CN112604718A - Recovery process of residual liquid in high-boiling cracking reaction - Google Patents
Recovery process of residual liquid in high-boiling cracking reaction Download PDFInfo
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- B01J38/00—Regeneration or reactivation of catalysts, in general
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- B01J38/48—Liquid treating or treating in liquid phase, e.g. dissolved or suspended
- B01J38/64—Liquid treating or treating in liquid phase, e.g. dissolved or suspended using alkaline material; using salts
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- C07C7/04—Purification; Separation; Use of additives by distillation
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Abstract
The invention relates to a recovery process of residual liquid in a high-boiling cracking reaction. A process for recovering residual liquid in high-boiling cracking reaction includes: s10: stopping adding new high-boiling-point substances at the later stage of the high-boiling cracking reaction, heating, and distilling unreacted high-boiling-point substances out of the system; s20: after taking out the unreacted high boiling point substance, adding a new high boiling point substance, and continuing the cracking reaction until the reaction tends to stop; s30: repeating the steps S10 and S20 until the liquid level of the reaction kettle cannot be reduced, and discharging residues to obtain residual liquid; s40: adding a sodium hydroxide solution into the residual liquid, reacting, and cooling to obtain a neutral residual liquid; s50: adding an extracting agent into the neutral residual liquid for extraction, standing for layering, wherein the upper layer is an organic phase containing a high-boiling cracking catalyst; s60: distilling the organic phase, condensing and recovering to obtain an extracting agent, and leaving the catalyst. The process for recovering the residual liquid in the high-boiling cracking reaction reduces the discharge of unreacted substances, reduces the production cost and reduces the cost and difficulty of downstream sewage treatment.
Description
Technical Field
The invention belongs to the technical field of polycrystalline silicon, and particularly relates to a process for recovering residual liquid in a high-boiling cracking reaction.
Background
Polycrystalline silicon is a basic material of semiconductor and solar energy industries, and high-purity silicon materials show a short supply and demand situation in the global scope along with the rapid development of the photovoltaic industry. At present, the production process of the polycrystalline silicon internationally mainly comprises an improved Siemens method and a silane method, wherein the improved Siemens method is adopted for more than 70 percent. In the production process of producing high-purity silicon materials by the Siemens method, polymerization reaction of trichlorosilane and silicon tetrachloride occurs in the silicon rod deposition and cold hydrogenation processes, and a certain amount of high-boiling-point substances (polymeric chlorosilane) are produced as byproducts, wherein the main components of the high-boiling-point substances are tetrachlorodisilane, pentachloroethylsilane, hexachlorodisilane and the like. These high boiling substances are active in nature, and their hydrolyzates have pyrophoric properties and are extremely dangerous because they are pyrophoric even in water. Therefore, the mainstream polysilicon manufacturers have started research on recycling of high boiling substances.
At present, one mode of high-boiling recovery is high-boiling catalytic conversion, i.e. high-boiling substances are subjected to cracking reaction under the action of a catalyst to generate chlorosilane, and the chlorosilane is separated and purified to be used as a polycrystalline silicon production raw material. The high-boiling cracking catalyst in the high-boiling catalytic conversion is an organic amine substance. The high-boiling cracking catalyst part loses activity along with the reaction, and reaction residual liquid which cannot be catalytically cracked is continuously accumulated, so that the catalytic reaction cannot be continuously carried out. Therefore, impurities that cannot be catalytically cracked and the deactivated catalyst must be periodically removed to maintain the catalytic reaction efficiently.
The treatment of high boiling cracking catalyst is currently the main treatment method in the industry, which basically adopts hydrolysis process (also called catalytic raffinate hydrolysis method). The deactivated catalyst is discharged into a hydrolyzer along with the reaction residual liquid for hydrolysis, and then neutralized into neutral wastewater by alkaline liquid for direct discharge. But has the following disadvantages: (1) the discharge amount of residual liquid is large, so that the amount of unreacted waste is large, and resource waste is caused; (2) the catalyst which is not inactivated can be discharged along with the residual liquid, and the discharge amount of the residual liquid is large, so that the utilization rate of the catalyst is low; (3) the high-boiling catalyst is an organic amine substance, and if the high-boiling catalyst is directly hydrolyzed, neutralized and discharged, the content of ammonia nitrogen and COD in wastewater can be increased, and the cost and difficulty of downstream sewage treatment are increased.
