CN110330521A - A kind of organosilicon slag slurry processing method - Google Patents
A kind of organosilicon slag slurry processing method Download PDFInfo
- Publication number
- CN110330521A CN110330521A CN201910486108.9A CN201910486108A CN110330521A CN 110330521 A CN110330521 A CN 110330521A CN 201910486108 A CN201910486108 A CN 201910486108A CN 110330521 A CN110330521 A CN 110330521A
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- China
- Prior art keywords
- slag slurry
- solid
- organosilicon slag
- processing method
- organosilicon
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- 239000002002 slurry Substances 0.000 title claims abstract description 40
- 239000002893 slag Substances 0.000 title claims abstract description 38
- 238000003672 processing method Methods 0.000 title claims abstract description 20
- YGZSVWMBUCGDCV-UHFFFAOYSA-N chloro(methyl)silane Chemical compound C[SiH2]Cl YGZSVWMBUCGDCV-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000009835 boiling Methods 0.000 claims abstract description 29
- 239000007788 liquid Substances 0.000 claims abstract description 25
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 20
- 230000002779 inactivation Effects 0.000 claims abstract description 20
- 239000000178 monomer Substances 0.000 claims abstract description 19
- 239000007787 solid Substances 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000005046 Chlorosilane Substances 0.000 claims abstract description 11
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052802 copper Inorganic materials 0.000 claims abstract description 10
- 239000010949 copper Substances 0.000 claims abstract description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 10
- 238000005336 cracking Methods 0.000 claims abstract description 7
- 238000004064 recycling Methods 0.000 claims abstract description 7
- 238000004821 distillation Methods 0.000 claims abstract description 6
- 239000007790 solid phase Substances 0.000 claims abstract 2
- 230000008707 rearrangement Effects 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910000077 silane Inorganic materials 0.000 claims description 2
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 claims 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000001704 evaporation Methods 0.000 claims 1
- 229940050176 methyl chloride Drugs 0.000 claims 1
- 238000007790 scraping Methods 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 abstract description 15
- 239000010703 silicon Substances 0.000 abstract description 15
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 12
- 238000000034 method Methods 0.000 abstract description 8
- 239000000126 substance Substances 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000009833 condensation Methods 0.000 abstract description 3
- 230000005494 condensation Effects 0.000 abstract description 3
- 231100001261 hazardous Toxicity 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000007789 gas Substances 0.000 abstract description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 abstract description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 230000002194 synthesizing effect Effects 0.000 description 4
- VABRONYHMNKEFB-UHFFFAOYSA-N chloromethane;silicon Chemical compound [Si].ClC VABRONYHMNKEFB-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- OGFYGJDCQZJOFN-UHFFFAOYSA-N [O].[Si].[Si] Chemical compound [O].[Si].[Si] OGFYGJDCQZJOFN-UHFFFAOYSA-N 0.000 description 1
- QZOVMCPHIQVUGV-UHFFFAOYSA-N [Si].[C].[Si] Chemical compound [Si].[C].[Si] QZOVMCPHIQVUGV-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000007701 flash-distillation Methods 0.000 description 1
- 239000010808 liquid waste Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- -1 methyl chloride silicon Alkane Chemical class 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- SBEQWOXEGHQIMW-UHFFFAOYSA-N silicon Chemical compound [Si].[Si] SBEQWOXEGHQIMW-UHFFFAOYSA-N 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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
- C07F7/12—Organo silicon halides
-
- 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
- C07F7/20—Purification, separation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
Abstract
The invention discloses a kind of safe and environment-friendly organosilicon slag slurry processing methods, and using efficient slurry solid-liquid separator, organosilicon synthesis slurry is carried out solid and liquid separation.It is the following steps are included: A, being synthetically produced organosilicon slag slurry for methyl chlorosilane monomer using nitrogen and being delivered to closed solid-liquid separator；B, organosilicon slag slurry heats in closed solid-liquid separator, distills higher boiling methylchlorosilane under vacuum and stirring condition, and the gaseous state methylchlorosilane isolated is collected by condenser condensation；C, higher boiling methylchlorosilane is converted into chlorosilane crude monomer by cracking, resetting, and the solid phase residue slag of distillation drains into inactivation reaction kettle and after inactivation, recycling metallic copper therein, and remaining silicon slag can take out brickmaking or ironmaking use after mentioning copper.After adopting the above method, anhydrous participation reaction in whole process, no hydrogen chloride gas generates, and safe, corrosion-free to equipment, non-hazardous to environment, all residues all recycle, and meets the environmental protection concept of green chemical industry.
Description
Technical field
The present invention relates to a kind of organic silicon chemical residue environmental protection treatment technology, at specifically a kind of organosilicon slag slurry
Reason method.
