CN112961033A - Five-tower five-effect rectification process method and device for methanol - Google Patents
Five-tower five-effect rectification process method and device for methanol Download PDFInfo
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 title claims abstract description 537
- 238000000034 method Methods 0.000 title claims abstract description 47
- 230000008569 process Effects 0.000 title claims abstract description 32
- 238000011084 recovery Methods 0.000 claims abstract description 100
- 239000001760 fusel oil Substances 0.000 claims abstract description 16
- 230000008878 coupling Effects 0.000 claims description 82
- 238000010168 coupling process Methods 0.000 claims description 82
- 238000005859 coupling reaction Methods 0.000 claims description 82
- 239000007791 liquid phase Substances 0.000 claims description 49
- 238000010992 reflux Methods 0.000 claims description 41
- 238000000605 extraction Methods 0.000 claims description 38
- 239000012071 phase Substances 0.000 claims description 36
- 239000000463 material Substances 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 12
- 239000002351 wastewater Substances 0.000 claims description 8
- 238000004821 distillation Methods 0.000 claims description 5
- 229920006395 saturated elastomer Polymers 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 description 11
- 238000004519 manufacturing process Methods 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 230000008901 benefit Effects 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
- B01D3/146—Multiple effect distillation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
- B01D3/322—Reboiler specifications
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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
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
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Abstract
The invention relates to a five-tower five-effect rectification method and a five-tower five-effect rectification device for methanol. The method adds a second pressurized rectifying tower and a recovery tower on the basis of the methanol three-tower three-effect rectifying process flow. The five-tower five-effect rectification process flow of the methanol is that the gas phase at the top of the first pressure rectification tower is used for extracting the refined methanol, the methanol steam is divided into three strands, the heat is used for meeting the heat load of a reboiler at the bottom of the second pressure rectification tower, the normal pressure tower and the recovery tower, the gas phase at the top of the second pressure rectification tower is used for extracting the refined methanol, and the heat of the methanol steam is used for meeting the heat load of the reboiler at the bottom of the pre-rectification tower. The methanol steam heat at the top of the first pressurized rectifying tower is utilized for three times and four times, and the pre-rectifying tower, the newly added second pressurized rectifying tower and the newly added recovery tower do not need saturated steam as a heat source. The recovery tower is used for recovering methanol in fusel oil extracted from the side line of the normal pressure tower, and the recovery rate of the methanol is improved.
Description
Technical Field
The invention relates to the technical field of methanol rectification, in particular to a five-tower five-effect rectification process method and a five-tower five-effect rectification device for methanol.
Background
Methanol is an important basic organic chemical raw material, and methanol rectification is a high-energy consumption production link. The method improves the quality of the methanol product, reduces the energy consumption of the methanol production process and can improve the competitiveness of enterprises. Therefore, the reduction of the energy consumption of the methanol rectification system attracts the attention of the researchers.
At present, the methanol rectification production process in China generally adopts a three-tower double-effect rectification process, wherein three towers are respectively a pre-rectification tower, a pressurization tower and an atmospheric tower. Steam at the top of the pressurizing tower and a reboiler at the bottom of the normal pressure tower form heat coupling rectification, methanol products are respectively obtained at the tops of the pressurizing tower and the normal pressure tower, fusel oil is extracted from the side line of the normal pressure tower, and qualified wastewater is discharged from the bottom of the normal pressure tower. And in order to improve the recovery rate of the methanol, a recovery tower is additionally arranged behind the normal pressure tower, the methanol in the fusel oil extracted from the side line of the normal pressure tower is recovered, and the four-tower double-effect rectification process of the methanol is formed. However, with the continuous expansion of production scale, the double-effect rectification process of methanol has larger production energy consumption.
In order to reduce the energy consumption of the methanol rectification process, various attempt schemes such as a three-tower and heat pump rectification coupling technology are provided, but the problems of equipment investment and power consumption exist.
Disclosure of Invention
The invention aims to provide a five-tower five-effect rectification method and a five-tower five-effect rectification device for methanol, aiming at the defects in the prior art. The method adds a second pressurized rectifying tower and a recovery tower on the basis of the methanol three-tower three-effect rectifying process flow. The five-tower five-effect rectification process flow of the methanol is that the gas phase at the top of the first pressure rectification tower is used for extracting the refined methanol, the methanol steam is divided into three strands, the heat is used for meeting the heat load of a reboiler at the bottom of the second pressure rectification tower, the normal pressure tower and the recovery tower, the gas phase at the top of the second pressure rectification tower is used for extracting the refined methanol, and the heat of the methanol steam is used for meeting the heat load of the reboiler at the bottom of the pre-rectification tower. The methanol steam heat at the top of the first pressurized rectifying tower is utilized for three times and four times, and the pre-rectifying tower, the newly added second pressurized rectifying tower and the newly added recovery tower do not need saturated steam as a heat source. The recovery tower is used for recovering methanol in fusel oil extracted from the side line of the normal pressure tower, and the recovery rate of the methanol is improved.
