CN112500261A - Energy-saving refining device and method for separating organic silicon crude monomer from chloromethane - Google Patents
Energy-saving refining device and method for separating organic silicon crude monomer from chloromethane Download PDFInfo
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Abstract
The invention relates to an energy-saving refining device and method for separating an organic silicon crude monomer from chloromethane. Liquid phase raw materials and gas phase raw materials respectively enter a separation tower, crude monomers are extracted from the tower kettle of the separation tower, gas phase materials extracted from the tower top are divided into two parts, one part of the materials enter a stripping tower after being pressurized by a compressor, and the other part of the materials enter a condenser of the separation tower and return to the tower top as reflux liquid of the separation tower; and a reboiler at the tower bottom of the separation tower is heated by steam. The top of the stripping tower is subjected to two-stage condensation by a water cooler and a deep cooler, then the liquid phase is subjected to total reflux, a small amount of non-condensable gas is extracted, and a liquid-phase methyl chloride product is extracted from the tower kettle. According to the heat pump rectification technology, a compressor is arranged at the top of the separation tower, so that the pressure of a gas-phase material at the top of the separation tower is increased and the gas-phase material is used as a gas-phase feed of a stripping tower and a heat source of a reboiler of a methyl chloride refining tower; compared with the common industrial device, the device can effectively reduce the steam consumption, simultaneously improve the quality of the methyl chloride product, has basically consistent requirements on equipment and automatic control, and has operability and industrial feasibility.
Description
Technical Field
The invention relates to the technical field of organic silicon material separation, in particular to an energy-saving refining device and method for separating organic silicon crude monomers from chloromethane.
Background
The organosilicon material has excellent performances of high and low temperature resistance, electrical insulation, corrosion resistance, oxidation resistance stability, safety, reliability, physiological inertia, no toxicity, no odor and the like, and is widely applied to the industries of aerospace, electronics and electricity, medical industry, chemical industry, building, daily necessities and the like. The organosilicon monomer methyl chlorosilane is a raw material for preparing organosilicon materials, and is a foundation and a support of the whole organosilicon industry. In recent years, with the rapid growth of the domestic organic silicon market, the investment heat of organic silicon monomer synthesis is brought forward, and the competition among monomer production enterprises is intensified. Therefore, in the monomer synthesis process, the key point of improving the product quality and saving the energy consumption is to improve the enterprise competitiveness.
In the traditional process, the methyl monomer synthesis takes silicon powder and chloromethane as raw materials, and the methyl chlorosilane mixed monomer, also called as crude monomer, is synthesized in a fluidized bed under certain temperature, pressure and catalyst conditions. The reaction of monomer synthesis is exothermic reaction, the reaction mechanism is complex, and side reactions are many. The fluidized bed produced gas mainly includes dimethyldichlorosilane (Me2), monomethyltrichlorosilane (Me1), trimethylchlorosilane (Me3), monomethylhydrosilane (MeH), low boiling substances, high boiling substances, noncondensable gases (nitrogen, hydrogen, methane, ethylene, etc.), unreacted chloromethane (MeCl), and the like. The reaction gas is dedusted, washed to separate a solid phase and a small amount of high boiling gas, and then is separated by a separation device to obtain a crude monomer and recycle the methyl chloride, the crude monomer enters a monomer rectification unit, and the methyl chloride is recycled.
The traditional process usually adopts equipment and a method for separating crude monomer and methyl chloride by three towers at present, and mainly comprises a crude monomer tower, a methyl chloride tower and a methyl chloride refining tower, and a condenser, a reboiler and a reflux tank which are matched with the crude monomer tower, the methyl chloride tower and the methyl chloride refining tower. Condensing the synthetic gas by a condenser at the top of the washing tower, feeding the condensate into a crude monomer tower, pressurizing the non-condensable gas by a compressor, feeding the non-condensable gas into a methyl chloride tower, obtaining a crude monomer at the tower bottom of the crude monomer tower, and feeding the material at the tower top into the methyl chloride tower; condensing the gas at the top of the methyl chloride tower to obtain methyl chloride, and returning heavy components at the bottom of the methyl chloride tower to the crude monomer tower; and (3) removing light component from purchased or synthesized chloromethane in a chloromethane refining tower to obtain a chloromethane product in the tower kettle. There is also a two-tower scheme, which mainly includes a separation tower and a chloromethane refining tower, and a condenser, a reboiler and a reflux tank which are matched with the separation tower and the chloromethane refining tower. Namely, gas-phase materials and liquid-phase materials respectively enter a separation tower, chloromethane is obtained at the top of the tower, and crude monomers are obtained at the bottom of the tower; the same treatment method is adopted for outsourcing or synthesizing methyl chloride. The equipment and the process method are conventional rectification equipment and processes, so that the energy consumption is relatively high, and the scheme of adding the preheater, adopting the heat pump technology and the intermediate reboiler can obviously reduce the energy consumption of the whole process and has obvious economic benefit. In addition, the traditional equipment and the process scheme can not effectively remove low-boiling carbon-containing substances in the methyl chloride, such as methane, ethylene and the like, low-boiling substances return to a synthesis unit along with the methyl chloride for cyclic utilization, and accumulated low-boiling substances easily cause coking of a catalyst in the fluidized bed, thereby influencing the normal operation of the fluidized bed.
Therefore, finding a method which can remove low-boiling carbon-containing substances in methyl chloride and simultaneously can reduce energy consumption is very significant for improving the competitiveness of organic silicon monomer synthesis enterprises.
Disclosure of Invention
In order to solve the problems of poor product quality and high energy consumption in the prior art, the invention provides an energy-saving device and method for separating an organosilicon crude monomer from chloromethane. The process parameters of the separation unit are adjusted, an intermediate heat exchange technology and a heat pump technology are adopted, the problems of low quality of the methyl chloride and high energy consumption in the production process in the traditional process are solved, and a heat source can be provided for the methyl chloride refining tower.