In view of the above, the invention provides a novel recovery process of residual liquid in a high-boiling cracking reaction, which reduces resource waste.
Disclosure of Invention
The invention aims to provide a recovery process of residual liquid in a high-boiling cracking reaction, which is used for recovering unreacted substances and improving the recovery rate; the deactivated catalyst is recovered to reduce the emission of environmental pollutants.
In order to realize the purpose, the adopted technical scheme is as follows:
a recovery process of residual liquid in high-boiling cracking reaction comprises the following steps:
s10: in the later stage of the high-boiling cracking reaction, stopping adding new high-boiling substances into the reaction kettle, heating to 145-155 ℃, and distilling unreacted high-boiling substances out of the system;
s20: after unreacted high-boiling-point substances are taken out in the step S10, adding new high-boiling-point substances into the reaction kettle, and continuing the cracking reaction until the reaction tends to stop;
s30: repeating the steps S10 and S20 until the liquid level of the reaction kettle cannot be reduced, and discharging residues to obtain residual liquid;
s40: adding a sodium hydroxide solution into the residual liquid, fully reacting, and cooling to obtain a neutral residual liquid;
s50: adding an extracting agent into the neutral residual liquid, fully stirring, extracting, standing and layering, wherein the lower layer is a metal salt solution, and the upper layer is an organic phase containing a high-boiling cracking catalyst;
s60: distilling the organic phase, condensing and recovering to obtain an extracting agent, and leaving the catalyst.
Further, the temperature of the high-boiling cracking reaction is 120-130 ℃.
Further, in the step S10, the temperature is raised to 150 ℃.
Further, the unreacted high-boiling-point substance is chloro siloxane.
Further, in step S40, the concentration of the sodium hydroxide solution is 5-10%.
Further, the extracting agent is petroleum ether or toluene.
Further, the metal salt solution is discharged to a three-waste treatment system for treatment.
Furthermore, the recovery process adopts a recovery system of residual liquid in the high-boiling cracking reaction; the recovery system comprises: the system comprises a cracking reaction kettle 1, a cracking reaction kettle 2, a cracking rectification tower system, a neutralization reaction kettle, a residual liquid metering buffer tank, an extraction kettle and an extractant recovery system;
the cracking rectifying tower system comprises: a pyrolysis rectifying tower, a top condenser of the pyrolysis rectifying tower, a condensate intermediate tank at the top of the pyrolysis rectifying tower, a reflux pump of the pyrolysis rectifying tower and a top condenser of the condensate intermediate tank of the pyrolysis rectifying tower;
the extractant recovery system comprises: the system comprises an extractant evaporation kettle, an extractant condenser, an extractant tank, an extractant delivery pump and a catalyst cooling sleeve system;
the cracking reaction kettle 1 and the cracking reaction kettle 2 are connected in series with a cracking rectifying tower in the cracking rectifying tower system;
the cracking reaction kettle 1 and the cracking reaction kettle 2 are communicated with the residual liquid metering buffer tank, and the residual liquid metering buffer tank is used for collecting residual liquid in the cracking reaction kettle;
the residual liquid metering buffer tank is communicated with the neutralization reaction kettle, and the neutralization reaction kettle is used for neutralizing residual liquid;
the neutralization reaction kettle is communicated with the extraction kettle, and the extraction kettle is used for extracting neutral residual liquid;
the extraction kettle is communicated with the extractant recovery system, and the extractant recovery system is used for distilling and extracting layered upper organic phases.
Compared with the prior art, the invention has the beneficial effects that:
(1) reduce the discharge of unreacted substances and reduce the waste of resources.
(2) The catalyst is recycled, so that the production cost is reduced.
(3) The inactivated catalyst is recycled, the content of ammonia nitrogen and COD in the hydrolysis wastewater is reduced, and the cost and difficulty of downstream sewage treatment are reduced.
