CN112321626A - Method for treating organic silicon slag slurry - Google Patents
Method for treating organic silicon slag slurry Download PDFInfo
- Publication number
- CN112321626A CN112321626A CN202011249648.4A CN202011249648A CN112321626A CN 112321626 A CN112321626 A CN 112321626A CN 202011249648 A CN202011249648 A CN 202011249648A CN 112321626 A CN112321626 A CN 112321626A
- Authority
- CN
- China
- Prior art keywords
- tank
- slurry
- hydrolysis
- hcl
- slag
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000002002 slurry Substances 0.000 title claims abstract description 78
- 239000002893 slag Substances 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 36
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 21
- 239000010703 silicon Substances 0.000 title claims abstract description 21
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 78
- 230000007062 hydrolysis Effects 0.000 claims abstract description 74
- 239000007788 liquid Substances 0.000 claims abstract description 29
- 238000010521 absorption reaction Methods 0.000 claims abstract description 22
- 239000000706 filtrate Substances 0.000 claims abstract description 19
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052802 copper Inorganic materials 0.000 claims abstract description 11
- 239000010949 copper Substances 0.000 claims abstract description 11
- 238000000926 separation method Methods 0.000 claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 84
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 38
- 239000007789 gas Substances 0.000 claims description 21
- 229910052757 nitrogen Inorganic materials 0.000 claims description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 239000010802 sludge Substances 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 6
- 238000003795 desorption Methods 0.000 claims description 6
- 239000000498 cooling water Substances 0.000 claims description 5
- 239000003921 oil Substances 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000000605 extraction Methods 0.000 claims description 3
- 238000003860 storage Methods 0.000 claims description 3
- 230000014759 maintenance of location Effects 0.000 claims description 2
- 238000005903 acid hydrolysis reaction Methods 0.000 claims 1
- 238000007664 blowing Methods 0.000 claims 1
- 229920006395 saturated elastomer Polymers 0.000 claims 1
- 239000002699 waste material Substances 0.000 abstract description 18
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 abstract description 6
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000003786 synthesis reaction Methods 0.000 abstract description 4
- 239000003513 alkali Substances 0.000 abstract description 2
- 239000006227 byproduct Substances 0.000 abstract description 2
- 238000007599 discharging Methods 0.000 abstract description 2
- 229940050176 methyl chloride Drugs 0.000 abstract description 2
- 239000002910 solid waste Substances 0.000 abstract description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 31
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 31
- 239000012071 phase Substances 0.000 description 16
- 238000009835 boiling Methods 0.000 description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 239000000413 hydrolysate Substances 0.000 description 5
- 239000000178 monomer Substances 0.000 description 5
- 238000005336 cracking Methods 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000002485 combustion reaction Methods 0.000 description 3
- 230000003301 hydrolyzing effect Effects 0.000 description 3
- 239000011863 silicon-based powder Substances 0.000 description 3
- 108010009736 Protein Hydrolysates Proteins 0.000 description 2
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000003595 mist Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 239000003570 air Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- PZPGRFITIJYNEJ-UHFFFAOYSA-N disilane Chemical compound [SiH3][SiH3] PZPGRFITIJYNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000000703 high-speed centrifugation Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910021654 trace metal Inorganic materials 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Images
Classifications
-
- 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
- C07F7/0834—Compounds having one or more O-Si linkage
- C07F7/0838—Compounds with one or more Si-O-Si sequences
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
-
- 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
- C07F7/0834—Compounds having one or more O-Si linkage
- C07F7/0838—Compounds with one or more Si-O-Si sequences
- C07F7/0872—Preparation and treatment thereof
- C07F7/0874—Reactions involving a bond of the Si-O-Si linkage
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Inorganic Chemistry (AREA)
- Processing Of Solid Wastes (AREA)
- Treating Waste Gases (AREA)
Abstract
The invention belongs to the technical field of treatment and comprehensive utilization of organic silicon byproducts, and particularly relates to a treatment method of organic silicon slag slurry, wherein a slurry slag moving tank is communicated with a slurry slag buffer tank through a hose, the slurry slag buffer tank is communicated with a hydrolysis tank, a solid-liquid mixture after hydrolysis is conveyed to a filter press for solid-liquid separation, filtrate enters a filtrate tank, and the filtrate in the filtrate tank is conveyed to a phase separator for oil-water separation; and (3) feeding the hydrolyzed gas phase into an HCl absorption tower to absorb HCl, feeding the gas discharged from the top of the HCl absorption tower into an alkaline washing tower to neutralize a small amount of HCl contained in the gas, feeding the gas discharged from the alkaline washing tower into a liquid seal tank, contacting with alkali liquor to further remove HCl, and discharging the gas into the atmosphere. The invention realizes the harmless treatment of a large amount of slurry slag generated in the production process of organic silicon, the treated solid waste can be subjected to the next procedure to extract copper, HCl gas generated in the hydrolysis process is absorbed and analyzed to obtain high-purity HCl, and the high-purity HCl is returned to the methyl chloride synthesis unit, thereby realizing the resource utilization of waste.
