CN113831361A - Energy-saving methyl chlorosilane mixed crude monomer pre-separation method - Google Patents
Energy-saving methyl chlorosilane mixed crude monomer pre-separation method Download PDFInfo
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- CN113831361A CN113831361A CN202110870527.XA CN202110870527A CN113831361A CN 113831361 A CN113831361 A CN 113831361A CN 202110870527 A CN202110870527 A CN 202110870527A CN 113831361 A CN113831361 A CN 113831361A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/12—Organo silicon halides
- C07F7/121—Preparation or treatment not provided for in C07F7/14, C07F7/16 or C07F7/20
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/383—Separation; Purification; Stabilisation; Use of additives by distillation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention discloses an energy-saving methyl chlorosilane mixed crude monomer pre-separation method. After raw materials enter a crude monomer pre-separation tower, extracting crude methyl chlorosilane monomers from the bottom of the tower, partially condensing vapor at the top of the tower, completely refluxing a liquid phase, and conveying a gas phase to a methyl chloride recovery tower to separate and recover methyl chloride; the condenser of the methyl chloride recovery tower discharges non-condensable gas, the methyl chloride is recovered from the top of the tower or the side line of the tower, and liquid extracted from the bottom of the tower flows back to the crude monomer pre-separation tower. Compared with the traditional methyl chlorosilane mixed crude monomer pre-separation method, the method can use the cold energy of low-grade public works or process materials in a crude monomer tower condenser, and simultaneously reduce the equipment size of the crude monomer pre-separation tower and a methyl chloride recovery tower, thereby saving investment and operation cost and creating benefits for enterprises.
Description
Technical Field
The invention belongs to the technical field of organic silicon separation, and particularly relates to a pre-separation method of a methyl chlorosilane mixed crude monomer.
Background
In the current organic silicon production process, a monomer synthesis device adopts the reaction of methane chloride and silicon powder to synthesize a methyl chlorosilane mixed monomer (hereinafter referred to as a crude monomer), a reaction product is subjected to dust removal washing and part of heavy components are removed, the methyl chlorosilane mixed crude monomer containing the crude monomer, the methane chloride and noncondensable gas enters a crude monomer tower for pre-separation, in the current industrial production, the crude monomer generated by the reaction is subjected to pre-separation by adopting the flow shown in fig. 1, the liquid methane chloride is separated and extracted at the top of the tower and returns to a feeding system for gasification and recycling, the noncondensable gas in the gas phase at the top of the tower is discharged into a tail gas system, and the crude monomer extracted at the bottom of the tower enters a monomer separation device for further separation and purification.
As shown in fig. 1, in the conventional process, the operating pressure of the crude monomer tower is generally 0.5-1.0 MPaG, and at this time, the temperature difference of the tower top and the tower bottom is as high as 124 ℃, which belongs to a typical rectification system of wide boiling range materials. The tower top generally adopts chilled water with the temperature of-15 ℃, the tower bottom needs to adopt 1.0MPaG steam as a heat source, the energy consumption of each ton of product is 885.8kg/h of standard oil, and the energy consumption is larger.
Disclosure of Invention
The invention aims to provide an energy-saving methyl chlorosilane mixed crude monomer pre-separation method, which comprises the steps of splitting an original crude monomer tower into a crude monomer pre-separation tower and a chloromethane recovery tower, additionally arranging a crude monomer pre-separation tower condenser, reducing separation energy consumption by adopting public engineering or process materials with lower heat level, reducing operation cost and simultaneously reducing the size of tower equipment.
The technical scheme is that the energy-saving methyl chlorosilane mixed crude monomer pre-separation device is characterized by comprising a crude monomer pre-separation tower and a methyl chloride recovery tower, wherein a crude monomer pre-separation tower condenser is arranged on a gas phase connecting pipeline of the two towers, a crude monomer pre-separation tower reboiler is arranged at the bottom of the crude monomer pre-separation tower, a methyl chloride recovery tower condenser is arranged at the top of the methyl chloride recovery tower, and the liquid in the methyl chloride recovery tower is pumped to the top of the crude monomer pre-separation tower through a middle reflux pump.