The scheme adopted by the invention is as follows:
a five-tower five-effect rectification process method for methanol comprises the following steps:
(1) crude methanol enters the pre-rectifying tower, a gas phase extracted from the top of the pre-rectifying tower is cooled by a pre-rectifying tower condenser, light components of non-condensable gas go to a torch system, a liquid phase flows back to the pre-rectifying tower, and a liquid phase extracted from the bottom of the pre-rectifying tower is pressurized by a pressure pump and enters the first pressurized rectifying tower;
(2) the gas phase extracted from the top of the first pressure rectifying tower is divided into three paths: the first path is connected to a tower bottom coupling reboiler of a second pressurized rectifying tower, the second path is connected to a tower bottom coupling reboiler of an atmospheric tower, the third path is connected to a tower bottom coupling reboiler of a recovery tower, heat sources are respectively provided for the second pressurized rectifying tower coupling reboiler, the atmospheric tower coupling reboiler and the recovery tower coupling reboiler, condensed liquid is converged into a stream, one part of the stream flows back to enter the first pressurized rectifying tower, the other part of the stream adopts a methanol product, and the stream adopted from the bottom of the first pressurized rectifying tower enters the second pressurized rectifying tower;
(3) a gas phase extracted from the top of the second pressurized rectifying tower is connected to a coupling reboiler at the bottom of the pre-rectifying tower to provide a heat source for the coupling reboiler at the bottom of the pre-rectifying tower, one part of a condensed liquid phase flows back to the second pressurized rectifying tower, the other part of the condensed liquid phase is extracted to obtain a qualified methanol product, and the liquid phase extracted from the bottom of the second pressurized rectifying tower is introduced to the atmospheric tower;
(4) gas phase is extracted from the top of the atmospheric tower, one part of condensed liquid phase flows back to the atmospheric tower, and the other part of liquid phase is extracted as a methanol product; qualified wastewater is extracted from the liquid phase at the bottom of the normal pressure tower, and fusel oil is extracted from the side line of the normal pressure tower and enters the recovery tower;
(5) and extracting a gas phase from the top of the recovery tower, refluxing one part of the condensed liquid phase into the recovery tower, extracting a methanol product from the other part of the condensed liquid phase, and extracting fusel oil from the bottom of the recovery tower to finish the whole rectification process.
The methanol gas phase at the top of the first pressure rectifying tower 2 is extracted and then divided into three material flows: the first material flow enters a reboiler at the bottom of a second pressurized rectifying tower, the second material flow enters a reboiler at the bottom of an atmospheric tower, the third material flow enters a reboiler at the bottom of a recovery tower, and heat exchange is carried out on the three material flows (the proportion is respectively 25-35%, 60-70% and 3.5-5%) with the reboilers at the bottoms of the second pressurized rectifying tower, the atmospheric tower and the recovery tower respectively, and the three material flows after heat exchange are combined into one material flow; the combined material flow is divided into two parts, one part of the combined material flow is used as reflux liquid to enter a first pressure rectifying tower, and the other part of the combined material flow is used as liquid phase to extract a methanol product (the proportion is 65-75 percent and 25-35 percent respectively).
And after the methanol gas phase at the top of the second pressurized rectifying tower is extracted, the material flow enters a reboiler at the bottom of the pre-rectifying tower and exchanges heat with the reboiler at the bottom of the pre-rectifying tower, the material flow after heat exchange is divided into two parts (the proportion is 70-80% and 20-30% respectively), one part is used as reflux liquid and enters the second pressurized rectifying tower, and the other part is used for extracting a methanol product.
The top liquid phase reflux of the pre-rectifying tower also comprises water (serving as an extracting agent), and the flow rate of the extracting water is 5-15% of that of the crude methanol.
The number of the pre-rectifying tower plates is 40-70, the operation temperature at the top of the pre-rectifying tower is 60-90 ℃, the operation pressure is 100-150KPa, the reflux ratio is 3.5-4.5, the temperature at the bottom of the pre-rectifying tower is 70-100 ℃, the operation pressure is 110-160KPa, and the feeding position is 9-14;
the tower number of the first pressurized rectifying tower is 70-100 layers, the operation temperature at the top of the tower is 100-140 ℃, the operation pressure is 500-900KPa, the reflux ratio is 1.5-3.5, the temperature at the bottom of the tower is 110-150 ℃, the operation pressure is 550-950KPa, and the feeding position is 63-80 blocks;
the number of the second pressure distillation tower plates is 70-90, the operation temperature at the top of the tower is 80-120 ℃, the operation pressure is 200-500KPa, the reflux ratio is 2.5-4.5, the temperature at the bottom of the tower is 90-130 ℃, the operation pressure is 250-550KPa, and the feeding position is 47-60;
the tower plate number of the atmospheric tower is 80-100 layers, the operation temperature of the tower top is 60-80 ℃, the operation pressure is 100-140KPa, the reflux ratio is 1.5-2.5, the temperature of the tower bottom is 90-130 ℃, the operation pressure is 120-160KPa, and the feeding position is 51-64 blocks;
the tower number of the recovery tower is 70-90 layers, the operation temperature at the top of the tower is 60-90 ℃, the operation pressure is 100-150KPa, the reflux ratio is 8-10, the temperature at the bottom of the tower is 90-120 ℃, the operation pressure is 140-190KPa, and the feeding position is 53-68.
The crude methanol feed consists of 85-90 w% of methanol, 2-5 w% of light components and 8-13 w% of heavy components;
the temperature difference between the tower top temperature of the first pressurized rectifying tower and the tower bottom temperature of the second pressurized rectifying tower, the tower bottom temperature of the atmospheric tower and the tower bottom temperature of the recovery tower is 10-25 ℃, and the temperature difference between the tower top temperature of the second pressurized rectifying tower and the tower bottom temperature of the pre-rectifying tower is 10-20 ℃.