Description
Technical Field
The invention belongs to the technical field of treatment and comprehensive utilization of organic silicon byproducts, and particularly relates to a treatment method of organic silicon slag slurry.
Background
The organosilicon slurry is waste slurry generated in the synthesis process of organosilicon monomers, accounts for about 3 percent of the monomer amount, and is accompanied by generation of a large amount of organosilicon waste slurry along with rapid expansion of the yield of the organosilicon monomers, and the organosilicon waste slurry mainly comprises more high-boiling residues and a small amount of silicon powder (the particle size is 2-150 um) brought out by a fluidized bed, copper powder, trace elements such as Fe, Zn, Al, Sn and the like. Wherein the boiling range of the high boiling substance is 70.5-250 ℃, the components are mainly disilane, siloxane and chloromethane, and the solid content is 20-25%. Because of their flammable and volatile properties, they are susceptible to strong acid mist and combustion if exposed to air, and therefore must be harmlessly treated. At present, slag slurry is discharged into a water tank for hydrolysis by a plurality of organic silicon production enterprises, the discharged hydrogen chloride is seriously polluted, and cuprous ions in the slag slurry are easy to cause combustion and explosion when meeting open fire and air due to strong reducibility, thereby causing serious potential safety hazard.
US patent US4221691 provides a method for treating waste pulp: a small amount of mineral oil was added to the waste sludge slurry to improve the hydrolysis characteristics. The obvious drawback of this process is the additional addition of organic solvents and the inability to recover; copper is not recovered, so that resource waste is caused; after hydrolysis, a large amount of waste is generated, and the post-treatment workload is large, so that a large amount of waste residue slurry is difficult to treat.
Patent CN1618840 describes a method for treating organosilicon slurry slag, which comprises the following steps:
(1) separating 90% (weight percentage) of high-boiling residue from waste residue slurry in the synthesis of organosilicon monomers by a gravity settling centrifuge, and using the high-boiling residue for cracking and other purposes;
(2) hydrolyzing the centrifuged high-viscosity waste residue slurry in a hydrolysis kettle, wherein the hydrolysis medium is 70% sulfuric acid solution;
(3) a small amount of hydrogen chloride gas containing siloxane is separated out from the liquid phase;
(4) and (4) carrying out liquid-solid separation on the hydrolysate, discharging the solid hydrolysate, and recovering copper after subsequent treatment of the liquid phase.
This has the advantage that part of the high boiling is recovered for cracking and other uses. The method has the disadvantages that the sulfuric acid solution is used as the hydrolysis liquid, HCl generated in the hydrolysis process cannot be recovered, a large amount of sulfuric acid-containing wastewater can be generated, the resource waste is caused, and the method is not environment-friendly.