An energy-saving methyl chlorosilane mixed crude monomer pre-separation method is characterized in that the device in claim 1 is utilized, after methyl chlorosilane mixed crude monomer enters a crude monomer pre-separation tower, methyl chlorosilane crude monomer is extracted from the bottom of the tower, vapor at the top of the tower is partially condensed, liquid phase of the vapor completely reflows, and gas phase of the vapor is sent to a methyl chloride recovery tower to separate and recover methyl chloride; and (3) discharging non-condensable gas from a condenser of the methyl chloride recovery tower, recovering methyl chloride from the top of the tower or a side line of the tower, and refluxing liquid extracted from the tower kettle to the top of the crude monomer pre-separation tower.
Further, the number of plates of the crude monomer pre-separation tower is 10-90, the feeding position is between the 5 th plate and the 80 th plate, and the operating pressure is 0.4 MPaG-2.0 MPaG; the number of plates of the methyl chloride recovery tower is 5-90, the feeding position is the bottom of the tower, gas phase feeding is carried out, and the operation pressure is 0.4-2.0 MPaG.
Further, the overhead condenser of the crude monomer pre-separation column only partially condenses; the cold side medium is selected from circulating water or other suitable public engineering media or process media.
Furthermore, a side branch pipeline which directly enters the bottom of the methyl chloride recovery tower from the top of the crude monomer pre-separation tower is additionally arranged, so that steam at the top of the crude monomer pre-separation tower directly enters the side branch pipeline at the bottom of the methyl chloride recovery tower, and sufficient gas flow in the methyl chloride recovery tower is ensured by adjusting the flow of the side branch pipeline, and the running stability of the device is enhanced.
Compared with the existing methyl chlorosilane mixed crude monomer pre-separation process, the method utilizes the characteristic of a wide boiling range of a separation system of a crude monomer tower to split the crude monomer tower into the crude monomer pre-separation tower and a methyl chloride recovery tower, a crude monomer pre-separation tower condenser is arranged on a gas phase connecting pipeline of the two towers, and the cold load required by the original crude monomer tower is distributed to the crude monomer pre-separation tower condenser and the methyl chloride recovery tower condenser. The crude monomer pre-separation tower condenser can use the cold energy of low-grade public works or engineering process materials, so that the crude monomer can be initially cooled under the condition that a low-grade cold source can be used, the heat load of the condenser of a subsequent methyl chloride recovery part is reduced, the process energy consumption is reduced, the investment and the operation cost are saved, and the benefit is created for enterprises.
Meanwhile, by adopting the method, the maximum flow of the gas phase of the crude monomer pre-separation tower and the maximum flow of the gas phase of the chloromethane recovery tower can be reduced simultaneously, and the gas-liquid load distribution in the tower is more reasonable, so that the size of equipment is reduced, and the equipment investment and the occupied area are reduced.
Drawings
FIG. 1 is a flow diagram of a conventional crude monomer pre-separation process.
FIG. 2 is a flow chart of an energy-saving pre-separation method of methyl chlorosilane mixed crude monomers.
FIG. 3 is a flow chart of an improved energy-saving method for pre-separation of crude methyl chlorosilane mixture monomers.
Detailed Description
The operational characteristics of the techniques and equipment involved in the present invention are further described below in conjunction with the appended drawings.
The original crude monomer tower shown in figure 1 is split into a crude monomer pre-dividing tower and a chloromethane recovery tower. Wherein, the crude monomer pre-separation tower is used for separating crude chloromethane and crude monomers, and only the tower bottom is required to contain no chloromethane; the methyl chloride recovery tower is used for purifying crude methyl chloride from the crude monomer pre-separation tower, and a reboiler is not arranged at the bottom of the tower.
As shown in fig. 2, after the methyl chlorosilane mixed crude monomer enters a crude monomer pre-separation tower, the methyl chlorosilane crude monomer is extracted from the bottom of the tower, vapor at the top of the tower is partially condensed, a liquid phase completely reflows, and a gas phase is sent to a methyl chloride recovery tower to separate and recover methyl chloride; and (3) discharging non-condensable gas from a condenser of the methyl chloride recovery tower, recovering methyl chloride from the top of the tower or a side line of the tower, and refluxing liquid extracted from the tower kettle to the top of the crude monomer pre-separation tower.