Background technique
Organosilicon slag slurry is generated solid-liquid mixing in organic silicon monomer especially methyl chlorosilane monomer synthesis process
Object is high mainly by a large amount of higher boiling methyl chlorosilane monomer and a small amount of fluidized bed take unreacted silicon powder out of, copper powder forms
Boiling point methyl chlorosilane monomer is 150~250 DEG C of boiling range generated in synthesis process, with silicon-silicon key, silicon-carbon-silicon key,
Higher boiling multi-silane mixture based on silicon-oxygen-silicon.If the exposure of this partial material is in air, it will burn or be formed strong
Acid mist or liquid, so if direct emission can cause environment seriously to pollute, it is necessary to carry out Harmless processing.
Currently, manufacturing enterprise is all to be recycled the lower substance of its mid-boiling point by flash distillation to the processing method of slurry, contain
Liquid waste residue, which is directly discharged into water, to be hydrolyzed.Existing this processing method does not only recycle organosilicon high-boiling product a large amount of in slurry
Utilize, cause a large amount of wastes of efficient resource, it is often more important that high-boiling components in slurry, meet air or open fire can cause fire or
Explosion, brings serious security risk.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of recycling safety, corrosion-free to equipment, it is non-hazardous to environment and
The organosilicon slag slurry processing method that whole residues can be recycled.
In order to solve the above-mentioned technical problem, organosilicon slag slurry processing method of the invention, comprising the following steps:
A, methyl chlorosilane monomer is synthetically produced organosilicon slag slurry using nitrogen and is delivered to efficient solid-liquid separator；
B, organosilicon slag slurry heats in closed solid-liquid separator, distills out higher boiling methyl chloride silicon under vacuum and stirring condition
Alkane, the gaseous state methyl chloride silicon isolated are collected by condenser condensation；
C, higher boiling methylchlorosilane is converted to the recycling of methylchlorosilane crude monomer by cracking, rearrangement, can also directly give birth to
High boiling point silicon oil is produced, for producing high-temperature-resistant silicon resin.Remaining solid residue drains into inactivation reaction kettle and inactivation processing.
In the step C, solid residue is after reacting inactivation with the alkaline deactivator in inactivation reaction kettle, recycling
Wherein metallic copper.
The pressure of the nitrogen is 0.1~0.8MPa.
The solid-liquid separator is a kind of stirring distiller for efficiently having scraper type, and scraper is in vertical direction and stirring
Axis is in 45~80 ° of angles.
In the step B distill heating temperature be 200~300 DEG C, the distillation vacuum degree for -0. 06MPa~-
0.1MPa。
Condensation temperature is 0~25 DEG C in the step B.
The solid residue and alkaline deactivator mass ratio: 1/1~1/5.
Solid content 10-40% in the organosilicon slag slurry.
After adopting the above method, organosilicon slag slurry is delivered to closed solid-liquid separator using nitrogen, heating, vacuum with
Higher boiling methylchlorosilane is distilled under stirring condition, the chlorosilane high-boiling components isolated are cracked, are reset and be converted to methyl chloride silicon
Alkane crude monomer, remaining solid residue drain into inactivation reaction kettle, can be directly for profession after reacting with deactivator and neutralizing inactivation
Producer recycles metallic copper, and the silicon slag after mentioning copper can innoxious brickmaking processing；Anhydrous participation reaction, no hydrogen chloride gas in whole process
Body generates, safe, corrosion-free to equipment, non-hazardous to environment, and all residues all recycle, and meets the ring of green chemical industry
Factoring is read.
Detailed description of the invention
Fig. 1 is organosilicon slag slurry processing equipment schematic diagram in the present invention.
Specific embodiment
With reference to the accompanying drawings and detailed description, organosilicon slag slurry processing method of the invention is made further specifically
It is bright.
Embodiment one:
As shown, the organosilicon slag slurry processing method of the present embodiment, comprising the following steps:
A, methyl chlorosilane monomer synthesizing organo-silicon slurry 1000kg (solid content 11%) utilizes nitrogen (pressure via rectifying workshop
It 0.3MPa) is delivered to closed solid-liquid separator 1, solid-liquid separator is the stirring distiller with scraper type, and scraper is in Vertical Square
To being in 45 ° of angles with agitating shaft, has stirring concurrently and squeeze fortune effect.Wherein, organosilicon slag slurry is methylchlorosilane high-boiling components and silicon
The mixture of powder, copper powder and other metal powders；Wherein, the operation temperature 200~300 of the distiller with scraper type stirring
DEG C, it is operated under vacuum condition, under the high temperature conditions, equipment No leakage.
