silicon powder and the waste silicon copper contacts in a grading manner, on one hand, the waste silicon powder and the waste silicon copper contacts with relatively large particle sizes are activated to regenerate organic silicon methyl monomers, so that the bed returning pressure of the fine silicon powder with relatively low activity is reduced in the aspect of industrial-grade organic silicon methyl monomer synthesis, the operation efficiency of a large bed is improved, the whole organic silicon methyl monomer synthesis efficiency is improved, the start cycle of the large bed is prolonged, good production benefits can be brought to enterprises, meanwhile, the continuous production of the waste silicon powder and the waste silicon copper contacts can be realized, and the process has good popularization and utilization values; on the other hand, valuable metal ions in the fine waste silicon powder and the contact body are subjected to reduction extraction, so that the pollution of the fine silicon powder and the waste copper contact body to the environment and the damage to a human body are avoided, the resource utilization of the waste silicon powder and the waste copper contact body is realized, the recovery rate of the waste copper reaches 89.2%, and the recovery rate of the waste zinc reaches 84.6%.
Claims (7)
1. A comprehensive utilization method of waste silicon powder in the synthetic process of an organic silicon monomer is characterized by comprising the following steps: the method comprises the following steps:
activating and stirring: adding waste silicon powder and waste silicon copper contacts generated in the synthetic process of industrial-grade production organic silicon monomers into an activation tank (1), stirring to prepare a copper-silicon powder mixture with the copper content of 1-20%, then adding an activating agent into the activation tank (1), adding the activating agent according to the proportion of 0.0001-100 g added in each kilogram of the copper-silicon powder mixture, stirring and activating the copper-silicon powder mixture and the activating agent in the activation tank (1) to prepare a silicon-copper powder activation material, and then conveying the silicon-copper powder activation material into a delivery tank (3) through a conveying pipe (2);
② reaction in a bed: replacing a return bed reactor (4) and all pipelines communicated with the return bed reactor (4) by inert gas, introducing heat conduction oil into a heat exchange pipe of the return bed reactor (4), controlling the temperature in the return bed reactor (4) to be 260-320 ℃ by utilizing the heat conduction oil, then conveying a silicon-copper powder activated material in a sending tank (3) into the fluidized bed reactor (4) through a feeding pipe (6) by utilizing a feeding pump (5), introducing methyl chloride into the fluidized bed reactor (4) from the bottom of the activated bed reactor (4) by utilizing a guide pipe (7), carrying out a fluidized reaction on the copper-silicon powder activated material and the methyl chloride in the fluidized bed reactor (4), and discharging gas-material mixed particles produced by the fluidized reaction from the top of the fluidized bed reactor (4);
thirdly, separation treatment: the gas-material mixed particles discharged from the top of the fluidized bed reactor (4) are conveyed into a primary cyclone separator (9) through a discharge pipe (8) for primary separation, coarse particles with the particle size larger than 400 meshes obtained by the primary separation are discharged from the bottom of the primary cyclone separator (9) and enter a storage tank (10), and then are introduced into the fluidized bed reactor (4) through a material returning pump (11) and a material returning pipe (12) for continuous fluidized reaction, the gas-material mixed particles obtained by the first-stage separation enter a second-stage cyclone separator (14) through a communicating pipe (13) for second-stage separation, the dusty gas obtained by the second-stage separation is discharged from the top of the second-stage cyclone separator (14) and is conveyed into a washing tower (15), the ultrafine particles with the particle size less than 1000 meshes obtained by the secondary separation are discharged from the bottom of the secondary cyclone separator (14) and conveyed into a fine powder storage tank (16);
leaching silicon powder: adding an acid solution into a fine powder storage tank (16) filled with ultrafine particles, stirring and soaking to obtain a mixed solution, wherein the solid-to-liquid ratio of ultrafine silicon powder particles to the acid solution is 1: 5-10 mL/g, adding reduced iron powder with the mass of 0.1-100 times of that of the mixed solution into the mixed solution for a displacement reaction after the soaking reaction is completed, and filtering and separating the mixed solution after the displacement reaction is completed to obtain a metal product and a silicon powder leaching solution; the metal product contains elements such as copper, zinc, tin and the like;
silicon powder recovery: and (4) conveying the silicon powder leachate obtained by separation in the step (IV) into a neutralization tank (17), adding an alkaline agent into the neutralization tank (17) to neutralize the silicon powder leachate in the neutralization tank (17), and after the neutralization reaction is finished, carrying out acid washing and filtering on the neutralized and leached solid silicon powder again to obtain a silicon powder product.
2. The method for comprehensively utilizing waste silicon powder in the synthetic process of the organic silicon monomer, according to claim 1, is characterized in that: in the first step, the activating agent is a mixture of tin powder, zinc powder, aluminum powder, sodium chloride and potassium chloride, the mass ratio of the tin powder to the zinc powder in the activating agent is 1: 1-2, the content of the aluminum powder is less than 0.1wt.%, and the content of the sodium chloride and the potassium chloride is less than 50 ppm.
3. The method for comprehensively utilizing waste silicon powder in the synthetic process of the organic silicon monomer, according to claim 1, is characterized in that: in the second step, the inert gas is one of argon, nitrogen or helium.
4. The method for comprehensively utilizing waste silicon powder in the synthetic process of the organic silicon monomer, according to claim 1, is characterized in that: in the second step, the feeding amount of the silicon copper powder activating material is controlled to be 80-500 kg/h, and the feeding amount of the chloromethane is controlled to be 320-2000 kg/h.
5. The method for comprehensively utilizing waste silicon powder in the synthetic process of the organic silicon monomer, according to claim 1, is characterized in that: in the second step, the gas-material mixed particles contain methyl chlorosilane, silicon, copper, tin, zinc and other components.
6. The method for comprehensively utilizing waste silicon powder in the synthetic process of the organic silicon monomer, according to claim 1, is characterized in that: in the step (iv), the acidic solution is one or a mixture of two of a hydrochloric acid solution with a concentration of 0.1 to 41wt.% and a sulfuric acid solution with a concentration of 0.1 to 41 wt.%.
7. The method for comprehensively utilizing waste silicon powder in the synthetic process of the organic silicon monomer, according to claim 1, is characterized in that: in the fifth step, the alkaline agent is soda or caustic soda.
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