The technical scheme of the invention is as follows:
an energy-saving refining device for separating crude organosilicon monomers from chloromethane, which comprises: a separation tower T01, a stripping tower T02, a separation tower reboiler E02, a separation tower condenser E05, a stripping tower water cooler E06, a stripping tower deep cooler E07 and a methyl chloride compressor C01; the gas phase, liquid phase crude monomer and methyl chloride mixed material pipelines are respectively connected with an inlet of a separation tower T01, a gas phase pipeline at the top of the separation tower T01 is divided into two parts, one part of the material is connected with an inlet of a methyl chloride compressor C01, an outlet of the methyl chloride compressor C01 is connected with an inlet pipeline of a stripping tower T02, one part of the material is connected with an inlet of a separation tower condenser E05, an outlet of the separation tower condenser E05 is connected with the top of a separation tower T01, a separation tower T01 tower kettle extraction pipeline is connected with an inlet of a separation tower reboiler E02, and an outlet of the separation tower reboiler E02 is connected with a separation tower T01 tower kettle. A gas phase extraction pipeline at the top of the stripping tower T02 is connected with an inlet of a stripping tower water cooler E06, a gas phase pipeline of a stripping tower water cooler E06 is connected with an inlet of a stripping tower deep cooler E07, and liquid phase pipelines of a stripping tower water cooler E06 and a stripping tower deep cooler E07 are connected with the top of a stripping tower T02. The water cooler E06 of the stripping tower is connected with a circulating water pipeline, the condenser E05 of the separation tower and the deep cooler E07 of the stripping tower are connected with an ethylene glycol solution pipeline, and the reboiler E02 of the separation tower is connected with a steam pipeline.
The operation method comprises the following steps: liquid phase raw materials and gas phase raw materials respectively enter a separation tower T01, a separation tower T01 tower bottom is used for extracting crude monomers, gas phase materials extracted from the tower top are divided into two parts, one part of the materials enter a stripping tower T02 after being pressurized by a compressor C01, and the other part of the materials enter a separation tower condenser E05 and return to the tower top as separation tower reflux; the knockout tower kettle reboiler E02 was heated with steam. The top of the stripping tower is condensed by a water cooler E06 and a deep cooler E07 in two stages, then the liquid phase is totally refluxed, a small amount of non-condensable gas is extracted, and a liquid-phase methyl chloride product is extracted from the tower bottom.
On the basis of the above-mentioned apparatus, the apparatus includes: a separation tower T01, a stripping tower T02, a chloromethane refining tower T03, a separation tower reboiler E02, a coupling reboiler E04, a separation tower condenser E05, a stripping tower water cooler E06, a stripping tower deep cooler E07, a chloromethane refining tower condenser E08 and a chloromethane compressor C01; the gas phase extraction of a separation tower T01 is set to be connected with an inlet of a chloromethane compressor C01, a pressurized gas phase material pipeline is divided into two parts, one part is connected with an inlet pipeline of a stripping tower T02, the other part is connected with an inlet of a coupling reboiler E04, an outlet of the coupling reboiler E04 is connected with an inlet of a separation tower condenser E05, a gas phase outlet pipeline of the separation tower condenser E05 is connected with the stripping tower T02, and a liquid phase outlet pipeline is connected with the top of the separation tower T01; the outsourcing/synthetic methyl chloride material pipeline is connected with an inlet of a methyl chloride refining tower T03, a gas-phase extraction pipeline at the top of the methyl chloride refining tower T03 is connected with an inlet of a methyl chloride refining tower condenser E08, an outlet pipeline of the methyl chloride refining tower condenser E08 is connected with the top of a methyl chloride refining tower T03, the tower kettle of the methyl chloride refining tower T03 is connected with an inlet of a coupling reboiler E04, and an outlet of the coupling reboiler E04 is connected with the tower kettle of the methyl chloride refining tower T03. The coupling reboiler E04 is arranged to exchange heat between the feed and the feed.
The operation method comprises the following steps: liquid phase raw materials and gas phase raw materials respectively enter a separation tower T01, a separation tower T01 tower bottom extracts crude monomers, gas phase materials extracted from the tower top are firstly pressurized by a compressor C01, part of high-pressure gas phase materials are extracted to enter a stripping tower T02, part of high-pressure gas phase materials are decoupled from a reboiler E04, the condensed materials enter a separation tower deep cooler E05 and return to the tower top as a separation tower reflux liquid, and a small amount of non-condensable gas also enters a stripping tower T02; a reboiler E02 at the bottom of the separation tower is heated by steam; the top of the stripping tower is condensed by a water cooler E06 and a deep cooler E07 in two stages, then the liquid phase is totally refluxed, a small amount of non-condensable gas is extracted, and a liquid-phase methyl chloride product is extracted from the tower bottom. Outsourcing or synthesizing methyl chloride enters the middle part of a methyl chloride refining tower T03, a small amount of low-boiling-point substances are extracted from the top of the tower, and a methyl chloride product is extracted from the bottom of the tower.
On the basis of the device, the device comprises a separation tower T01, a stripping tower T02, a methyl chloride refining tower T03, a preheater E01, a separation tower reboiler E02, a coupling reboiler E04, a separation tower condenser E05, a stripping tower water cooler E06, a stripping tower deep cooler E07, a methyl chloride refining tower condenser E08 and a methyl chloride compressor C01; the liquid phase material pipeline is firstly connected with an inlet of a preheater E01, an outlet of the preheater E01 is connected with a liquid phase inlet of a separation tower T01, a pipeline extracted from the tower bottom of the separation tower T01 is divided into two parts and is respectively connected with inlets of the preheater E01 and a separation tower reboiler E02, and an outlet of the separation tower reboiler E02 is connected with the tower bottom of the separation tower T01.