B, vapo(u)rizing temperature is heated in closed solid-liquid separator to be 280 DEG C, distill vacuum degree for -0.65MPa and mixing speed
To distill higher boiling methylchlorosilane under the conditions of 30r/min, the gaseous state methylchlorosilane isolated is cold by secondary condenser 2(
Solidifying temperature is 25 DEG C) it collects and obtains chlorosilane high-boiling components 880kg；
C, higher boiling methylchlorosilane is converted to chlorosilane crude monomer by cracking, rearrangement, and remaining solid residue 120kg is drained into
In inactivation reaction kettle 3, after inactivation is reacted with alkaline deactivator (140kg), it is sold to specialized factory outside and recycles metallic copper therein, it is residual
Remaining silicon slag brickmaking processing.
Embodiment two:
As shown, the organosilicon slag slurry processing method of the present embodiment, comprising the following steps:
A, methyl chlorosilane monomer synthesizing organo-silicon slurry 1000kg (solid content 20%) utilizes nitrogen (pressure via rectifying workshop
It 0.5MPa) is delivered to closed solid-liquid separator 1, solid-liquid separator is the stirring distiller with scraper type, and scraper is in Vertical Square
To being in 45 ° of angles with agitating shaft, has stirring concurrently and squeeze fortune effect；
B, heat that vapo(u)rizing temperature is 220 DEG C, distillation vacuum degree is that -0.08MPa is with mixing speed in closed solid-liquid separator
Higher boiling methylchlorosilane is distilled under the conditions of 30r/min, the gaseous state methylchlorosilane isolated is condensed by secondary condenser 2(
Temperature be 25 DEG C) collect obtain chlorosilane high-boiling components 780kg；
C, higher boiling methylchlorosilane is converted to chlorosilane crude monomer by cracking, rearrangement, and remaining solid residue 240kg is drained into
In inactivation reaction kettle 3, after inactivation is reacted with alkaline deactivator (500kg), it is sold to specialized factory outside and recycles metallic copper therein, it is residual
Remaining silicon slag brickmaking processing.
Embodiment three:
As shown, the organosilicon slag slurry processing method of the present embodiment, comprising the following steps:
A, methyl chlorosilane monomer synthesizing organo-silicon slurry 1000kg (solid content 29%) utilizes nitrogen (pressure via rectifying workshop
It 0.5MPa) is delivered to closed solid-liquid separator 1, solid-liquid separator is the stirring distiller with scraper type, and scraper is in Vertical Square
To being in 45 ° of angles with agitating shaft, has stirring concurrently and squeeze fortune effect；
B, heat that vapo(u)rizing temperature is 300 DEG C, distillation vacuum degree is that -0.095MPa is with mixing speed in closed solid-liquid separator
Higher boiling methylchlorosilane is distilled under the conditions of 30r/min, the gaseous state methylchlorosilane isolated is condensed by secondary condenser 2(
Temperature be 25 DEG C) collect obtain chlorosilane high-boiling components 700kg；
C, higher boiling methylchlorosilane is converted to chlorosilane crude monomer by cracking, rearrangement, and remaining solid residue 300kg is drained into
In inactivation reaction kettle 3, after inactivation is reacted with alkaline deactivator (900kg), it is sold to specialized factory's recycling wherein metallic copper outside, it is remaining
Silicon slag brickmaking processing.
Example IV:
As shown, the organosilicon slag slurry processing method of the present embodiment, comprising the following steps:
A, methyl chlorosilane monomer synthesizing organo-silicon slurry 1000kg (solid content 39%) utilizes nitrogen (pressure via rectifying workshop
It 0.5MPa) is delivered to closed solid-liquid separator 1, solid-liquid separator is the stirring distiller with scraper type, and scraper is in Vertical Square
To being in 45 ° of angles with agitating shaft, has stirring concurrently and squeeze fortune effect；
B, heat that vapo(u)rizing temperature is 300 DEG C, distillation vacuum degree is that -0.095MPa is with mixing speed in closed solid-liquid separator
Higher boiling methylchlorosilane is distilled under the conditions of 30r/min, the gaseous state methylchlorosilane isolated is condensed by secondary condenser 2(
Temperature be 25 DEG C) collect obtain chlorosilane high-boiling components 600kg；
C, higher boiling methylchlorosilane is converted to chlorosilane crude monomer by cracking, rearrangement, and remaining solid residue 400kg is drained into
In inactivation reaction kettle 3, after inactivation is reacted with alkaline deactivator (1200kg), it is sold to specialized factory's recycling wherein metallic copper outside, it is residual
Remaining silicon slag brickmaking processing.