Drawings
FIG. 1 is a recovery system used in example 1 of the present invention; in the figure, 1 is a cracking reaction kettle 1, 2 is a cracking reaction kettle 2, 3 is a cracking rectification tower, 4 is a cooling condenser at the top of the cracking rectification tower, 5 is a cooling condenser at the top of a condensate intermediate tank of the cracking rectification tower, 6 is a condensate intermediate tank at the top of the cracking rectification tower, 7 is a residual liquid metering buffer tank, 8 is a high-boiling-point substance discharge pump, 9 is a reflux pump of the cracking rectification tower, 10 is a neutralization reaction kettle, 11 is an extraction kettle, 12 is an extraction agent evaporation kettle, 13 is an extraction agent condenser, 14 is an extraction agent tank, 15 is a catalyst cooling sleeve system, 16 is an extraction agent delivery pump, 17 is a waste catalyst box, 18 is an extraction agent box, and 19 is an extraction diaphragm pump.
Detailed Description
In order to further illustrate the process for recovering the raffinate from the high-boiling cracking reaction of the present invention and achieve the desired objects, the following embodiments are combined with the preferred embodiments to provide a process for recovering the raffinate from the high-boiling cracking reaction, the detailed description of the embodiments, structures, characteristics and effects thereof. In the following description, different "one embodiment" or "an embodiment" refers to not necessarily the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
The process for recovering the residual liquid from the high-boiling cracking reaction of the present invention will be described in further detail with reference to the following specific examples:
and (3) feeding the fresh high-boiling-point substances treated by the high-boiling-point substance pretreatment system into a reaction kettle, stirring and mixing the fresh high-boiling-point substances with a catalyst, heating, introducing a certain amount of HCL gas, and carrying out cracking reaction under a heating working condition. With the continuous progress of the reaction, trace metal impurities in the fresh high-boiling residues are accumulated continuously, so that the catalyst loses activity, the reaction efficiency is gradually reduced, and the reaction is finally stopped. At this time, it is necessary to take out the deactivated catalyst and the metal impurities accumulated in the system, and the reaction residual liquid composed of the unreacted high boiling substance, and to re-establish the reaction system to maintain the progress of the production.
The reaction residual liquid comprises inactivated catalyst, metal impurities, non-inactivated catalyst and non-reacted high-boiling-point substances, the invention carries out fractional recovery, and the technical scheme is as follows:
a recovery process of residual liquid in high-boiling cracking reaction comprises the following steps:
withdrawing unreacted high boiling components of S10: and stopping adding new high-boiling-point substances into the reaction kettle at the later stage of the high-boiling-point cracking reaction, heating to 145-155 ℃, and distilling unreacted high-boiling-point substances out of the system.
The high-boiling-point substances are mainly chloro-siloxane, can not be subjected to cracking reaction in a reaction kettle, but can be separated from residual liquid and returned to a polycrystalline silicon production system, and the high-boiling-point substances have good utilization value.
Recycling the catalyst without deactivation of S20: after the unreacted high boiling substance is taken out in the step S10, new high boiling substance is added into the reaction kettle, and the cracking reaction is continued until the reaction tends to stop.
After the unreacted high boiling point substance is taken out, the residual liquid mainly contains the catalyst which is not deactivated, a small part of deactivated catalyst and trace metal impurities. Because the content of the catalyst which is not deactivated is relatively high and the utilization value is high, fresh high-boiling-point substances can be added continuously to continue the cracking reaction until the reaction tends to stop.
S30: and repeating the steps S10 and S20 until the liquid level of the reaction kettle can not be reduced, which indicates that the reaction kettle can not receive fresh high-boiling residues any more, and residue removal is required to obtain residual liquid.
S40: and (3) residual liquid neutralization treatment: and adding a sodium hydroxide solution into the residual liquid to fully react substances such as chlorosiloxanes in the residual liquid, and cooling to obtain a neutral residual liquid.
S50: adding an extracting agent into the neutral residual liquid, fully stirring, extracting, standing and layering, wherein the lower layer is a metal salt solution, and the upper layer is an organic phase containing a high-boiling cracking catalyst;
s60: distilling the organic phase, condensing and recovering to obtain an extracting agent, and leaving the catalyst. The residual liquid which is not evaporated is most of the inactivated catalyst and a small part of the inactivated catalyst, and the residual liquid is barreled and returned to a catalyst manufacturer for recovery treatment.