The methanol content extracted from the top of the pre-rectifying tower is 50-70 w%, the methanol content extracted from the bottom of the pre-rectifying tower is 70-90 w%, and the methanol content extracted from the non-condensable gas after the condensation at the top of the pre-rectifying tower is 5-10 w%; the content of methanol extracted from the top of the first pressure rectifying tower is 99.99w percent, and the content of methanol extracted from the bottom of the first pressure rectifying tower is 60 to 80 percent; the content of methanol extracted from the top of the second pressure rectifying tower is 99.99w percent, and the content of methanol extracted from the bottom of the second pressure rectifying tower is 50-70w percent; the content of methanol extracted from the top of the atmospheric tower is 99.99w percent, the content of wastewater at the bottom of the atmospheric tower is 99.99w percent, and the content of methanol extracted from the side line is 20-25w percent; the content of methanol extracted from the top of the recovery tower is 99.99w percent, and the content of methanol extracted from the bottom of the recovery tower is 1-3w percent.
A five-tower five-effect rectification process device for methanol comprises a pre-rectification tower, a first pressurized rectification tower, a second pressurized rectification tower, an atmospheric tower and a recovery tower;
wherein the bottom of the pre-rectifying tower is connected with a pressure pump through a pipeline, and the pressure pump is also connected with a feed inlet of the first pressure rectifying tower; the tower kettle of the first pressurized rectifying tower is connected with the feed inlet of the second pressurized rectifying tower, and the tower kettle of the second pressurized rectifying tower is connected with the feed inlet of the atmospheric tower; the tower kettle of the atmospheric tower is connected with the feed inlet of the recovery tower;
the bottoms of the pre-rectifying tower, the second pressurized rectifying tower, the atmospheric tower and the recovery tower are respectively provided with a pre-rectifying tower bottom coupling reboiler, a second pressurized rectifying tower bottom coupling reboiler, an atmospheric tower bottom coupling reboiler and a recovery tower bottom coupling reboiler; the top parts of the pre-rectifying tower, the atmospheric tower and the recovery tower are respectively provided with a pre-rectifying tower condenser, an atmospheric tower condenser and a recovery tower condenser, the outflow pipeline of the atmospheric tower condenser is respectively connected with the top of the atmospheric tower and the methanol product extraction pipeline, and the outflow pipeline of the recovery tower condenser is respectively connected with the top of the recovery tower and the methanol product extraction pipeline; a corresponding reboiler, namely a first pressurized rectifying tower reboiler, is arranged at the bottom of the first pressurized rectifying tower;
the tower top of the first pressurized rectifying tower is respectively connected with the inflow of a tower bottom coupling reboiler, a tower bottom coupling reboiler of the atmospheric tower and a tower bottom coupling reboiler of the recovery tower through pipelines; the pipelines after the outflow confluence of the second pressurized rectifying tower bottom coupling reboiler, the atmospheric tower bottom coupling reboiler and the recovery tower bottom coupling reboiler are respectively connected with the tower top of the first pressurized rectifying tower and the methanol product extraction pipeline;
the top of the second pressurized rectifying tower is connected with an inflow pipeline of a coupling reboiler at the bottom of the pre-rectifying tower, and an outflow pipeline of the coupling reboiler at the bottom of the pre-rectifying tower is respectively connected with the top of the second pressurized rectifying tower and a methanol product extraction pipeline;
and a reflux liquid inlet of the condenser at the top of the pre-rectifying tower is also connected with an extraction water pipeline.
The invention adopts multi-effect rectification, and the technical scheme provided by the invention has the beneficial effects that:
according to the five-tower five-effect rectification process system for the methanol, steam at the top of the rectification tower with high operation pressure provides a heat source for a reboiler at the bottom of the rectification tower with low operation pressure, so that five times of heat utilization is formed, and energy consumption is reduced.
The extracted methanol product meets the standard, the ethanol content in the methanol product is less than or equal to 50ppm (wt), the recovery rate of the methanol is 99.79 percent, and the recovery rate is improved by 0.57 percent.
The invention has the beneficial effects that:
in the invention, the heat sources of the reboilers at the bottoms of the second pressurized rectifying tower, the atmospheric tower and the recovery tower are all from the heat of methanol steam at the top of the first pressurized rectifying tower, the heat source of the reboilers at the bottom of the pre-rectifying tower is from the heat of the methanol steam at the top of the second pressurized rectifying tower, and the heat of the methanol steam at the top of the first pressurized rectifying tower is utilized for three times and four times, thereby effectively reducing the unit energy consumption of methanol production. Meanwhile, the methanol in the fusel oil is recovered, so that the recovery rate of the methanol is improved. The steam consumption of refined methanol in a unit production unit by applying the five-tower five-effect rectification process of methanol is 0.800-0.850 kg (steam)/kg (methanol), and compared with the steam consumption of 1.183kg (steam)/kg (methanol) in three-tower double-effect rectification, the energy consumption is reduced by 28.15-32.38%.
Due to the presence of a certain amount of methanol in the fusel oil, the current methanol market price is 2270 yuan/ton, and the steam price is 50 yuan/ton. In the process, 460-480 kg/h of methanol is recovered, and the energy consumption of a reboiler at the bottom of a recovery tower is 1600 KW. Because the tower top steam of the first pressurized rectifying tower provides a heat source for the tower bottom reboilers of the second pressurized rectifying tower, the normal pressure tower and the recovery tower, the tower bottom reboilers of the second pressurized rectifying tower, the normal pressure tower and the recovery tower do not need saturated steam as a heat source, and the saturated steam is used as a heat source for the first pressurized rectifying tower. Therefore, the steam consumption of the recovery column was 1500 kg/h. Namely, the economic benefit of recycling the methanol every hour is 969.2-1014.6 yuan. The economic benefit of one year is 775.36-811.68 ten thousand yuan per year according to 8000 h.