The number of theoretical plates of the crude monomer pre-separation tower is 10-90, the feeding position is between the 5 th theoretical plate and the 80 th theoretical plate (the theoretical plates are numbered from the top of the tower to the bottom of the tower in sequence), and the operating pressure is 0.4 MPaG-2.0 MPaG; the number of theoretical plates of the methyl chloride recovery tower is 5-90, the feeding position is the bottom of the tower, gas phase feeding is carried out, and the operation pressure is 0.4-2.0 MPaG.
The overhead condenser of the crude monomer pre-separation tower only partially condenses; the cold side media can be recycled water or other suitable utility or process media.
In practical implementation, the gas flow of the methyl chloride recovery tower is too small to normally operate due to the condition of temperature change or cold quantity change of a condenser at the top of the crude monomer pre-separation tower. The improved method proposed by the present invention is therefore shown in fig. 3. The method is characterized in that a side branch pipeline which directly enters the bottom of the methyl chloride recovery tower from the top of the crude monomer pre-separation tower is additionally arranged, so that the method can ensure that enough gas flow and proper operation temperature exist in the methyl chloride recovery tower in a bypass flow adjusting mode, and the operation stability of the device is enhanced.
A certain organic silicon monomer synthesis workshop is reformed by adopting the method of the invention, and the conditions are as follows:
the crude monomer liquid phase and the crude monomer vapor phase enter the crude monomer pre-splitter column from an upstream device and the feed data are as follows. The theoretical plate number of the crude monomer pre-separation tower is 50, the operation pressure at the top of the tower is 1.0MPaG, the theoretical plate number of the methyl chloride recovery tower is 20, the operation pressure at the top of the tower is 0.9MPaG, the outlet temperature of a condenser of the recovery tower is-3.5 ℃, and the cooling is carried out by using chilled water at the temperature of-15 ℃. The reboiler outlet temperature of the column bottom was 163 ℃ and heating was carried out using 1.0MPaG steam.
Before reforming, the flow scheme only has a crude monomer tower as shown in figure 1; after transformation, the crude monomer is separated into a separation unit consisting of a crude monomer pre-separation tower and a chloromethane recovery tower as shown in fig. 2, wherein a pre-separation tower condenser uses circulating water as a cooling medium.
The separation indexes before modification all meet the requirements, and the energy consumption indexes are shown in the following table:
| device name | Material inlet/outlet temperature | Name of public works | Unit of | Thermal load | Remarks for note |
| Crude monomer tower condenser | 41.3℃/-4.1℃ | Freezing water at-15 deg.C | MJ/h | 17205.8 | |
| Crude monomer tower reboiler | 163.4℃/163.4℃ | 1.0MPaG steam | Kg/h | 6221.5 | 12443MJ/h |
The separation indexes after modification all meet the requirements, and the energy consumption indexes are shown in the following table:
| device name | Material inlet/outlet temperature | Name of public works | Unit of | Thermal load | Remarks for note |
| Pre-dividing tower condenser | 44.3℃/41.6℃ | Circulating water at 32 DEG C | t/h | 333.5 | 8375MJ/h |
| Condenser of recovery tower | 39.8℃/-3.5℃ | Freezing water at-15 deg.C | MJ/h | 8902.6 | |
| Pre-separation tower reboiler | 163.4℃/163.4℃ | 1.0MPaG steam | Kg/h | 6221.5 | 12443MJ/h |
According to the national standard GB/T50441-2007 petrochemical engineering design energy consumption calculation standard, the energy conversion value (kg standard oil) of the used public engineering is as follows: circulating water 0.10 kg/t; the cold energy at the temperature of minus 15 ℃ is 0.024 kg/MJ; 1.0MPaG grade steam 76 kg/t. The energy consumption of the process without the method is 885.8kg/h standard oil, and the hourly energy conversion value is 698.6kg/h standard oil after the method is adopted for transformation, so that the comprehensive energy conservation of 21 percent is realized.
In addition, the diameter of the crude monomer column without the process proposed by the present invention is
The tower diameter of the crude monomer pre-separation tower after the method is used can be reduced to
The tower diameter of the chloromethane recovery tower can be reduced to
The total tower height is relatively substantially constant. Therefore, the design size of the tower can be reduced, and the equipment investment is obviously reduced.
The energy-saving pre-separation method of methyl chlorosilane mixed crude monomers proposed by the invention has been described by the implementation examples, and the related technical personnel can obviously modify the structure and the equipment described herein and properly modify and combine the structure and the equipment to realize the invention without departing from the content, the spirit and the scope of the invention. It is expressly intended that all such similar substitutes and modifications apparent to those skilled in the art are deemed to be within the spirit, scope and content of the invention.