Preferably, the temperature of the high-boiling cracking reaction is 120-130 ℃.
Preferably, in step S10, the temperature is raised to 150 ℃.
Preferably, the unreacted high boiling point material is chlorosiloxane.
Preferably, in step S40, the concentration of the sodium hydroxide solution is 5-10%.
Preferably, the extractant is petroleum ether or toluene.
Preferably, the metal salt solution is discharged to a three-waste treatment system for treatment.
Preferably, the recovery process adopts a recovery system of residual liquid in the high-boiling cracking reaction; the recovery system comprises: the system comprises a cracking reaction kettle 1, a cracking reaction kettle 2, a cracking rectification tower system, a neutralization reaction kettle, a residual liquid metering buffer tank, an extraction kettle and an extractant recovery system;
the cracking rectifying tower system comprises: a pyrolysis rectifying tower, a top condenser of the pyrolysis rectifying tower, a condensate intermediate tank at the top of the pyrolysis rectifying tower, a reflux pump of the pyrolysis rectifying tower and a top condenser of the condensate intermediate tank of the pyrolysis rectifying tower;
the extractant recovery system comprises: the system comprises an extractant evaporation kettle, an extractant condenser, an extractant tank, an extractant delivery pump and a catalyst cooling sleeve system;
the cracking reaction kettle 1 and the cracking reaction kettle 2 are connected in series with a cracking rectifying tower in the cracking rectifying tower system;
the cracking reaction kettle 1 and the cracking reaction kettle 2 are communicated with the residual liquid metering buffer tank, and the residual liquid metering buffer tank is used for collecting residual liquid in the cracking reaction kettle;
the residual liquid metering buffer tank is communicated with the neutralization reaction kettle, and the neutralization reaction kettle is used for neutralizing residual liquid;
the neutralization reaction kettle is communicated with the extraction kettle, and the extraction kettle is used for extracting neutral residual liquid;
the extraction kettle is communicated with the extractant recovery system, and the extractant recovery system is used for distilling and extracting layered upper organic phases.
Example 1.
The recovery system of fig. 1 is specifically adopted:
2 cracking reaction kettles, namely the cracking reaction kettle 1 and the cracking reaction kettle 2, are arranged in parallel and are connected with the cracking rectifying tower 3 in series, so that the cracking reaction kettles can be alternately used, and the reaction online rate of the reaction kettles is improved. The cracking reaction kettle uses 1.2MPa.G saturated steam or equivalent heat medium as heat medium.
Setting a cracking rectification tower system: comprises a cracking rectification tower 3, a cracking rectification tower top condenser 4, a cracking rectification tower top condensate intermediate tank 6, a cracking rectification tower reflux pump 9, a cracking rectification tower condensate intermediate tank top condenser 5 and a high-boiling-point substance discharge pump 8.
Setting a neutralization reaction kettle 10: fresh water and dilute alkali solution are added into the kettle, and neutralization reaction is carried out on the fresh water and the dilute alkali solution and the cracking residual liquid. The neutralization reaction kettle is an exothermic reaction and needs circulating cooling water or an equivalent cooling medium as a cooling medium.
And setting a residual liquid metering buffer tank 7: and the residual liquid after cracking is buffered, the influence on a former system is reduced, and the residual liquid amount added into the neutralization reaction kettle is accurately controlled in a small amount and multiple times.
Setting an extraction kettle 11: transferring the neutralized liquid to an extraction kettle, and adding an extracting agent for extraction. The extract and the metal brine were separated.
An extractant evaporating kettle 12, an extractant condenser 13, an extractant tank 14, an extractant conveying pump 16, a catalyst cooling sleeve and other systems 15, a waste catalyst box 17, an extractant box 18 and an extraction diaphragm pump 19 are arranged to separate the catalyst from the extractant. The heating medium of the extractant evaporating kettle uses 0.3MPa.G saturated steam or equivalent heating medium.