Drawings
FIG. 1 is a schematic diagram of a five-tower five-effect rectification process and a five-tower five-effect rectification device for methanol in the invention.
In the figure: 1-a pre-rectifying tower, 2-a first pressurized rectifying tower, 3-a second pressurized rectifying tower, 4-an atmospheric tower, 5-a recovery tower, 6-a pre-rectifying tower condenser, 7-an atmospheric tower condenser, 8-a recovery tower condenser, 9-a pre-rectifying tower bottom coupling reboiler, 10-a first pressurized rectifying tower reboiler, 11-a second pressurized rectifying tower bottom coupling reboiler, 12-an atmospheric tower bottom coupling reboiler, 13-a recovery tower bottom coupling reboiler and 14-a pressurizing pump.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to the following embodiments and the accompanying drawings. It should be understood that the description of the specific embodiments is intended to be illustrative of the invention and is not intended to limit the invention.
The five-tower five-effect rectification process device for methanol is shown in figure 1 and comprises a pre-rectification tower 1, a first pressurized rectification tower 2, a second pressurized rectification tower 3, an atmospheric tower 4 and a recovery tower 5;
wherein, the bottom of the pre-rectifying tower is connected with a booster pump 14 through a pipeline, and the booster pump 14 is also connected with a feed inlet of the first pressurized rectifying tower 2; the tower kettle of the first pressurized rectifying tower 2 is connected with the feed inlet of the second pressurized rectifying tower 3, and the tower kettle of the second pressurized rectifying tower 3 is connected with the feed inlet of the atmospheric tower 4; the tower kettle of the atmospheric tower 4 is connected with the feed inlet of the recovery tower 5;
the bottoms of the pre-rectifying tower 1, the second pressurized rectifying tower 2, the atmospheric tower 4 and the recovery tower 5 are respectively provided with corresponding coupling reboilers, namely a second pressurized rectifying tower bottom coupling reboiler 11, an atmospheric tower bottom coupling reboiler 12 and a recovery tower bottom coupling reboiler 13; the top parts of the pre-rectifying tower 1, the atmospheric tower 4 and the recovery tower 5 are respectively provided with corresponding condensers, namely a pre-rectifying tower condenser 6, an atmospheric tower condenser 7 and a recovery tower condenser 8, wherein the outflow pipeline of the atmospheric tower condenser 7 is respectively connected with the top part of the atmospheric tower 4 and a methanol product extraction pipeline, and the outflow pipeline of the recovery tower condenser 8 is respectively connected with the top part of the recovery tower 5 and the methanol product extraction pipeline; a corresponding reboiler, namely a first pressurized rectifying tower reboiler 10, is arranged at the bottom of the first pressurized rectifying tower;
the top of the first pressurized rectifying tower 2 is respectively connected with the inflow of a second pressurized rectifying tower bottom coupling reboiler 11, a normal pressure tower bottom coupling reboiler 12 and a recovery tower bottom coupling reboiler 13 through pipelines; the outflow converged pipelines of the second pressurized rectifying tower bottom coupling reboiler 11, the atmospheric tower bottom coupling reboiler 12 and the recovery tower bottom coupling reboiler 13 are respectively connected with the tower top of the first pressurized rectifying tower 2 and a methanol product extraction pipeline;
the top of the second pressurized rectifying tower 3 is connected with an inflow pipeline of a coupling reboiler 9 at the bottom of the pre-rectifying tower, and an outflow pipeline of the coupling reboiler 9 at the bottom of the pre-rectifying tower is respectively connected with the top of the second pressurized rectifying tower 3 and a methanol product extraction pipeline;
and a reflux liquid inlet of the condenser at the top of the pre-rectifying tower 1 is also connected with an extraction water pipeline.
The five-tower five-effect rectification process method for methanol comprises the following steps:
(1) crude methanol enters the pre-rectifying tower 1, a gas phase extracted from the top of the pre-rectifying tower 1 is cooled by a pre-rectifying tower condenser 6, light components of non-condensable gas flow to a torch system, a liquid phase flows back to the pre-rectifying tower, and a liquid phase extracted from the bottom of the pre-rectifying tower 1 is pressurized by a pressure pump 14 and enters the first pressure rectifying tower 2;
(2) the gas phase extracted from the top of the first pressure rectifying tower 2 is divided into three paths: the first path is connected to a coupling reboiler 11 at the bottom of a second pressurized rectifying tower 3, the second path is connected to a coupling reboiler 12 at the bottom of an atmospheric tower 4, the third path is connected to a coupling reboiler 13 at the bottom of a recovery tower 5, heat sources are respectively provided for the coupling reboiler at the bottom of the second pressurized rectifying tower, the coupling reboiler at the bottom of the atmospheric tower and the coupling reboiler at the bottom of the recovery tower, condensed liquid is gathered into a stream, one part of the stream flows back to enter a first pressurized rectifying tower 2, the other part of the stream produces qualified methanol products, and the stream produced at the bottom of the first pressurized rectifying tower 2 enters the second pressurized rectifying tower 3;
(3) a gas phase is extracted from the top of the second pressurized rectifying tower 3, the gas phase is connected to a coupling reboiler 9 at the bottom of the pre-rectifying tower 1 to provide a heat source for the coupling reboiler at the bottom of the pre-rectifying tower, one part of a condensed liquid phase flows back to the second pressurized rectifying tower 3, the other part of the condensed liquid phase is extracted to obtain a qualified methanol product, and the liquid phase extracted from the bottom of the second pressurized rectifying tower 3 enters the atmospheric tower 4;
(4) a gas phase is extracted from the top of the atmospheric tower 4, one part of the condensed liquid phase flows back to the atmospheric tower 4, and qualified methanol products are extracted from the other part of the condensed liquid phase; qualified wastewater is extracted from the liquid phase at the bottom of the atmospheric tower, and fusel oil is extracted from the side line of the atmospheric tower and enters the recovery tower 5;
(5) and gas phase is extracted from the top of the recovery tower 5, one part of the condensed liquid phase flows back to enter the recovery tower, the other part of the condensed liquid phase is extracted to obtain qualified methanol products, and fusel oil is extracted from the bottom of the recovery tower, so that the whole rectification process is completed.