The operation method comprises the following steps: preheating a liquid phase raw material by a preheater E01, feeding the liquid phase raw material into the middle lower part of a separation tower T01, and feeding a gas phase raw material into the middle upper part of a separation tower T01; crude monomers are extracted from the bottom of the separation tower T01 and enter a preheater E01 as a heat source to provide heat for liquid phase raw materials, gas phase materials extracted from the top of the tower are pressurized by a compressor C01 at first, part of high-pressure gas phase materials are extracted and enter a stripping tower T02, part of the high-pressure gas phase materials are decoupled from the reboiler E04, the condensed materials enter a separation tower condenser E05 again and return to the top of the tower as separation tower reflux liquid, and a small amount of non-condensable gas also enters a stripping tower T02; the knockout tower kettle reboiler E02 was heated with steam. The top of the stripping tower is condensed by a water cooler E06 and a deep cooler E07 in two stages, then the liquid phase is totally refluxed, a small amount of non-condensable gas is extracted, and a liquid-phase methyl chloride product is extracted from the tower bottom. Outsourcing or synthesizing methyl chloride enters the middle part of a methyl chloride refining tower T03, a small amount of low-boiling-point substances are extracted from the top of the tower, and a methyl chloride product is extracted from the bottom of the tower.
On the basis of the above-mentioned apparatus, the apparatus includes: a separation tower T01, a stripping tower T02, a methyl chloride refining tower T03, a preheater E01, a separation tower reboiler E02, a separation tower middle reboiler E03, a coupling reboiler E04, a separation tower condenser E05, a stripping tower water cooler E06, a stripping tower deep cooler E07, a methyl chloride refining tower condenser E08 and a methyl chloride compressor C01; the side-draw pipeline of the stripping section of the separating tower T01 is connected with the inlet of an intermediate reboiler E03, and the outlet of the intermediate reboiler E03 is connected with the separating tower T01. The intermediate reboiler E03 is connected to a vapor condensate line.
The operation method comprises the following steps: preheating a liquid phase raw material by a preheater E01, then feeding the liquid phase raw material into the middle lower part of a separation tower T01, feeding a gas phase raw material into the middle upper part of the separation tower T01, extracting a crude monomer at the tower bottom of a separation tower T01, feeding the crude monomer as a heat source into a preheater E01 to provide heat for the liquid phase raw material, pressurizing a gas phase material extracted from the tower top by a compressor C01, extracting a part of a high-pressure gas phase material into a stripping tower T02, decoupling a part of the high-pressure gas phase material from a reboiler E04, feeding the condensed material into a deep cooler E05 of the separation tower, feeding the condensed material as a reflux liquid of the separation; the knockout tower kettle reboiler E02 is heated by steam, and an intermediate reboiler E03 is provided in the stripping section, heated by steam condensate generated by E02 and supplemented by other units. The top of the stripping tower is condensed by a water cooler E06 and a deep cooler E07 in two stages, then the liquid phase is totally refluxed, a small amount of non-condensable gas is extracted, and a liquid-phase methyl chloride product is extracted from the tower bottom. Outsourcing or synthesizing methyl chloride enters the middle part of a methyl chloride refining tower T03, a small amount of low-boiling-point substances are extracted from the top of the tower, and a methyl chloride product is extracted from the bottom of the tower.
The temperature of the top of the separating tower T01 is controlled to be-4-15 ℃, the pressure of the top of the separating tower T01 is controlled to be 150-350 kPaG, and the reflux-feed ratio is controlled to be 0.25-0.52; the temperature of the top of the stripping tower T02 is controlled to be 37-50 ℃, the pressure of the top of the stripping tower is controlled to be 800-1150 kPaG, and the reflux-feed ratio is controlled to be 0.95-1.1; the tower kettle degree of the chloromethane refining tower T03 is controlled to be 42-46 ℃, the tower top pressure is controlled to be 800-900 kPaG, and the reflux ratio feeding is controlled to be 0.37-0.5; the outlet pressure of a chloromethane compressor C01 is controlled to be 850-1200 kPaG, and the outlet temperature is controlled to be 80-120 ℃; the dew point temperature of the outlet of the methyl chloride compressor is 12-20 ℃ higher than the tower kettle temperature of a methyl chloride refining tower T03; and controlling the liquid phase extraction temperature of the material side of the intermediate reboiler E03 to be 85-97 ℃.
The separation tower deep cooler E05 uses glycol solution as a refrigerant according to the difference of the operation pressure of the separation tower, the inlet temperature of the refrigerant is-15 ℃, and the outlet temperature of the refrigerant is-10 ℃; or using water with the temperature of 7 ℃ as a refrigerant, wherein the inlet temperature of the refrigerant is 7, and the outlet temperature of the refrigerant is 12 ℃; the knockout tower reboiler E02 was saturated with 200kPaG of steam or with 500kPaG of steam depending on the operation pressure of the knockout tower.
The invention has the beneficial effects that:
1. on the basis of a conventional separation process, according to a heat pump rectification technology, a compressor is arranged at the top of a separation tower, so that the pressure of a gas-phase material at the top of the separation tower is increased, and the gas-phase material is used as a gas-phase feed of a stripping tower and a heat source of a reboiler of a chloromethane refining tower;
2. by reducing the operating pressure of the separation tower, the relative volatility of light and heavy components of the separation tower is increased, the reflux feed ratio of the separation tower can be reduced, the steam consumption is reduced, and low-pressure steam can be used as a heat source;
3. after crude monomers at the tower bottom of the separation tower are extracted, the crude monomers are used as a heat source of a preheater, so that the temperature of liquid-phase feeding is increased, and the steam consumption is reduced;
4. an intermediate reboiler is arranged at the middle lower part of the separation tower, and steam condensate at the tower bottom of the separation tower and supplementary steam condensate are used as heat sources to reduce steam consumption;
5. the stripping tower is arranged, the non-condensable gas is removed from the top of the tower, the methyl chloride product is extracted from the tower kettle, and the stripping tower does not need an additional heat source and can effectively reduce the content of low-boiling-point substances in the methyl chloride.
6. Compared with the common industrialized device, the method can effectively reduce the steam consumption, simultaneously improve the quality of the methyl chloride product, has basically consistent requirements on equipment and automatic control, and has stronger operability and industrialized feasibility.