The specific operation steps are as follows:
(1) adding the high-boiling-point substance into a high-boiling-point cracking kettle, adding a catalyst according to a certain proportion, introducing HCL according to a certain proportion, heating the reaction kettle by using steam, and starting a cracking reaction at about 125 ℃. As the reaction proceeds, the high boiling substance is gradually replenished to keep the reaction continuing.
(2) The cracked steam is recycled through a cracked rectifying tower system, the non-condensable gas is condensed by a condenser 5 at the top of a condensate intermediate tank of the cracked rectifying tower to recycle the spray foam, three-waste treatment is carried out, and the product is sent to a polycrystalline silicon system for use.
(3) In the later stage of the high-boiling cracking reaction, the cracking residual liquid needs to be discharged and replaced by fresh high-boiling substances so as to maintain the continuous production. Firstly, separating unreacted high-boiling substances by the following operations: stopping adding new high-boiling-point substances into the reaction kettle, raising the temperature of the cracking reaction kettle to 150 +/-5 ℃ for continuous distillation, and simultaneously extracting the distillate by using a high-boiling-point substance discharging pump 8 to obtain unreacted high-boiling-point substances.
Meanwhile, fresh high-boiling-point material, catalyst and the like can be prepared for the standby cracking reaction kettle.
(4) When the unreacted high boiling point substance is distilled off basically, i.e. the liquid level of the reaction kettle is not reduced, the heating is stopped, and the residual liquid in the cracking reaction kettle is discharged into a residual liquid metering buffer tank 7.
(5) Adding fresh water into the neutralization reaction kettle 10, slowly adding NaOH, adjusting the pH to be alkalescent (the NaOH content in the alkali liquor is about 5-10%), slowly adding the residual liquor into the neutralization reaction kettle, and properly adjusting the pH to be neutral to obtain neutral residual liquor. In the process, cooling water is needed to be introduced into the neutralization reaction kettle for cooling, and the stirrer is started for stirring.
(6) And (3) after the neutralization is finished, transferring the neutral residual liquid to an extraction kettle 11, adding an extractant (the extractant is petroleum ether or toluene), starting stirring, introducing jacket cooling water for cooling, and standing for layering. The lower layer is metal salt solution, and the three wastes are directly discharged for treatment.
The catalyst enters the extractant, and is layered to form an upper organic phase layer. Multiple extractions may be performed to separate the catalyst from the extractant.
(7) The upper organic phase with the dissolved catalyst was transferred to an extractant evaporator. Heating the extractant evaporating kettle, evaporating the extractant, condensing by a condenser, recovering to an extractant tank, and recycling by an extractant conveying pump.
When the extractant is completely evaporated, only the catalyst is left in the extractant evaporating kettle, and the extractant evaporating kettle is cooled by a catalyst cooling sleeve and then barreled and returned to a catalyst manufacturer for recovery processing.
(8) And (5) repeating the steps (1) to (7) to realize continuous production operation.
The technical scheme of the embodiment of the invention is provided with the double cracking reaction kettle, the residual liquid metering tank, the neutralization reaction kettle, the extraction kettle and the extraction evaporation kettle, which are used for buffering and metering, thereby realizing the near-continuous operation of the system and improving the production reliability. The technical scheme of the embodiment of the invention can recycle unreacted high-boiling-point substances, reduce the discharge of unreacted substances and reduce the resource waste; the catalyst is recycled, so that the production cost is reduced; the inactivated catalyst is recycled, the content of ammonia nitrogen and COD in the wastewater caused by the hydrolysis catalyst is reduced, and the cost and difficulty of downstream sewage treatment are reduced.
Example 2.
The procedure of example 2 is the same as that of example 1, except for the following steps (3) to (4):
(3) in the later stage of the high-boiling cracking reaction, the cracking residual liquid needs to be discharged and replaced by fresh high-boiling substances so as to maintain the continuous production. Firstly, separating unreacted high-boiling substances by the following operations: stopping adding new high-boiling-point substances into the reaction kettle, raising the temperature of the cracking reaction kettle to 150 +/-5 ℃ for continuous distillation, and simultaneously extracting the distillate by using a high-boiling-point substance discharging pump to obtain unreacted high-boiling-point substances.