Patent CN200310115386.2 describes a method for treating waste sludge slurry: separating high-boiling residues from solids by a horizontal screw centrifuge, wherein most of the recovered high-boiling residues are used for cracking, and the separated concentrated residue slurry is used for hydrolyzing and recovering copper in the high-boiling residues. The method has the defects that most of the recovered high-boiling residues have about 2 percent of fine silicon powder carrying trace metal elements in the high-boiling residues due to the particle size of the silicon powder being 2-150 mu m, and can not be directly used for cracking due to catalyst poisoning; in addition, under the action of strong centrifugal force of a horizontal screw centrifuge, a large amount of acid mist is formed and discharged, so that environmental pollution is caused; cuprous ions with strong reducibility are easy to contact with air to cause combustion under high-speed centrifugation, and are unsafe; the high-boiling-point substances are strong in corrosivity and need to be subjected to sealing treatment, so that the material selection of the centrifugal machine is expensive.
Disclosure of Invention
The invention aims to provide a method for treating organic silicon slurry residues, which can realize harmless treatment of a large amount of slurry residues generated in the production process of organic silicon.
The method comprises the following specific steps:
(1) transferring the slurry slag generated in the front-end procedure to a production site through a slurry slag moving tank, and pressing the slurry slag into a slurry slag buffer tank a and a slurry slag buffer tank b in a nitrogen pressurization mode;
(2) 30% concentrated hydrochloric acid is added into the hydrolysis tank and a certain liquid level is maintained;
(3) conveying the slurry residues in the slurry residue buffer tank a and the slurry residue buffer tank b to the hydrolysis tank in a nitrogen pressurization mode;
(4) after entering a hydrolysis tank, the slurry residue is stirred by a stirrer to be fully contacted with concentrated hydrochloric acid for hydrolysis, and the reaction retention time is 5-10 minutes;
(5) the solid-liquid mixture after hydrolysis is sent into a filter press by a pump a for solid-liquid separation;
(6) conveying the filter-pressed solid slag to a copper extraction unit to recover copper;
(7) the filtrate enters a filtrate tank for temporary storage, and the filtrate is sent into a phase separator through a pump b for oil-water separation;
(8) sending the oil phase separated by the phase separator into a front-end process or barreling for sale, and returning the acid water to the hydrolysis tank to be used as a hydrolysis supplementary liquid;
(9) the gas phase discharged from the hydrolysis tank enters an HCl absorption tower to absorb HCl, so that high-concentration hydrochloric acid is obtained;
(10) sending the high-concentration hydrochloric acid into a hydrochloric acid desorption system through a pump for desorption to obtain high-purity HCl;
(11) tail gas discharged by the HCl absorption tower enters an alkaline washing tower to neutralize unabsorbed HCl;
(12) and the tail gas discharged by the alkaline tower is washed by a liquid seal tank and then discharged after reaching the standard.
(13) The heat generated by the hydrolysis reaction in the hydrolysis tank is taken away by the circulating cooling water in the jacket, and the temperature in the hydrolysis tank is kept to be less than 50 ℃.
Has the advantages that: the invention realizes the harmless treatment of a large amount of slurry slag generated in the production process of organic silicon, the treated solid waste can be subjected to the next procedure to extract copper, HCl gas generated in the hydrolysis process is absorbed and analyzed to obtain high-purity HCl, and the high-purity HCl is returned to the methyl chloride synthesis unit, thereby realizing the resource utilization of waste. The process has the advantages of low investment, convenient operation, less discharge of three wastes, safety and environmental protection, and solves the problem of treatment of the organic silicon slurry slag.
1. Compared with open hydrolysis, no HCl gas is dissipated into the environment, the field operation environment is good, and the environmental pollution is small.
2. The closed hydrolysis avoids the contact of inflammable and explosive substances and air, and nitrogen is added into the system for protection, so that the micro-positive pressure of the system is always ensured, and the safety is high. 3. The saturated hydrochloric acid is used for hydrolysis, so that HCl can be recovered from a gas phase, the waste of chlorine resources is reduced, the use of alkali is reduced, and the discharge of three wastes is reduced. 4. The hydrolyzed substance is separated into phases by a filter to obtain a hydrolysate with higher quality, and the hydrolysate can be used as a high-boiling silicone oil product by washing and the like. 5. The automation level of the equipment can be effectively improved, the labor intensity of personnel is reduced, the labor force is reduced, and the production cost is saved.