The methanol at the top of the first pressure rectifying tower 2 is extracted in a gas phase and then is divided into three streams (the proportions are respectively 25-35%, 60-70% and 3.5-5%): the first material flow enters a second pressurized rectifying tower bottom coupling reboiler 11, the second material flow enters a normal pressure tower bottom coupling reboiler 12, the third material flow enters a recovery tower bottom coupling reboiler 13, the three material flows are respectively subjected to heat exchange with the second pressurized rectifying tower 3, the normal pressure tower 4 and the recovery tower 5 bottom coupling reboilers, and the three material flows after heat exchange are combined into one material flow. The combined material flow is divided into two parts (the proportion is 65-75% and 25-35% respectively), one part is used as reflux liquid to enter the first pressure rectifying tower 2, and the other part is used as liquid phase to extract a methanol product.
And the material flow after the gas phase extraction of the methanol at the top of the second pressurized rectifying tower 3 enters a coupling reboiler 9 at the bottom of the pre-rectifying tower and exchanges heat with the coupling reboiler 9 at the bottom of the pre-rectifying tower, the material flow after heat exchange is divided into two parts (the proportion is respectively 70-80% and 20-30%), one part is used as reflux liquid to enter the second pressurized rectifying tower 3, and the other part is used as liquid phase extraction of a methanol product.
The top liquid phase reflux of the pre-rectifying tower 1 further comprises water (serving as an extracting agent), and the flow rate of the extracting water is 5-15% of that of the crude methanol.
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention.
The number of the pre-rectifying tower plates is 40-70, the operation temperature at the top of the pre-rectifying tower is 60-90 ℃, the operation pressure is 100-150KPa, the reflux ratio is 3.5-4.5, the temperature at the bottom of the pre-rectifying tower is 70-100 ℃, the operation pressure is 110-160KPa, and the feeding position is 9-14;
the tower number of the first pressurized rectifying tower is 70-100 layers, the operation temperature at the top of the tower is 100-140 ℃, the operation pressure is 500-900KPa, the reflux ratio is 1.5-3.5, the temperature at the bottom of the tower is 110-150 ℃, the operation pressure is 550-950KPa, and the feeding position is 63-80 blocks;
the number of the second pressure distillation tower plates is 70-90, the operation temperature at the top of the tower is 80-120 ℃, the operation pressure is 200-500KPa, the reflux ratio is 2.5-4.5, the temperature at the bottom of the tower is 90-130 ℃, the operation pressure is 250-550KPa, and the feeding position is 47-60;
the tower plate number of the atmospheric tower is 80-100 layers, the operation temperature of the tower top is 60-80 ℃, the operation pressure is 100-140KPa, the reflux ratio is 1.5-2.5, the temperature of the tower bottom is 90-130 ℃, the operation pressure is 120-160KPa, and the feeding position is 51-64 blocks;
the tower number of the recovery tower is 70-90 layers, the operation temperature at the top of the tower is 60-90 ℃, the operation pressure is 100-150KPa, the reflux ratio is 8-10, the temperature at the bottom of the tower is 90-120 ℃, the operation pressure is 140-190KPa, and the feeding position is 53-68.
The raw methanol feed consists of 85-90 w% of methanol, 2-5 w% of light components such as dimethyl ether, carbon monoxide, carbon dioxide and the like, and 8-13 w% of heavy components such as ethanol, amyl alcohol, water and the like; the methanol content extracted from the top of the pre-rectifying tower is 50-70 w%, the methanol content extracted from the bottom of the pre-rectifying tower is 70-90 w%, and the methanol content extracted from the non-condensable gas after the condensation at the top of the pre-rectifying tower is 5-10 w%; the content of methanol extracted from the top of the first pressure rectifying tower is 99.99w percent, and the content of methanol extracted from the bottom of the first pressure rectifying tower is 60 to 80 percent; the content of methanol extracted from the top of the second pressure rectifying tower is 99.99w percent, and the content of methanol extracted from the bottom of the second pressure rectifying tower is 50-70w percent; the content of methanol extracted from the top of the atmospheric tower is 99.99w percent, the content of wastewater at the bottom of the atmospheric tower is 99.99w percent, and the content of methanol extracted from the side line is 20-25w percent; the content of methanol extracted from the top of the recovery tower is 99.99w percent, and the content of methanol extracted from the bottom of the recovery tower is 1-3w percent.