Adding new high-boiling-point substance into the cracking reaction kettle which takes out the unreacted high-boiling-point substance, and continuing the cracking reaction until the reaction tends to stop.
(4) And (4) repeating the step (3) until the liquid level of the reaction kettle can not be reduced, stopping heating, and completely discharging residual liquid in the cracking reaction kettle into a residual liquid metering buffer tank.
On the basis of the embodiment 1, unreacted high-boiling-point substances are heated, distilled, separated and recovered at the final stage of the cracking reaction, and are repeatedly fed and separated for multiple times, residues are intensively discharged until the operation is stopped, and the influence of the residue discharge on the production online rate can be reduced.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention are within the scope of the technical solution of the present invention.
Claims (8)
1. A recovery process of residual liquid in high-boiling cracking reaction is characterized by comprising the following steps:
s10: in the later stage of the high-boiling cracking reaction, stopping adding new high-boiling substances into the reaction kettle, heating to 145-155 ℃, and distilling unreacted high-boiling substances out of the system;
s20: after unreacted high-boiling-point substances are taken out in the step S10, adding new high-boiling-point substances into the reaction kettle, and continuing the cracking reaction until the reaction tends to stop;
s30: repeating the steps S10 and S20 until the liquid level of the reaction kettle cannot be reduced, and discharging residues to obtain residual liquid;
s40: adding a sodium hydroxide solution into the residual liquid, fully reacting, and cooling to obtain a neutral residual liquid;
s50: adding an extracting agent into the neutral residual liquid, fully stirring, extracting, standing and layering, wherein the lower layer is a metal salt solution, and the upper layer is an organic phase containing a high-boiling cracking catalyst;
s60: distilling the organic phase, condensing and recovering to obtain an extracting agent, and leaving the catalyst.
2. The recycling process according to claim 1,
the temperature of the high-boiling cracking reaction is 120-130 ℃.
3. The recycling process according to claim 1,
in step S10, the temperature is raised to 150 ℃.
4. The recycling process according to claim 1,
the unreacted high-boiling-point substance is chloro siloxane.
5. The recycling process according to claim 1,
in step S40, the concentration of the sodium hydroxide solution is 5-10%.
6. The recycling process according to claim 1,
the extractant is petroleum ether or toluene.
7. The recycling process according to claim 1,
and discharging the metal salt solution to a three-waste treatment system for treatment.
8. The recycling process according to claim 1,
the recovery process adopts a recovery system of residual liquid in the high-boiling cracking reaction; the recovery system comprises: the system comprises a cracking reaction kettle 1, a cracking reaction kettle 2, a cracking rectification tower system, a neutralization reaction kettle, a residual liquid metering buffer tank, an extraction kettle and an extractant recovery system;
the cracking rectifying tower system comprises: a pyrolysis rectifying tower, a top condenser of the pyrolysis rectifying tower, a condensate intermediate tank at the top of the pyrolysis rectifying tower, a reflux pump of the pyrolysis rectifying tower and a top condenser of the condensate intermediate tank of the pyrolysis rectifying tower;
the extractant recovery system comprises: the system comprises an extractant evaporation kettle, an extractant condenser, an extractant tank, an extractant delivery pump and a catalyst cooling sleeve system;
the cracking reaction kettle 1 and the cracking reaction kettle 2 are connected in series with a cracking rectifying tower in the cracking rectifying tower system;
the cracking reaction kettle 1 and the cracking reaction kettle 2 are communicated with the residual liquid metering buffer tank, and the residual liquid metering buffer tank is used for collecting residual liquid in the cracking reaction kettle;
the residual liquid metering buffer tank is communicated with the neutralization reaction kettle, and the neutralization reaction kettle is used for neutralizing residual liquid;
the neutralization reaction kettle is communicated with the extraction kettle, and the extraction kettle is used for extracting neutral residual liquid;
the extraction kettle is communicated with the extractant recovery system, and the extractant recovery system is used for distilling and extracting layered upper organic phases.