Drawings
FIG. 1 is a schematic flow diagram of an energy-saving, refining apparatus for the separation of crude monomer from methyl chloride based on a pressure reduction scheme;
FIG. 2 is a schematic flow diagram of an energy-saving refining apparatus for separating crude monomers from methyl chloride, which is based on the apparatus of FIG. 1 and is added with a heat pump rectification scheme;
FIG. 3 is a schematic flow diagram of an energy-saving refining apparatus for separating crude monomers from methyl chloride, which is based on the apparatus of FIG. 2 and has an added heat exchange scheme for materials;
FIG. 4 is a schematic flow diagram of an energy-saving, refining apparatus for the separation of crude monomer from methyl chloride with the addition of an intermediate reboiling scheme to the apparatus of FIG. 3;
wherein: t01-separation tower, T02-stripping tower, T03-chloromethane refining tower, E01-preheater, E02-separation tower reboiler, E03-separation tower middle reboiler, E04-coupling reboiler, E05-separation tower condenser, E06-stripping tower water cooler, E07-stripping tower deep cooler, E08-chloromethane refining tower condenser, and C01-chloromethane compressor.
Detailed Description
The invention is described in further detail below with reference to the following figures and specific examples:
example 1
As shown in fig. 1, an energy-saving and refining device and method for separating crude organosilicon monomers from chloromethane, the device comprises: a separation tower T01, a stripping tower T02, a methyl chloride refining tower T03, a separation tower reboiler E02, a coupling reboiler E04, a separation tower condenser E05, a stripping tower water cooler E06, a stripping tower deep cooler E07, a methyl chloride refining tower condenser E08 and a methyl chloride compressor C01.
The invention adjusts the technological parameters of the separation unit, and the separation tower T01 is operated under reduced pressure, and the technological process comprises the following steps: calculated according to the yield of 18 ten thousand tons of crude monomers per year, the liquid phase raw material from the top of the washing tower at the upstream section is 22245t/h, and the composition is as follows: 15 wt% of MeCl, 2 wt% of Me3, 75 wt% of Me2, 5 wt% of Me1, 2 wt% of high-boiling substances and 1 wt% of the rest low-boiling and non-condensable gases, and 27140t/h of gas-phase raw material, the composition of which is: 75 wt% of CH3Cl, 1 wt% of Me3, 20 wt% of Me2, 1 wt% of Me1, 0.5 wt% of high-boiling components and 2.5 wt% of the balance of low-boiling and non-condensable gases. The liquid phase raw material enters the middle-lower part of a separation tower T01, and the gas phase raw material enters the middle-upper part of a separation tower T01; crude monomer is extracted from the bottom of the separation tower T01, gas phase material extracted from the top of the separation tower is divided into two parts, one part of the material is pressurized by a compressor C01 and then enters a stripping tower T02, the other part of the material enters a separation tower condenser E05, the condensed material is returned to the top of the separation tower as reflux of the separation tower, and a reboiler E02 at the bottom of the separation tower adopts steam for heating. The top of the stripping tower is condensed by a water cooler E06 and a deep cooler E07 in two stages, then the liquid phase is totally refluxed, a small amount of non-condensable gas is extracted, and a liquid-phase methyl chloride product is extracted from the tower bottom. Outsourcing or synthesizing methyl chloride enters the middle part of a methyl chloride refining tower T03, a small amount of low-boiling-point substances are extracted from the top of the tower, and a methyl chloride product is extracted from the bottom of the tower.
The operation pressure at the top of the separation tower T01 is 150kPaG, the reflux-feed ratio is 0.25, the temperature at the top of the tower is-4 ℃, and the temperature at the bottom of the tower is 106 ℃; the operation pressure at the top of the stripping tower T02 is 1150kPaG, the temperature at the top of the stripping tower is 50 ℃, and the reflux feed ratio is 0.95; the operation pressure at the top of the chloromethane refining tower T03 is 900kPaG, the temperature of the tower bottom is 46 ℃, and the reflux feed ratio is 0.5; the outlet pressure of the compressor is 1200kPaG, and the outlet temperature is controlled at 120 ℃. The separation tower condenser E05 adopts ethylene glycol solution as a refrigerant, the inlet temperature is-15 ℃, and the outlet temperature is-10 ℃. The knockout tower reboiler E02 used 200kPaG saturated steam as the heat source.
Compared with the conventional process device, the invention adopts deep cooling at the top condenser of the separation tower, and additionally increases the power consumption; on the other hand, by lowering the operating pressure of separator T01, the separator steam and recycle water consumption is reduced. According to the steam unit price: 200 yuan/ton, electricity charge: 0.6 yuan/degree, circulating water: 0.1 yuan/m 3, and the operation cost can be saved by 38 ten thousand yuan per year according to the crude monomer yield of 18 ten thousand tons per year and the annual operation time of 7200 h. After the stripping tower is arranged, the purity of the chloromethane can be improved to more than 99.8 percent from the original 99.05 percent.
Example 2
As shown in fig. 2, an energy-saving and refining device and method for separating crude organosilicon monomers from chloromethane, the device comprises: a separation tower T01, a stripping tower T02, a methyl chloride refining tower T03, a separation tower reboiler E02, a coupling reboiler E04, a separation tower condenser E05, a stripping tower water cooler E06, a stripping tower deep cooler E07, a methyl chloride refining tower condenser E08 and a methyl chloride compressor C01.