Example 1
Crude methanol (the feeding amount is 96900kg/h, the methanol content is 87.9%) enters a pre-rectifying tower, the feeding temperature is 80 ℃, 56 layers of tower plates are arranged in the tower, light components in the crude methanol are extracted from the top of the pre-rectifying tower, the extracted temperature at the top of the tower is 76.0 ℃, the pressure is 130KPa, gas phase extracted from the top of the tower is cooled by a pre-rectifying tower condenser 6, and then the light components of non-condensable gas go to a torch system; liquid phase flows back to enter the pre-rectifying tower, the reflux ratio is 4.38, the reflux temperature is 40 ℃, and meanwhile, in order to further effectively remove impurities azeotropic with methanol in crude methanol, 9200kg/h of extract water is added to the top of the pre-rectifying tower, so that the treatment effect of the pre-rectifying tower is improved, and the quality of a methanol product is further improved. And pressurizing a liquid phase extracted from the bottom of the pre-rectifying tower by a pressurizing pump and feeding the liquid phase into a first pressurizing rectifying tower.
The first pressure rectifying tower is internally provided with 80 layers of tower plates, the gas phase is extracted from the top of the tower, the temperature extracted from the top of the tower is 123.2 ℃, the pressure is 700KPa, and the gas phase at the top of the tower is divided into three paths: the first path is connected to a coupling reboiler at the bottom of a second pressurized rectifying tower, the second path is connected to a coupling reboiler at the bottom of an atmospheric tower, the third path is connected to a coupling reboiler at the bottom of a recovery tower, heat sources are respectively provided for the coupling reboiler at the bottom of the second pressurized rectifying tower, the coupling reboiler at the bottom of the atmospheric tower and the coupling reboiler at the bottom of the recovery tower, liquid condensed after heat exchange is converged into a stream, one part of the stream flows back to enter the first pressurized rectifying tower, the reflux ratio is 2.52, the reflux temperature is 115.0 ℃, the qualified methanol product is extracted from the other part of liquid phase, the methanol content is 99.994%, the extraction temperature is 115.0 ℃, the pressure is 700KPa, and the liquid phase at the bottom of the first pressurized rectifying tower.
The content of methanol in aqueous methanol solution extracted from the bottom of the first pressurized rectifying tower is about 70.24%, the extraction temperature at the bottom of the tower is 132.7 ℃, the extraction pressure is 740KPa, the aqueous methanol solution enters the lower part of the second pressurized rectifying tower, 75 layers of tower plates are arranged in the second pressurized rectifying tower, the gas phase extracted from the top of the tower is 94.9 ℃ and 300KPa, the gas phase extracted from the top of the tower is connected to a coupling reboiler at the bottom of a pre-rectifying tower and provides a heat source for the coupling reboiler at the bottom of the pre-rectifying tower, part of the liquid phase condensed after heat exchange flows back to the second pressurized rectifying tower, the reflux ratio is 2.92, the reflux temperature is 94.9 ℃, the qualified methanol product is extracted from the other part of the liquid phase, the content of methanol is 99.998%, the extraction temperature is 94.9 ℃, the pressure is 300KPa, and the second pressurized rectifying liquid phase is extracted from the bottom.
The content of methanol in the aqueous methanol solution extracted from the bottom of the second pressurized rectifying tower is about 62.81%, the extraction temperature at the bottom of the tower is 107.9 ℃, the extraction pressure is 340KPa, the aqueous methanol solution enters the middle part of the atmospheric tower, 86 layers of tower plates are arranged in the atmospheric tower, the gas phase is extracted from the top of the tower, the extraction temperature at the top of the tower is 66.6 ℃, the pressure is 110KPa, one part of the condensed liquid phase reflows to enter the atmospheric tower, the reflux ratio is 1.7, the reflux temperature is 34.1 ℃, the qualified methanol product is extracted from the other part of the liquid phase, the content of methanol is 99.995%, the extraction temperature is 34.1 ℃, the pressure is 110KPa, the qualified wastewater is extracted from the bottom of the atmospheric tower, the water content is 99.999%, the content of methanol is 3ppm, and the fusel.
The methanol content in the fusel oil extracted from the side line of the atmospheric tower is 23.22 percent, the fusel oil extraction temperature is 91.5 ℃, the extraction pressure is 140.8KPa, the fusel oil enters the lower part of the recovery tower, 75 layers of tower plates are arranged in the recovery tower, the gas phase is extracted from the top of the tower, the extraction temperature at the top of the tower is 71.0 ℃, the pressure is 130KPa, one part of the condensed liquid phase reflows to enter the recovery tower, the reflux ratio is 9.2, the reflux temperature is 71.0 ℃, the qualified methanol product is extracted from the other part of the liquid phase, the methanol content is 99.999 percent, the extraction temperature is 71.0 ℃, the pressure is 130KPa, the fusel oil is extracted from the liquid phase at the bottom of the recovery tower, wherein the water content is 83.29 percent, the extraction temperature is 102.1.
The methanol products extracted from the top of the first pressurized rectifying tower, the second pressurized rectifying tower, the atmospheric tower and the recovery tower are mixed, the temperature of the extracted refined methanol is 40 ℃, the methanol content in the product is 99.995 percent, and the ethanol content is below 50 ppm.