6. The generated hydrolysate is the same as the hydrolysate generated by hydrolyzing the organic silicon monomer, and the hydrolysate can be recycled.
7. The production amount of three wastes is small, and the concentrated hydrochloric acid is recycled internally, so that the method is safe and environment-friendly.
8. The sludge at the lower level is conveyed to a buffer tank at the upper level by using nitrogen.
9. The two buffer tanks are used alternately, so that the adjustment and the equipment maintenance are convenient, and the production efficiency is improved;
10. the phase separator can effectively separate oil from water in the mixed liquid, and the separation efficiency is more than 99 percent.
Drawings
FIG. 1 is a schematic diagram of the present invention.
Wherein, 1 is a slurry residue moving tank, 2 is a slurry residue buffer tank a, 3 is a slurry residue buffer tank b, 4 is a hydrolysis tank stirrer, 5 is a hydrolysis tank, 6 is a hydrolysis tank delivery pump, 7 is a filter press, 8 is a filtrate tank, 9 is a filtrate tank delivery pump, 10 is a phase separator, 11 is an HCl absorption tower, 12 is an HCl absorption tower circulating pump, 13 is an alkaline tower, 14 is an alkaline tower circulating pump, 15 is a liquid seal tank, and 16 is a hydrolysis tank jacket.
Detailed Description
The present invention will be further described with reference to the following specific examples, but the scope of the present invention is not limited thereto.
As shown in fig. 1, the treatment system of the organic silicon slag slurry comprises a slurry slag moving tank 1, wherein the slurry slag moving tank 1 is communicated with a slurry slag buffer tank through a pipeline, the slurry slag buffer tank is communicated with a hydrolysis tank 5 through a pipeline, and a stirrer 4 is arranged on the hydrolysis tank; a slurry outlet at the bottom of the hydrolysis tank 5 is connected with a filter press 7 through a hydrolysis tank delivery pump 6, a filtrate outlet of the filter press 7 is connected with a filtrate tank 8 through a pipeline, the filtrate tank 8 is connected with a phase separator 10 through a filtrate tank delivery pump 9, the phase separator 10 performs oil-water separation, an oil phase separated by the phase separator is sent to a front-end process or is barreled for sale, and acid water is returned to the hydrolysis tank as hydrolysis make-up liquid;
a gas outlet is formed in the hydrolysis tank 5 and is connected with the HCl absorption tower 11 through a pipeline, a gas outlet at the top end of the HCl absorption tower 11 is connected with the alkaline washing tower 13 through a pipeline, a gas outlet at the top end of the alkaline washing tower 13 is connected with the liquid seal tank 15 through a pipeline, a pipeline of the gas outlet of the alkaline washing tower 13 extends below the liquid level of the liquid seal tank 15, and a pipeline is arranged on the upper surface of the liquid seal tank 25 for emptying;
nitrogen inlets are arranged on the slurry residue moving tank 1, the slurry residue buffer tank, the hydrolysis tank 5, the HCl absorption tower 11 and the alkaline washing tower 13;
and gate valves are arranged on all the pipelines.
Furthermore, the slurry-slag buffer tanks are two, namely a slurry-slag buffer tank a2 and a slurry-slag buffer tank b3, the slurry-slag moving tank is respectively connected with the slurry-slag buffer tank a2 and the slurry-slag buffer tank b3 through pipelines, the slurry-slag buffer tank a2 and the slurry-slag buffer tank b3 are respectively connected with the hydrolysis tank 5 through pipelines, the slurry-slag buffer tank a and the slurry-slag buffer tank b are respectively provided with an exhaust port, and the exhaust ports are provided with gate valves; and nitrogen inlets are arranged on pipelines connecting the pulp and slag buffer tank a2 and the pulp and slag buffer tank b3 with the hydrolysis tank 5, and gate valves are arranged at the nitrogen inlets. If pipelines between the pulp and slag buffer tank a and between the pulp and slag buffer tank b and the nitrogen input pipe are blocked, closing gate valves of the pipelines and the hydrolysis tank, and carrying out back flushing by using nitrogen; if the pipeline between the nitrogen input pipe and the hydrolysis tank is blocked, the blocked part is directly blown into the hydrolysis tank by using nitrogen, and the blockage is blown off.