The invention adjusts the technological parameters of the separation unit, the separation tower T01 is operated under reduced pressure, and the heat pump technology is adopted, and the processing capacity and the feeding composition are the same as those of the embodiment 1. The process flow comprises the following steps: the liquid phase raw material enters the middle-lower part of a separation tower T01, and the gas phase raw material enters the middle-upper part of a separation tower T01; crude monomers are extracted from the bottom of a separation tower T01, gas-phase materials extracted from the top of the tower are pressurized by a compressor C01, part of high-pressure gas-phase materials are extracted and enter a stripping tower T02, part of the high-pressure gas-phase materials are decoupled from a reboiler E04, the condensed materials enter a separation tower condenser E05 and return to the top of the tower as a separation tower reflux liquid, and a small amount of non-condensable gas also enters a stripping tower T02; the kettle reboiler E02 was heated with steam. The top of the stripping tower is condensed by a water cooler E06 and a deep cooler E07 in two stages, then the liquid phase is totally refluxed, a small amount of non-condensable gas is extracted, and a liquid-phase methyl chloride product is extracted from the tower bottom. Outsourcing or synthesizing methyl chloride enters the middle part of a methyl chloride refining tower T03, a small amount of low-boiling-point substances are extracted from the top of the tower, and a methyl chloride product is extracted from the bottom of the tower.
The operation pressure at the top of the separation tower T01 is 200kPaG, the reflux-feed ratio is 0.3, the temperature at the top of the tower is 1.3 ℃, and the temperature at the bottom of the tower is 113 ℃; the operation pressure at the top of the stripping tower T02 is 1100kPaG, the temperature at the top of the stripping tower is 48 ℃, and the reflux feed ratio is 1.07; the operation pressure at the top of the chloromethane refining tower T03 is 850kPaG, the temperature of the tower bottom is 44 ℃, and the reflux feed ratio is 0.46; the outlet pressure of the compressor is 900kPaG, and the outlet temperature is controlled at 86 ℃. The deep cooler E05 of the separation tower adopts ethylene glycol solution as a refrigerant, the inlet temperature is-15 ℃, and the outlet temperature is-10 ℃. The knockout tower reboiler E02 used 200kPaG saturated steam as the heat source.
Compared with the conventional process device, the process has the advantages that the processing capacity of the compressor is increased, namely the power consumption is increased, and the power consumption is additionally increased because the condenser at the top of the separation tower adopts deep cooling; on the other hand, the steam and circulating water consumption of the separation tower is reduced, and the methyl chloride refining tower does not need steam any more. According to the steam unit price: 200 yuan/ton, electricity charge: 0.6 yuan/degree, circulating water: 0.1 yuan/m 3, calculated according to 18 ten thousand tons/year crude monomer yield and the annual operation time of 7200h, the operation cost can be saved by 337 ten thousand yuan per year, and the method has obvious economic benefit. After the stripping tower is arranged, the purity of the chloromethane can be improved to more than 99.8 percent from the original 99.05 percent.
Example 3
As shown in fig. 3, an energy-saving and refining device and method for separating crude organosilicon monomer from chloromethane, the device comprises: a separation tower T01, a stripping tower T02, a methyl chloride refining tower T03, a preheater E01, a separation tower reboiler E02, a coupling reboiler E04, a separation tower condenser E05, a stripping tower water cooler E06, a stripping tower deep cooler E07, a methyl chloride refining tower condenser E08 and a methyl chloride compressor C01.
The invention adjusts the technological parameters of the separation unit, the pressure reduction operation of the separation tower T01, and the heat pump technology and the heat exchange scheme between materials are adopted, and the processing capacity and the feeding composition are the same as those of the embodiment 1. Preheating a liquid phase raw material by a preheater E01, feeding the liquid phase raw material into the middle lower part of a separation tower T01, and feeding a gas phase raw material into the middle upper part of a separation tower T01; crude monomers are extracted from the bottom of the separation tower T01 and enter a preheater E01 as a heat source to provide heat for liquid phase raw materials, gas phase materials extracted from the top of the tower are pressurized by a compressor C01 at first, part of high-pressure gas phase materials are extracted and enter a stripping tower T02, part of the high-pressure gas phase materials are decoupled from a reboiler E04, the condensed materials enter a separation tower condenser E05 again and return to the top of the tower as reflux liquid of the separation tower, a small amount of non-condensable gas also enters a stripping tower T02, and the reboiler E02 at the bottom of the tower is heated by steam. The top of the stripping tower is condensed by a water cooler E06 and a deep cooler E07 in two stages, then the liquid phase is totally refluxed, a small amount of non-condensable gas is extracted to remove a membrane separation system, and a liquid-phase methyl chloride product is extracted from the bottom of the stripping tower. Outsourcing or synthesizing methyl chloride enters the middle part of a methyl chloride refining tower T03, a small amount of low-boiling-point substances are extracted from the top of the tower, and a methyl chloride product is extracted from the bottom of the tower.
The operation pressure at the top of the separation tower T01 is 300kPaG, the reflux feed ratio is 0.41, the temperature at the top of the tower is 10.5 ℃, the temperature at the bottom of the tower is 124 ℃, the operation pressure at the top of the stripping tower T02 is 800kPaG, the temperature at the top of the tower is 37 ℃, and the reflux feed ratio is 1.1; the operation pressure at the top of the chloromethane refining tower T03 is 800kPaG, the temperature of the tower kettle is 42 ℃, and the reflux feed ratio is 0.37; the outlet pressure of the compressor is 1100kPaG, and the outlet temperature is controlled at 112 ℃. The deep cooler E05 of the separation tower adopts ethylene glycol solution as a refrigerant, the inlet temperature is-15 ℃, and the outlet temperature is-10 ℃. The knockout tower reboiler E02 used 500kPaG saturated steam as the heat source.
Compared with the conventional process device, the process has the advantages that the processing capacity of the compressor is increased, namely the power consumption is increased, and the power consumption is additionally increased because the condenser at the top of the separation tower adopts deep cooling; on the other hand, the steam and circulating water consumption of the separation tower is reduced, and the methyl chloride refining tower does not need steam any more. According to the steam unit price: 200 yuan/ton, electricity charge: 0.6 yuan/degree, circulating water: 0.1 yuan/m 3, calculated according to the crude monomer yield of 18 ten thousand tons/year and the annual operation time of 7200h, the operation cost can be saved by 298 ten thousand yuan per year, and the method has obvious economic benefit. After the stripping tower is arranged, the purity of the chloromethane can be improved to more than 99.8 percent from the original 99.05 percent.