In the process, the heat of the methanol steam extracted from the top of the first pressurized rectifying tower is reasonably distributed and utilized to meet the heat load of a coupling reboiler at the bottom of the second pressurized rectifying tower, the atmospheric tower and the recovery tower, the methanol steam extracted from the top of the second pressurized rectifying tower meets the heat load of the coupling reboiler at the bottom of the pre-rectifying tower, and the pre-rectifying tower does not need saturated steam as a heat source, so that the energy consumption of a rectifying system is reduced. Wherein the first pressure rectifying tower and the second pressure rectifying tower, the atmospheric tower and the recovery tower form four-effect rectification, and the second pressure rectifying tower and the pre-rectifying tower form five-effect rectification.
The steam consumption of each ton of refined methanol produced by the methanol five-tower five-effect rectification process is 0.834 ton, the recovery rate of the methanol is 99.79 percent, the energy consumption is reduced by 29.50 percent compared with the methanol three-tower double-effect rectification process, and the recovery rate of the methanol is improved by 0.57 percent;
table 1 operating parameters and data results
Example 2
The other steps are the same as the example 1, except that the amount of extraction water is 9200kg/h is replaced by 8000 kg/h; the reflux ratio of the first pressure distillation tower is 2.52 to 2.5, and the pressure is 700KPa to 680 KPa; the second pressure distillation column reflux ratio of 2.92 was replaced with 2.9.
Under the condition, the gas phase extraction temperature at the top of the pre-rectifying tower is 65.23 ℃, and the tower kettle temperature is 79.06 ℃; the gas phase extraction temperature of the top of the first pressure rectification tower is 122.14 ℃, and the tower kettle temperature is 131.40 ℃; the gas phase extraction temperature at the top of the second pressure rectifying tower is 94.88 ℃, and the tower kettle temperature is 107.58 ℃; the gas phase extraction temperature at the top of the atmospheric tower is 66.63 ℃, and the tower kettle temperature is 110.35 ℃; the gas phase extraction temperature at the top of the recovery tower is 70.99 ℃, and the tower kettle temperature is 102.14 ℃.
Table 2 operating parameters and data results
Finally, the description is as follows: the present invention is not limited to the above embodiments, and any modifications, equivalent replacements, and improvements made within the spirit of the present invention should be included in the protection scope of the present invention.
The invention is not the best known technology.
Claims (8)
1. A methanol five-tower five-effect rectification process method is characterized by comprising the following steps:
(1) crude methanol enters the pre-rectifying tower, a gas phase extracted from the top of the pre-rectifying tower is cooled by a pre-rectifying tower condenser, light components of non-condensable gas go to a torch system, a liquid phase flows back to the pre-rectifying tower, and a liquid phase extracted from the bottom of the pre-rectifying tower is pressurized by a pressure pump and enters the first pressurized rectifying tower;
(2) the gas phase extracted from the top of the first pressure rectifying tower is divided into three paths: the first path is connected to a tower bottom coupling reboiler of a second pressurized rectifying tower, the second path is connected to a tower bottom coupling reboiler of an atmospheric tower, the third path is connected to a tower bottom coupling reboiler of a recovery tower, heat sources are respectively provided for the second pressurized rectifying tower coupling reboiler, the atmospheric tower coupling reboiler and the recovery tower coupling reboiler, condensed liquid is converged into a stream, one part of the stream flows back to enter the first pressurized rectifying tower, the other part of the stream adopts a methanol product, and the stream adopted from the bottom of the first pressurized rectifying tower enters the second pressurized rectifying tower;
(3) a gas phase extracted from the top of the second pressurized rectifying tower is connected to a coupling reboiler at the bottom of the pre-rectifying tower to provide a heat source for the coupling reboiler at the bottom of the pre-rectifying tower, one part of a condensed liquid phase flows back to the second pressurized rectifying tower, the other part of the condensed liquid phase is extracted to obtain a qualified methanol product, and the liquid phase extracted from the bottom of the second pressurized rectifying tower is introduced to the atmospheric tower;
(4) gas phase is extracted from the top of the atmospheric tower, one part of condensed liquid phase flows back to the atmospheric tower, and the other part of liquid phase is extracted as a methanol product; qualified wastewater is extracted from the liquid phase at the bottom of the normal pressure tower, and fusel oil is extracted from the side line of the normal pressure tower and enters the recovery tower;
(5) extracting a gas phase from the top of the recovery tower, refluxing a part of condensed liquid phase into the recovery tower, extracting a methanol product from the other part of the condensed liquid phase, and extracting fusel oil from the bottom of the recovery tower to finish the whole rectification process;
the number of the pre-rectifying tower plates is 40-70, the operation temperature at the top of the pre-rectifying tower is 60-90 ℃, the operation pressure is 100-150KPa, the reflux ratio is 3.5-4.5, the temperature at the bottom of the pre-rectifying tower is 70-100 ℃, the operation pressure is 110-160KPa, and the feeding position is 9-14;
the tower number of the first pressurized rectifying tower is 70-100 layers, the operation temperature at the top of the tower is 100-140 ℃, the operation pressure is 500-900KPa, the reflux ratio is 1.5-3.5, the temperature at the bottom of the tower is 110-150 ℃, the operation pressure is 550-950KPa, and the feeding position is 63-80 blocks;
the number of the second pressure distillation tower plates is 70-90, the operation temperature at the top of the tower is 80-120 ℃, the operation pressure is 200-500KPa, the reflux ratio is 2.5-4.5, the temperature at the bottom of the tower is 90-130 ℃, the operation pressure is 250-550KPa, and the feeding position is 47-60;
the tower plate number of the atmospheric tower is 80-100 layers, the operation temperature of the tower top is 60-80 ℃, the operation pressure is 100-140KPa, the reflux ratio is 1.5-2.5, the temperature of the tower bottom is 90-130 ℃, the operation pressure is 120-160KPa, and the feeding position is 51-64 blocks;
the tower number of the recovery tower is 70-90 layers, the operation temperature at the top of the tower is 60-90 ℃, the operation pressure is 100-150KPa, the reflux ratio is 8-10, the temperature at the bottom of the tower is 90-120 ℃, the operation pressure is 140-190KPa, and the feeding position is 53-68.