Further, a hydrolysis tank jacket 16 is arranged on the outer side of the hydrolysis tank 5, and cooling water is introduced into the hydrolysis tank jacket 16 to cool the hydrolysis tank.
Further, a dilute hydrochloric acid inlet is formed in the upper end of the HCl absorption tower 11, a spray header is arranged at the lower end of the HCl absorption tower 11 through an HCl absorption tower circulating pump 12, and the spray header is arranged inside the upper end of the HCl absorption tower 11; a concentrated hydrochloric acid outlet is formed in the pipeline at the upper end of the HCl absorption tower circulating pump 12, a gate valve is arranged on the concentrated hydrochloric acid outlet, and a gate valve is arranged on the pipeline.
Further, a spray head is arranged at the lower end 13 of the alkaline tower through an alkaline tower circulating pump 14, the spray head is arranged inside the upper end of the alkaline tower 13, a NaOH solution with the concentration of 10-20% is added into the alkaline tower 13, and a gate valve is arranged on a pipeline.
Further, a 10-20% NaOH solution is added into the liquid-sealed tank 15.
Further, the lower end of the alkaline tower 13 is connected with the upper end of the alkaline tower 13 through an alkaline tower circulating pump 14, and a gate valve is arranged on a pipeline.
Further, the lower end of the alkaline tower 13 is connected with the upper part of the liquid seal tank 15 through an alkaline tower circulating pump 14, and a gate valve is arranged on a pipeline.
Further, the lower part of the liquid seal tank 15 is connected with the upper end of the alkaline washing tower 13 through a pipeline, and a gate valve is arranged on the pipeline.
The method comprises the following steps:
(1) the slurry slag generated in the front-end procedure (organic silicon) is transferred to a hydrolysis device through a slurry slag moving tank 1 and is connected with a slurry slag buffer tank through a hose, 0.6MPa nitrogen is introduced into the slurry slag moving tank, when the pressure of the slurry slag moving tank is increased to 0.3MPa, a valve of the slurry slag moving tank is slowly opened to the slurry slag buffer tank, the slurry slag is pressed into the slurry slag buffer tank, and the speed of pressing the slurry slag into the slurry slag buffer tank is adjusted through the opening degree of the valve;
(2) after the pulp slag is pressed in, purging the pressing-in pipeline by using nitrogen, and after the purging is finished, returning the pulp slag moving tank to the front-end process to perform the next working cycle;
(3) adding 30% concentrated hydrochloric acid into the hydrolysis tank 5 and keeping a certain liquid level;
(4) opening a 0.6MPa nitrogen valve of the slurry residue buffer tank to pressurize the slurry residue buffer tank, closing the nitrogen valve when the pressure is increased to 0.3MPa, opening a regulating valve of the slurry residue buffer tank to the hydrolysis tank, controlling the feeding amount of the hydrolysis tank 5 through the regulating valve, and fully stirring and contacting the slurry residue with 30% hydrochloric acid for 5-10 minutes through a stirrer after the slurry residue enters the hydrolysis tank;
(5) the solid-liquid mixture after hydrolysis is sent to a filter press 7 through a hydrolysis tank delivery pump 6 for solid-liquid separation;
(6) conveying the filter-pressed solid slag to a copper extraction unit to recover copper;
(7) the filtrate enters a filtrate tank 8 for temporary storage in a self-flowing mode, and then is sent to a phase separator 10 by a filtrate delivery pump 9 for oil-water separation;
(8) sending the oil phase separated by the phase separator 10 to a front-end process or barreling for sale, and returning the acid water to a hydrolysis tank to be used as a hydrolysis supplementary liquid;
(9) the gas phase discharged from the hydrolysis tank 5 enters an HCl absorption tower to absorb HCl gas under the pressure drive of the hydrolysis tank, and 1% hydrochloric acid absorption liquid conveyed from the outside is continuously and circularly sprayed in the packed tower to obtain high-concentration hydrochloric acid;
(10) sending high-concentration hydrochloric acid into a hydrochloric acid desorption system through an HCl absorption tower circulating pump 12 for desorption to obtain high-purity HCl;
(11) the tail gas discharged after the HCl absorption tower absorbs more than or equal to 95% of HCl enters an alkaline washing tower 13, a NaOH solution with the concentration of 10-20% is added into the alkaline washing tower 13, a small amount of unabsorbed HCl is neutralized in a leaching mode, and when the pH value of a leaching solution is 6-8, the HCl is discharged to a sewage treatment station;
(12) the tail gas discharged after being neutralized and washed by the alkaline tower 13 is washed by the liquid seal tank 15 and discharged after reaching the standard.