Claims (8)
1. a kind of processing method of organosilicon slag slurry, comprising the following steps:
A, closed solid-liquid separator is delivered to using the organosilicon slag slurry that methyl chlorosilane monomer is synthetically produced by nitrogen；
B, organosilicon slag slurry is in closed solid-liquid separator by distilling high boiling methyl chloride under heating, vacuum and stirring condition
Silane, the gaseous state methylchlorosilane isolated pass through the collection of at least one level condenser；
C, the higher boiling chlorosilane of collection is converted to methylchlorosilane crude monomer by cracking, rearrangement, distills remaining solid phase residue
Object drains into inactivation reaction kettle and inactivation processing.
2. organosilicon slag slurry processing method described in accordance with the claim 1, it is characterised in that: in the step C, by with inactivation
After alkaline deactivator reaction inactivation in reaction kettle, recycling metallic copper therein.
3. organosilicon slag slurry processing method according to claim 1 or 2, it is characterised in that: the pressure of nitrogen in the step A
Power is 0.1MPa~0.8MPa.
4. organosilicon slag slurry processing method described in accordance with the claim 3, it is characterised in that: the solid-liquid separator is with scraping
The distiller of blade stirring, scraper are in 45~80 ° of angles in vertical direction and agitating shaft.
5. according to organosilicon slag slurry processing method described in claim 1,2 or 4, it is characterised in that: heat and steam in the step B
Evaporating temperature is 200~300 DEG C, and the distillation vacuum degree is -0.06MPa~-0.1MPa.
6. organosilicon slag slurry processing method according to claim 5, it is characterised in that: condenser is cold in the step B
Solidifying temperature is 0~25 DEG C.
7. organosilicon slag slurry processing method according to claim 6, it is characterised in that: the solid residue and alkalinity are lost
Agent mass ratio living: 1/1~1/5.
8. organosilicon slag slurry processing method according to claim 7, it is characterised in that: the solid in the organosilicon slag slurry
Content 10-40%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910486108.9A CN110330521A (en) | 2019-06-05 | 2019-06-05 | A kind of organosilicon slag slurry processing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910486108.9A CN110330521A (en) | 2019-06-05 | 2019-06-05 | A kind of organosilicon slag slurry processing method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110330521A true CN110330521A (en) | 2019-10-15 |
Family
ID=68141179
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CN201910486108.9A Pending CN110330521A (en) | 2019-06-05 | 2019-06-05 | A kind of organosilicon slag slurry processing method |
Country Status (1)
| Country | Link |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114292288A (en) * | 2021-12-13 | 2022-04-08 | 华陆工程科技有限责任公司 | Method for treating synthetic reaction slurry in production of methyl silicate by directly synthesizing silicon powder |
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| CN101386626A (en) * | 2008-10-31 | 2009-03-18 | 江苏宏达新材料股份有限公司 | Organosilicon slag slurry treatment method and apparatus thereof |
| CN102174674A (en) * | 2011-03-11 | 2011-09-07 | 上海竟茨环保科技有限公司 | Processing and recycling process for silicon slurry |
| CN103408023A (en) * | 2013-07-19 | 2013-11-27 | 中国恩菲工程技术有限公司 | Method and equipment for treatment of chlorosilane-containing waste liquid |
| CN105037414A (en) * | 2015-07-29 | 2015-11-11 | 湖北兴瑞化工有限公司 | Method and device for recovering efficient high-boiling substance from organic silicon residue slurry |
| CN106220666A (en) * | 2016-07-18 | 2016-12-14 | 聊城市鲁西化工工程设计有限责任公司 | The processing system of a kind of organic silicon slurry slag and processing method |
| CN108558928A (en) * | 2018-05-09 | 2018-09-21 | 成都斯力康科技股份有限公司 | A kind of method and apparatus of organosilicon slag slurry synthetical recovery processing |
-
2019
- 2019-06-05 CN CN201910486108.9A patent/CN110330521A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101386626A (en) * | 2008-10-31 | 2009-03-18 | 江苏宏达新材料股份有限公司 | Organosilicon slag slurry treatment method and apparatus thereof |
| CN102174674A (en) * | 2011-03-11 | 2011-09-07 | 上海竟茨环保科技有限公司 | Processing and recycling process for silicon slurry |
| CN103408023A (en) * | 2013-07-19 | 2013-11-27 | 中国恩菲工程技术有限公司 | Method and equipment for treatment of chlorosilane-containing waste liquid |
| CN105037414A (en) * | 2015-07-29 | 2015-11-11 | 湖北兴瑞化工有限公司 | Method and device for recovering efficient high-boiling substance from organic silicon residue slurry |
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| CN114292288A (en) * | 2021-12-13 | 2022-04-08 | 华陆工程科技有限责任公司 | Method for treating synthetic reaction slurry in production of methyl silicate by directly synthesizing silicon powder |
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Application publication date: 20191015 |