Example 4
As shown in fig. 4, an energy-saving and refining device and method for separating crude organosilicon monomer from chloromethane, the device comprises: a separation tower T01, a stripping tower T02, a methyl chloride refining tower T03, a preheater E01, a separation tower reboiler E02, a separation tower middle reboiler E03, a coupling reboiler E04, a separation tower condenser E05, a stripping tower water cooler E06, a stripping tower deep cooler E07, a methyl chloride refining tower condenser E08 and a methyl chloride compressor C01.
The technological parameters of the separation unit of the invention, the decompression operation of the separation tower T01, the heat pump technology, the intermediate reboiling and the heat exchange scheme between materials are adopted, and the processing capacity and the feeding composition are the same as those of the embodiment 1. The process flow comprises the following steps: preheating a liquid phase raw material by a preheater E01, feeding the liquid phase raw material into the middle lower part of a separation tower T01, and feeding a gas phase raw material into the middle upper part of a separation tower T01; crude monomers are extracted from the bottom of a separation tower T01 and enter a preheater E01 as a heat source to provide heat for liquid phase raw materials, gas phase materials extracted from the top of the tower are pressurized by a compressor C01 at first, part of high-pressure gas phase materials are extracted and enter a stripping tower T02, part of the high-pressure gas phase materials are decoupled from the reboiler E04, the condensed materials enter a deep cooler E05 of the separation tower and return to the top of the tower as reflux liquid of the separation tower, and a small amount of non-condensable gas also enters a stripping tower T02; the reboiler E02 of the separation tower T01 tower bottom adopts steam for heating, the stripping section is provided with an intermediate reboiler E03, and steam condensate generated by the reboiler E02 and other reboilers is used for heating. The top of the stripping tower is condensed by a water cooler E06 and a deep cooler E07 in two stages, then the liquid phase is totally refluxed, a small amount of non-condensable gas is extracted, and a liquid-phase methyl chloride product is extracted from the tower bottom. Outsourcing or synthesizing methyl chloride enters the middle part of a methyl chloride refining tower T03, a small amount of low-boiling-point substances are extracted from the top of the tower, and a methyl chloride product is extracted from the bottom of the tower.
The operation pressure at the top of the separation tower T01 is 150kPaG, the reflux-feed ratio is 0.25, the temperature at the top of the tower is-4 ℃, and the temperature at the bottom of the tower is 106 ℃; the operation pressure at the top of the stripping tower T02 is 1150kPaG, the temperature at the top of the stripping tower is 50 ℃, and the reflux feed ratio is 0.95; the operation pressure at the top of the chloromethane refining tower T03 is 900kPaG, the temperature of the tower bottom is 46 ℃, and the reflux feed ratio is 0.5; the outlet pressure of the compressor is 1200kPaG, and the outlet temperature is controlled at 120 ℃; and the liquid phase extraction temperature of the intermediate reboiler is 85 ℃. The deep cooler E05 of the separation tower adopts ethylene glycol solution as a refrigerant, the inlet temperature is-15 ℃, and the outlet temperature is-10 ℃. The knockout tower reboiler E02 used 200kPaG saturated steam as the heat source.
Compared with the conventional process device, the process has the advantages that the processing capacity of the compressor is increased, namely the power consumption is increased, and the power consumption is additionally increased because the condenser at the top of the separation tower adopts deep cooling; on the other hand, the steam and circulating water consumption of the separation tower is reduced, and the methyl chloride refining tower does not need steam any more. According to the steam unit price: 200 yuan/ton, electricity charge: 0.6 yuan/degree, circulating water: 0.1 yuan/m 3, calculated according to 18 ten thousand tons/year crude monomer yield and the annual operation time of 7200h, the operation cost can be saved by 469 ten thousand yuan per year, and the economic benefit is remarkable. After the stripping tower is arranged, the purity of the chloromethane can be improved to more than 99.8 percent from the original 99.05 percent.
Example 5
As shown in FIG. 4, the treatment capacity and the feed composition of an energy-saving and refining device and method for separating crude organosilicon monomers from chloromethane are the same as those of example 1, and the process flow is the same as that of example 4.
The operation pressure at the top of the separation tower T01 is 250kPaG, the reflux-feed ratio is 0.37, the temperature at the top of the tower is 6 ℃, and the temperature at the bottom of the tower is 119 ℃; the operation pressure at the top of the stripping tower T02 is 1000kPaG, the temperature at the top of the stripping tower is 45 ℃, and the reflux feed ratio is 1.01; the operation pressure at the top of the chloromethane refining tower T03 is 850kPaG, the temperature of the tower bottom is 44 ℃, and the reflux feed ratio is 0.46; the outlet pressure of the compressor is 1100kPaG, and the outlet temperature is controlled at 112 ℃; in the intermediate reboiler, the liquid phase extraction temperature is 90 ℃. The deep cooler E05 of the separation tower adopts ethylene glycol solution as a refrigerant, the inlet temperature is-15 ℃, and the outlet temperature is-10 ℃. The knockout tower reboiler E02 used 200kPaG saturated steam as the heat source.
According to the calculation, compared with the conventional process device, 391 ten thousand yuan of operation cost can be saved every year according to the consistency of the embodiment 1. The purity of the chloromethane can reach more than 99.8 percent.
Example 6
As shown in FIG. 4, the treatment capacity and the feed composition of an energy-saving and refining device and method for separating crude organosilicon monomers from chloromethane are the same as those of example 1, and the process flow is the same as that of example 4.