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1982004062A1 (en) * | 1981-05-13 | 1982-11-25 | Busch Lloyd E | A combination process for upgrading residual oils |
| CN103663460A (en) * | 2013-11-27 | 2014-03-26 | 新特能源股份有限公司 | Method and device for pyrolysis recycling of chlorosilane high-boiling residues in polycrystalline silicon production |
| CN204057977U (en) * | 2014-08-01 | 2014-12-31 | 江苏中能硅业科技发展有限公司 | For the apparatus system of halogen silicon polymer cracking for halosilanes |
| US20160053184A1 (en) * | 2012-07-23 | 2016-02-25 | Envirolles Inc. | Hybrid thermal process to separate and transform contaminated or uncontaminated hydrocarbon materials into useful products, uses of the process, manufacturing of the corresponding system and plant |
| CN205634908U (en) * | 2015-12-25 | 2016-10-12 | 内蒙古神舟硅业有限责任公司 | Raffinate height processing apparatus of thing that boils in polycrystalline silicon production |
| CN106188545A (en) * | 2016-08-30 | 2016-12-07 | 浙江中天氟硅材料有限公司 | Utilize the method that organosilicon high-boiling product prepares inertia high boiling point silicon oil |
| CN107098826A (en) * | 2017-05-18 | 2017-08-29 | 常州冀德环保科技有限公司 | The ten towers six effect distillation system and recovery method of a kind of DMAC or DMF waste liquids |
| CN110314515A (en) * | 2019-04-29 | 2019-10-11 | 新疆大全新能源股份有限公司 | The processing system and processing method of silicon powder residue in a kind of production of trichlorosilane |
| CN112010823A (en) * | 2019-05-29 | 2020-12-01 | 中国石油化工股份有限公司 | Alkylene oxide separation and benzyl alcohol purification method |
-
2020
- 2020-12-24 CN CN202011548720.3A patent/CN112604718B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1982004062A1 (en) * | 1981-05-13 | 1982-11-25 | Busch Lloyd E | A combination process for upgrading residual oils |
| US20160053184A1 (en) * | 2012-07-23 | 2016-02-25 | Envirolles Inc. | Hybrid thermal process to separate and transform contaminated or uncontaminated hydrocarbon materials into useful products, uses of the process, manufacturing of the corresponding system and plant |
| CN103663460A (en) * | 2013-11-27 | 2014-03-26 | 新特能源股份有限公司 | Method and device for pyrolysis recycling of chlorosilane high-boiling residues in polycrystalline silicon production |
| CN204057977U (en) * | 2014-08-01 | 2014-12-31 | 江苏中能硅业科技发展有限公司 | For the apparatus system of halogen silicon polymer cracking for halosilanes |
| CN205634908U (en) * | 2015-12-25 | 2016-10-12 | 内蒙古神舟硅业有限责任公司 | Raffinate height processing apparatus of thing that boils in polycrystalline silicon production |
| CN106188545A (en) * | 2016-08-30 | 2016-12-07 | 浙江中天氟硅材料有限公司 | Utilize the method that organosilicon high-boiling product prepares inertia high boiling point silicon oil |
| CN107098826A (en) * | 2017-05-18 | 2017-08-29 | 常州冀德环保科技有限公司 | The ten towers six effect distillation system and recovery method of a kind of DMAC or DMF waste liquids |
| CN110314515A (en) * | 2019-04-29 | 2019-10-11 | 新疆大全新能源股份有限公司 | The processing system and processing method of silicon powder residue in a kind of production of trichlorosilane |
| CN112010823A (en) * | 2019-05-29 | 2020-12-01 | 中国石油化工股份有限公司 | Alkylene oxide separation and benzyl alcohol purification method |
Non-Patent Citations (3)
| Title |
|---|
| LAURA P. TOVAR等: "Centrifugal Reactive-Molecular Distillation from High-Boiling-Point Petroleum Fractions. 1. Mathematical Modeling, Screening Variables,and Experimental Validation", 《INDUSTRIAL & ENGINEERING CHEMISTRY RESEARCH》 * |
| 李晓光等: "有机硅高沸物乙氧基酯化中残液的再利用工艺研究", 《弹性体》 * |
| 王海霞等: "多晶硅副产物综合处理研究进展", 《化工管理》 * |
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