Claims (5)
1. An energy-saving methyl chlorosilane mixed crude monomer pre-separation device is characterized by comprising a crude monomer pre-separation tower and a methyl chloride recovery tower, wherein a crude monomer pre-separation tower condenser is arranged on a gas phase connecting pipeline of the two towers, a crude monomer pre-separation tower reboiler is arranged at the bottom of the crude monomer pre-separation tower, a methyl chloride recovery tower condenser is arranged at the top of the methyl chloride recovery tower, and a methyl chloride recovery tower kettle liquid is pumped to the top of the crude monomer pre-separation tower through a middle reflux pump.
2. An energy-saving methyl chlorosilane mixed crude monomer pre-separation method is characterized in that the device in claim 1 is utilized, after methyl chlorosilane mixed crude monomer enters a crude monomer pre-separation tower, methyl chlorosilane crude monomer is extracted from the bottom of the tower, vapor at the top of the tower is partially condensed, liquid phase of the vapor completely reflows, and gas phase of the vapor is sent to a methyl chloride recovery tower to separate and recover methyl chloride; and (3) discharging non-condensable gas from a condenser of the methyl chloride recovery tower, recovering methyl chloride from the top of the tower or a side line of the tower, and refluxing liquid extracted from the tower kettle to the top of the crude monomer pre-separation tower.
3. The energy-saving pre-separation method of methyl chlorosilane mixed crude monomers as claimed in claim 2, wherein the number of plates of the crude monomer pre-separation tower is 10-90, the feeding position is between the 5 th and the 80 th plates, and the operating pressure is 0.4 MPaG-2.0 MPaG; the number of plates of the methyl chloride recovery tower is 5-90, the feeding position is the bottom of the tower, gas phase feeding is carried out, and the operation pressure is 0.4-2.0 MPaG.
4. The energy-saving methyl chlorosilane mixed crude monomer pre-separating method as claimed in claim 2, wherein the overhead condenser of the crude monomer pre-separating tower is only partially condensed; the cold side medium is selected from circulating water or other suitable public engineering media or process media.
5. The energy-saving methyl chlorosilane mixed crude monomer pre-separation method as claimed in claim 2, which is characterized in that a side branch pipeline is additionally arranged, which directly enters the bottom of the methyl chloride recovery tower from the top of the crude monomer pre-separation tower, so that the steam at the top of the crude monomer pre-separation tower directly enters the side branch pipeline at the bottom of the methyl chloride recovery tower, and the sufficient gas flow in the methyl chloride recovery tower is ensured by adjusting the flow of the side branch pipeline, thereby enhancing the operation stability of the device.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101148394A (en) * | 2006-09-21 | 2008-03-26 | 蓝星化工新材料股份有限公司 | Method for separating methyl chlorosilane and methyl chloride by technique of increasing and reducing pressure |
| CN101870709A (en) * | 2010-06-25 | 2010-10-27 | 天津大学 | Method for refining and reclaiming chloromethane from organic silicon production process |
| CN108689798A (en) * | 2018-06-28 | 2018-10-23 | 湖北兴瑞硅材料有限公司 | A method of improving organic silicon monomer synthesis recycling chloromethanes quality |
| CN112500261A (en) * | 2020-11-30 | 2021-03-16 | 天津大学 | Energy-saving refining device and method for separating organic silicon crude monomer from chloromethane |
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- 2021-07-30 CN CN202110870527.XA patent/CN113831361A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101148394A (en) * | 2006-09-21 | 2008-03-26 | 蓝星化工新材料股份有限公司 | Method for separating methyl chlorosilane and methyl chloride by technique of increasing and reducing pressure |
| CN101870709A (en) * | 2010-06-25 | 2010-10-27 | 天津大学 | Method for refining and reclaiming chloromethane from organic silicon production process |
| CN108689798A (en) * | 2018-06-28 | 2018-10-23 | 湖北兴瑞硅材料有限公司 | A method of improving organic silicon monomer synthesis recycling chloromethanes quality |
| CN112500261A (en) * | 2020-11-30 | 2021-03-16 | 天津大学 | Energy-saving refining device and method for separating organic silicon crude monomer from chloromethane |
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