The operation pressure at the top of the separation tower T01 is 350kPaG, the reflux-feed ratio is 0.52, the temperature at the top of the tower is 15 ℃, and the temperature at the bottom of the tower is 129 ℃; the operation pressure at the top of the stripping tower T02 is 800kPaG, the temperature at the top of the stripping tower is 37 ℃, and the reflux feed ratio is 1.1; the operation pressure at the top of the chloromethane refining tower T03 is 800kPaG, the temperature of the tower kettle is 42 ℃, and the reflux feed ratio is 0.37; the outlet pressure of the compressor is 850kPaG, and the outlet temperature is controlled at 80 ℃; in the intermediate reboiler, the liquid phase extraction temperature is 97 ℃. The deep cooler E05 of the separation tower adopts water with the temperature of 7 ℃ as a refrigerant, the inlet temperature is 7, and the outlet temperature is 12 ℃. The knockout tower reboiler E02 used 500kPaG saturated steam as the heat source.
The calculation is consistent with the embodiment 1, and the operation cost can be saved by 113 ten thousand yuan per year compared with the conventional process device. The purity of the chloromethane can reach more than 99.8 percent.
Claims (10)
1. An energy-saving and refining device for separating organic silicon crude monomers from chloromethane is characterized by comprising: a separation tower T01, a stripping tower T02, a separation tower reboiler E02, a separation tower condenser E05, a stripping tower water cooler E06, a stripping tower deep cooler E07 and a methyl chloride compressor C01; a gas phase, liquid phase crude monomer and methyl chloride mixed material pipeline is respectively connected with an inlet of a separation tower T01, a gas phase pipeline at the top of the separation tower T01 is divided into two parts, one part of the material is connected with an inlet of a methyl chloride compressor C01, an outlet of the methyl chloride compressor C01 is connected with an inlet pipeline of a stripping tower T02, one part of the material is connected with an inlet of a separation tower condenser E05, an outlet of the separation tower condenser E05 is connected with the top of a separation tower T01, a separation tower T01 tower kettle extraction pipeline is connected with an inlet of a separation tower reboiler E02, and an outlet of the separation tower reboiler E02 is connected with a separation tower T01 tower kettle; a gas phase extraction pipeline at the top of the stripping tower T02 is connected with an inlet of a stripping tower water cooler E06, a gas phase pipeline of a stripping tower water cooler E06 is connected with an inlet of a stripping tower deep cooler E07, and liquid phase pipelines of a stripping tower water cooler E06 and a stripping tower deep cooler E07 are connected with the top of a stripping tower T02; the water cooler E06 of the stripping tower is connected with a circulating water pipeline, the condenser E05 of the separation tower and the deep cooler E07 of the stripping tower are connected with an ethylene glycol solution pipeline, and the reboiler E02 of the separation tower is connected with a steam pipeline.
2. The apparatus of claim 1, wherein the apparatus comprises: a separation tower T01, a stripping tower T02, a chloromethane refining tower T03, a separation tower reboiler E02, a coupling reboiler E04, a separation tower condenser E05, a stripping tower water cooler E06, a stripping tower deep cooler E07, a chloromethane refining tower condenser E08 and a chloromethane compressor C01; the gas phase extraction of a separation tower T01 is set to be connected with an inlet of a chloromethane compressor C01, a pressurized gas phase material pipeline is divided into two parts, one part is connected with an inlet pipeline of a stripping tower T02, the other part is connected with an inlet of a coupling reboiler E04, an outlet of the coupling reboiler E04 is connected with an inlet of a separation tower condenser E05, a gas phase outlet pipeline of the separation tower condenser E05 is connected with the stripping tower T02, and a liquid phase outlet pipeline is connected with the top of the separation tower T01; the outsourcing/synthetic methyl chloride material pipeline is connected with an inlet of a methyl chloride refining tower T03, a gas-phase extraction pipeline at the top of the methyl chloride refining tower T03 is connected with an inlet of a methyl chloride refining tower condenser E08, an outlet pipeline of the methyl chloride refining tower condenser E08 is connected with the top of a methyl chloride refining tower T03, the tower kettle of the methyl chloride refining tower T03 is connected with an inlet of a coupling reboiler E04, and an outlet of the coupling reboiler E04 is connected with the tower kettle of the methyl chloride refining tower T03; the coupling reboiler E04 is arranged to exchange heat between the feed and the feed.
3. The apparatus of claim 2, wherein the apparatus comprises a separation column T01, a stripper column T02, a methyl chloride finishing column T03, a preheater E01, a separation column reboiler E02, a coupling reboiler E04, a separation column condenser E05, a stripper column water cooler E06, a stripper column chiller E07, a methyl chloride finishing column condenser E08, a methyl chloride compressor C01; the liquid phase material pipeline is firstly connected with an inlet of a preheater E01, an outlet of the preheater E01 is connected with a liquid phase inlet of a separation tower T01, a pipeline extracted from the tower bottom of the separation tower T01 is divided into two parts and is respectively connected with inlets of the preheater E01 and a separation tower reboiler E02, and an outlet of the separation tower reboiler E02 is connected with the tower bottom of the separation tower T01.
4. The apparatus of claim 3, wherein the apparatus comprises: a separation tower T01, a stripping tower T02, a methyl chloride refining tower T03, a preheater E01, a separation tower reboiler E02, a separation tower middle reboiler E03, a coupling reboiler E04, a separation tower condenser E05, a stripping tower water cooler E06, a stripping tower deep cooler E07, a methyl chloride refining tower condenser E08 and a methyl chloride compressor C01; a side extraction pipeline of a stripping section of the separation tower T01 is connected with an inlet of an intermediate reboiler E03, and an outlet of the intermediate reboiler E03 is connected with a separation tower T01; the intermediate reboiler E03 is connected to a vapor condensate line.
5. The energy-saving and refining method for separating crude organosilicon monomer from chloromethane by using the device of claim 1 is characterized in that liquid phase raw materials and gas phase raw materials respectively enter a separation tower T01, crude organosilicon monomer is extracted from the bottom of the separation tower T01, gas phase materials extracted from the tower top are divided into two parts, one part of the materials enter a stripping tower T02 after being pressurized by a compressor C01, and the other part of the materials enter a separation tower condenser E05 and return to the tower top as separation tower reflux; a reboiler E02 at the bottom of the separation tower is heated by steam; the top of the stripping tower is condensed by a water cooler E06 and a deep cooler E07 in two stages, then the liquid phase is totally refluxed, a small amount of non-condensable gas is extracted, and a liquid-phase methyl chloride product is extracted from the tower bottom.