(13) The heat generated by the hydrolysis reaction in the hydrolysis tank 5 is taken away by the circulating cooling water in the jacket, and the temperature in the hydrolysis tank is kept to be less than 50 ℃.
Claims (6)
1. The method for treating the organosilicon slurry is characterized by comprising the following steps of:
(1) transferring the slurry slag generated in the organic silicon production procedure to a production site through a slurry slag moving tank, and pressing the slurry slag into a slurry slag buffer tank a and a slurry slag buffer tank b in a nitrogen pressurization mode;
(2) adding a certain amount of concentrated hydrochloric acid into the hydrolysis tank;
(3) conveying the slurry residues in the slurry residue buffer tank a and the slurry residue buffer tank b to the hydrolysis tank in a nitrogen pressurization mode;
(4) after entering a hydrolysis tank, the slurry residue is stirred by a stirrer to be fully contacted with concentrated hydrochloric acid for hydrolysis, the reaction retention time is 5-10 minutes, and the temperature in the hydrolysis tank is kept within 50 ℃;
(5) the solid-liquid mixture after hydrolysis is sent into a filter press by a pump a for solid-liquid separation;
(6) sending the solid after filter pressing to a copper extraction unit to recover copper;
(7) the filtrate enters a filtrate tank for temporary storage, and the filtrate is sent into a phase separator through a pump b for oil-water separation;
(8) sending the oil phase separated by the phase separator into a front-end process or barreling for sale, and returning the acid water to the hydrolysis tank to be used as a hydrolysis supplementary liquid;
(9) the gas phase discharged from the hydrolysis tank enters an HCl absorption tower to absorb HCl, so that high-concentration hydrochloric acid is obtained;
(10) sending the high-concentration hydrochloric acid into a hydrochloric acid desorption system through a pump c for desorption to obtain high-purity HCl;
(11) tail gas discharged by the HCl absorption tower enters an alkaline washing tower to neutralize unabsorbed HCl;
(12) and the tail gas discharged by the alkaline tower is washed by a liquid seal tank and then discharged after reaching the standard.
2. The method for treating the organic silicon sludge according to claim 1, which is characterized in that: saturated hydrochloric acid is arranged in the hydrolysis tank, HCl gas is extracted by adopting a saturated hydrochloric acid hydrolysis mode, HCl is insoluble in water in a saturated state, and HCl gas generated by hydrolysis reaction is completely discharged from a gas phase and then absorbed by an HCl absorption tower.
3. The method for treating the organic silicon sludge according to claim 1, which is characterized in that: the outer side of the hydrolysis tank is provided with a cooling water jacket, heat generated by hydrolysis reaction in the hydrolysis tank is taken away through circulating cooling water in the outer jacket, the heat of the hydrolysis tank can be effectively controlled, the heat in the hydrolysis tank is basically constant, and the stability of the solubility of HCl is ensured.
4. The method for treating the organic silicon sludge according to claim 1, which is characterized in that: and back-blowing nitrogen is added between the slurry and slag buffer tank a and the slurry and slag buffer tank b and the hydrolysis tank, so that the probability that the solid in the slurry and slag blocks the pipeline can be effectively reduced.
5. The method for treating the organic silicon sludge according to claim 1, which is characterized in that: the reaction is completely carried out in a closed container; slurry residue removes jar 1, slurry residue buffer tank an and slurry residue buffer tank b, and the hydrolysis tank, HCl absorption tower all insert nitrogen protection, and the possibility of isolated slurry residue and air contact can effectively reduce the safety risk.
6. The method for treating the organic silicon sludge according to claim 1, which is characterized in that: and adding a 10-20% NaOH solution into the alkaline tower and the liquid seal tank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011249648.4A CN112321626A (en) | 2020-11-10 | 2020-11-10 | Method for treating organic silicon slag slurry |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011249648.4A CN112321626A (en) | 2020-11-10 | 2020-11-10 | Method for treating organic silicon slag slurry |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112321626A true CN112321626A (en) | 2021-02-05 |
Family
ID=74319106
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011249648.4A Pending CN112321626A (en) | 2020-11-10 | 2020-11-10 | Method for treating organic silicon slag slurry |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112321626A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113582183A (en) * | 2021-08-26 | 2021-11-02 | 枣阳市一鸣化工有限公司 | Treatment method and treatment system for organic silicon waste residue slurry |
| CN114262792A (en) * | 2021-12-01 | 2022-04-01 | 鲁西化工集团股份有限公司硅化工分公司 | Organic silicon slurry residue hydrolysis treatment process and resource recycling method |
| CN114984879A (en) * | 2022-05-26 | 2022-09-02 | 中国化学赛鼎宁波工程有限公司 | Treatment system and method for organic silicon slurry slag |
| CN115475825A (en) * | 2022-09-29 | 2022-12-16 | 鲁西化工集团股份有限公司硅化工分公司 | Organic silicon slurry slag treatment process |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1618840A (en) * | 2003-11-21 | 2005-05-25 | 中国石油天然气股份有限公司 | Treatment method of organic silicon waste slag |
| CN102390860A (en) * | 2011-08-04 | 2012-03-28 | 山东东岳有机硅材料有限公司 | Environmentally-friendly treatment method and device for organosilicon slurry |
| CN104262379A (en) * | 2014-08-29 | 2015-01-07 | 浙江恒业成有机硅有限公司 | Organic silicon residue slurry treatment device and treatment method |
| CN105036081A (en) * | 2015-08-03 | 2015-11-11 | 昆明理工大学 | Method for producing HCl gas through chlorosilane residual liquor |
| CN105294751A (en) * | 2015-11-21 | 2016-02-03 | 唐山三友硅业有限责任公司 | Method for processing slag slurry generated during organic silicon monomer synthesis process |
| CN108570558A (en) * | 2018-05-15 | 2018-09-25 | 成都斯力康科技股份有限公司 | The method that copper is recycled from organosilicon slag slurry |
| CN110339622A (en) * | 2019-06-05 | 2019-10-18 | 江苏明珠硅橡胶材料有限公司 | A kind of organosilicon slag slurry hydrolysis process method |
-
2020
- 2020-11-10 CN CN202011249648.4A patent/CN112321626A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1618840A (en) * | 2003-11-21 | 2005-05-25 | 中国石油天然气股份有限公司 | Treatment method of organic silicon waste slag |
| CN102390860A (en) * | 2011-08-04 | 2012-03-28 | 山东东岳有机硅材料有限公司 | Environmentally-friendly treatment method and device for organosilicon slurry |
| CN104262379A (en) * | 2014-08-29 | 2015-01-07 | 浙江恒业成有机硅有限公司 | Organic silicon residue slurry treatment device and treatment method |
| CN105036081A (en) * | 2015-08-03 | 2015-11-11 | 昆明理工大学 | Method for producing HCl gas through chlorosilane residual liquor |
| CN105294751A (en) * | 2015-11-21 | 2016-02-03 | 唐山三友硅业有限责任公司 | Method for processing slag slurry generated during organic silicon monomer synthesis process |
| CN108570558A (en) * | 2018-05-15 | 2018-09-25 | 成都斯力康科技股份有限公司 | The method that copper is recycled from organosilicon slag slurry |
| CN110339622A (en) * | 2019-06-05 | 2019-10-18 | 江苏明珠硅橡胶材料有限公司 | A kind of organosilicon slag slurry hydrolysis process method |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113582183A (en) * | 2021-08-26 | 2021-11-02 | 枣阳市一鸣化工有限公司 | Treatment method and treatment system for organic silicon waste residue slurry |