6. The energy-saving and refining method for separating crude organosilicon monomer from chloromethane by using the device of claim 2 is characterized in that liquid phase raw materials and gas phase raw materials respectively enter a separation tower T01, crude organosilicon monomer is extracted from the bottom of the separation tower T01, gas phase materials extracted from the tower top are pressurized by a compressor C01, part of high-pressure gas phase materials are extracted and enter a stripping tower T02, part of high-pressure gas phase materials are decoupled with a reboiler E04, the condensed materials enter a separation tower deep cooler E05 and return to the tower top as reflux of the separation tower, and a small amount of non-condensable gas also enters a stripping tower T02; a reboiler E02 at the bottom of the separation tower is heated by steam; the tower top of the stripping tower is condensed by a water cooler E06 and a deep cooler E07 in two stages, then the liquid phase is totally refluxed, a small amount of non-condensable gas is extracted, and a liquid-phase methyl chloride product is extracted from the tower kettle; outsourcing or synthesizing methyl chloride enters the middle part of a methyl chloride refining tower T03, a small amount of low-boiling-point substances are extracted from the top of the tower, and a methyl chloride product is extracted from the bottom of the tower.
7. The energy-saving and refining method for separating crude organosilicon monomers from chloromethane by using the device as claimed in claim 3 is characterized in that liquid phase raw materials enter the middle lower part of a separation tower T01 after being preheated by a preheater E01, and gas phase raw materials enter the middle upper part of a separation tower T01; crude monomers are extracted from the bottom of the separation tower T01 and enter a preheater E01 as a heat source to provide heat for liquid phase raw materials, gas phase materials extracted from the top of the tower are pressurized by a compressor C01 at first, part of high-pressure gas phase materials are extracted and enter a stripping tower T02, part of the high-pressure gas phase materials are decoupled from the reboiler E04, the condensed materials enter a separation tower condenser E05 again and return to the top of the tower as separation tower reflux liquid, and a small amount of non-condensable gas also enters a stripping tower T02; a reboiler E02 at the bottom of the separation tower is heated by steam; the tower top of the stripping tower is condensed by a water cooler E06 and a deep cooler E07 in two stages, then the liquid phase is totally refluxed, a small amount of non-condensable gas is extracted, and a liquid-phase methyl chloride product is extracted from the tower kettle; outsourcing or synthesizing methyl chloride enters the middle part of a methyl chloride refining tower T03, a small amount of low-boiling-point substances are extracted from the top of the tower, and a methyl chloride product is extracted from the bottom of the tower.
8. The energy-saving and refining method for separating the crude organosilicon monomer from the chloromethane by using the device as claimed in claim 4 is characterized in that a liquid phase raw material is preheated by a preheater E01 and then enters the middle lower part of a separation tower T01, a gas phase raw material enters the middle upper part of the separation tower T01, crude monomer is extracted from the bottom of a separation tower T01 and enters a preheater E01 as a heat source to provide heat for the liquid phase raw material, the gas phase material extracted from the top of the tower is pressurized by a compressor C01, one part of the high-pressure gas phase material is extracted and enters a stripping tower T02, one part of the high-pressure gas phase material is decoupled by a reboiler E04, the condensed material enters a deep cooler E05 of the separation tower and returns to the top of the tower as a reflux liquid of the; a reboiler E02 at the bottom of the separation tower is heated by steam, an intermediate reboiler E03 is arranged at the stripping section, and steam condensate generated by E02 and supplemented by other units is heated; the tower top of the stripping tower is condensed by a water cooler E06 and a deep cooler E07 in two stages, then the liquid phase is totally refluxed, a small amount of non-condensable gas is extracted, and a liquid-phase methyl chloride product is extracted from the tower kettle; outsourcing or synthesizing methyl chloride enters the middle part of a methyl chloride refining tower T03, a small amount of low-boiling-point substances are extracted from the top of the tower, and a methyl chloride product is extracted from the bottom of the tower.
9. The method as claimed in any one of claims 5 to 8, wherein the temperature of the top of the separation column T01 is controlled to be-4 to 15 ℃, the pressure of the top of the separation column T01 is controlled to be 150 to 350kPaG, and the reflux-feed ratio is controlled to be 0.25 to 0.52; the temperature of the top of the stripping tower T02 is controlled to be 37-50 ℃, the pressure of the top of the stripping tower is controlled to be 800-1150 kPaG, and the reflux-feed ratio is controlled to be 0.95-1.1; the tower kettle degree of the chloromethane refining tower T03 is controlled to be 42-46 ℃, the tower top pressure is controlled to be 800-900 kPaG, and the reflux ratio feeding is controlled to be 0.37-0.5; the outlet pressure of a chloromethane compressor C01 is controlled to be 850-1200 kPaG, and the outlet temperature is controlled to be 80-120 ℃; the dew point temperature of the outlet of the methyl chloride compressor is 12-20 ℃ higher than the tower kettle temperature of a methyl chloride refining tower T03; and controlling the liquid phase extraction temperature of the material side of the intermediate reboiler E03 to be 85-97 ℃.
10. The method as claimed in any one of claims 5 to 8, wherein the deep cooler E05 of the separation tower uses glycol solution as refrigerant according to the difference of the operation pressure of the separation tower, the inlet temperature of the refrigerant is-15 ℃, and the outlet temperature is-10 ℃; or using water with the temperature of 7 ℃ as a refrigerant, wherein the inlet temperature of the refrigerant is 7, and the outlet temperature of the refrigerant is 12 ℃; the knockout tower reboiler E02 was saturated with 200kPaG of steam or with 500kPaG of steam depending on the operation pressure of the knockout tower.
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