| CN114262792A (en) * | 2021-12-01 | 2022-04-01 | 鲁西化工集团股份有限公司硅化工分公司 | Organic silicon slurry residue hydrolysis treatment process and resource recycling method |
| CN114984879A (en) * | 2022-05-26 | 2022-09-02 | 中国化学赛鼎宁波工程有限公司 | Treatment system and method for organic silicon slurry slag |
| CN114984879B (en) * | 2022-05-26 | 2024-03-01 | 中国化学赛鼎宁波工程有限公司 | Organosilicon slurry slag treatment system and method |
| CN115475825A (en) * | 2022-09-29 | 2022-12-16 | 鲁西化工集团股份有限公司硅化工分公司 | Organic silicon slurry slag treatment process |
| CN115475825B (en) * | 2022-09-29 | 2023-06-27 | 鲁西化工集团股份有限公司硅化工分公司 | Organosilicon slurry residue treatment process |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112321626A (en) | Method for treating organic silicon slag slurry | |
| CN106623370B (en) | Organic silicon slurry slag treatment process and system | |
| CN104759462B (en) | A kind of Soil leaching upgrading prosthetic device with tail gas treating function | |
| CN213951049U (en) | Processing system of organosilicon sediment thick liquid | |
| CN114984879B (en) | Organosilicon slurry slag treatment system and method | |
| CN112960881A (en) | Method and system for breaking package of ultrasonic hot-washing oily sludge | |
| CN111994928A (en) | Aluminum ash recycling system and processing method thereof | |
| CN211078840U (en) | Oily sludge recycling and reduction treatment system | |
| CN109179930B (en) | Method for three-phase separation of oil, mud and water in tank bottom oil sludge and efficient recovery of oil in oil sludge | |
| CN108423952B (en) | Combined process for treating oily sludge by supercritical fluid gradient extraction-oxidative degradation coupling | |
| CN108383142B (en) | Method for producing alumina by recycling regenerated aluminum ash | |
| CN212450663U (en) | Aluminum ash recovery processing system | |
| CN216073092U (en) | High-efficient extraction and clean system of calcium fluoride in aluminium electroloysis overhaul sediment | |
| CN110963510B (en) | Recovery processing device and process for waste sulfuric acid | |
| CN102452688B (en) | Device and method for treating polyolefin catalyst filtrate | |
| CN213944301U (en) | Processing apparatus of organosilicon thick liquid sediment | |
| CN114032119A (en) | Safe, simple, efficient and environment-friendly tar purification and solid waste treatment system | |
| CN113415797A (en) | Aluminum electrolytic cell waste cathode carbon block treatment process | |
| CN209226803U (en) | A kind of resource reclaim processing system that oil sludge is innoxious | |
| CN216005580U (en) | Petroleum sludge cleaning and organic solvent recovery device | |
| CN215209043U (en) | System is abolished in parcel of oily sludge is washed to supersound heat | |
| CN103641073A (en) | Method and device for drying working solution in production of hydrogen peroxide of slurry reactor | |
| CN113845283A (en) | Process, device and method for cleaning and recovering petroleum sludge | |
| CN212999170U (en) | Tail gas recovery device of polyethylene antioxidant reaction kettle | |
| CN214881296U (en) | Integrated treatment equipment for acidified oil and aging oil |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20221116 Address after: 655000 building 7, Zhanhua Hotel, Xinglong company, Huashan street, Zhanyi District, Qujing City, Yunnan Province Applicant after: Yunnan nengtou Silicon Technology Development Co.,Ltd. Applicant after: SEDIN NINGBO ENGINEERING Co.,Ltd. Address before: 655000 building 7, Zhanhua Hotel, Xinglong company, Huashan street, Zhanyi District, Qujing City, Yunnan Province Applicant before: Yunnan nengtou Silicon Technology Development Co.,Ltd. |
|
| TA01 | Transfer of patent application right |