2. The five-tower five-effect rectification process method for methanol as claimed in claim 1, characterized in that the methanol at the top of the first pressurized rectification tower is separated into three streams after gas phase extraction: the first material flow enters a reboiler at the bottom of a second pressurized rectifying tower, the second material flow enters a reboiler at the bottom of an atmospheric tower, the third material flow enters a reboiler at the bottom of a recovery tower, and heat exchange is carried out on the three material flows (the proportion is respectively 25-35%, 60-70% and 3.5-5%) with the reboilers at the bottoms of the second pressurized rectifying tower, the atmospheric tower and the recovery tower respectively, and the three material flows after heat exchange are combined into one material flow; the combined material flow is divided into two parts, one part of the material flow is used as reflux liquid to enter a first pressure rectifying tower, and the other part of the material flow is used for extracting a methanol product (the proportion is 65-75 percent and 25-35 percent respectively);
and after the methanol gas phase at the top of the second pressurized rectifying tower is extracted, the material flow enters a reboiler at the bottom of the pre-rectifying tower and exchanges heat with the reboiler at the bottom of the pre-rectifying tower, the material flow after heat exchange is divided into two parts (the proportion is 70-80% and 20-30% respectively), one part is used as reflux liquid and enters the second pressurized rectifying tower, and the other part is used for extracting a methanol product.
3. The five-tower five-effect rectification process method for methanol as claimed in claim 1, wherein the overhead liquid phase reflux of the pre-rectification tower further comprises water, and the flow rate of the extraction water is 5-15% of the flow rate of the crude methanol.
4. The five-tower five-effect rectification process method of methanol as claimed in claim 1, characterized in that the crude methanol feed comprises 85-90 w% of methanol, 2-5 w% of light components and 8-13 w% of heavy components.
5. The temperature difference between the tower top temperature of the first pressurized rectifying tower and the tower bottom temperature of the second pressurized rectifying tower, the tower bottom temperature of the atmospheric tower and the tower bottom temperature of the recovery tower is 10-25 ℃, and the temperature difference between the tower top temperature of the second pressurized rectifying tower and the tower bottom temperature of the pre-rectifying tower is 10-20 ℃.
6. The five-tower five-effect rectification process method of methanol as claimed in claim 1, characterized in that the pre-rectification tower has a top methanol content of 50-70 w%, a bottom methanol content of 70-90 w%, and a top condensed noncondensable gas methanol content of 5-10 w%; the content of methanol extracted from the top of the first pressure rectifying tower is 99.99w percent, and the content of methanol extracted from the bottom of the first pressure rectifying tower is 60 to 80 percent; the content of methanol extracted from the top of the second pressure rectifying tower is 99.99w percent, and the content of methanol extracted from the bottom of the second pressure rectifying tower is 50-70w percent; the content of methanol extracted from the top of the atmospheric tower is 99.99w percent, the content of wastewater at the bottom of the atmospheric tower is 99.99w percent, and the content of methanol extracted from the side line is 20-25w percent; the content of methanol extracted from the top of the recovery tower is 99.99w percent, and the content of methanol extracted from the bottom of the recovery tower is 1-3w percent.
7. A methanol five-tower five-effect rectification process device is characterized by comprising a pre-rectification tower, a first pressurized rectification tower, a second pressurized rectification tower, an atmospheric tower and a recovery tower;
wherein the bottom of the pre-rectifying tower is connected with a pressure pump through a pipeline, and the pressure pump is also connected with a feed inlet of the first pressure rectifying tower; the tower kettle of the first pressurized rectifying tower is connected with the feed inlet of the second pressurized rectifying tower, and the tower kettle of the second pressurized rectifying tower is connected with the feed inlet of the atmospheric tower; the tower kettle of the atmospheric tower is connected with the feed inlet of the recovery tower;
the bottoms of the pre-rectifying tower, the second pressurized rectifying tower, the atmospheric tower and the recovery tower are respectively provided with a pre-rectifying tower bottom coupling reboiler, a second pressurized rectifying tower bottom coupling reboiler, an atmospheric tower bottom coupling reboiler and a recovery tower bottom coupling reboiler; the top parts of the pre-rectifying tower, the atmospheric tower and the recovery tower are respectively provided with a pre-rectifying tower condenser, an atmospheric tower condenser and a recovery tower condenser, the outflow pipeline of the atmospheric tower condenser is respectively connected with the top of the atmospheric tower and the methanol product extraction pipeline, and the outflow pipeline of the recovery tower condenser is respectively connected with the top of the recovery tower and the methanol product extraction pipeline; a corresponding reboiler, namely a first pressurized rectifying tower reboiler, is arranged at the bottom of the first pressurized rectifying tower;
the tower top of the first pressurized rectifying tower is respectively connected with the inflow of a tower bottom coupling reboiler, a tower bottom coupling reboiler of the atmospheric tower and a tower bottom coupling reboiler of the recovery tower through pipelines; the pipelines after the outflow confluence of the second pressurized rectifying tower bottom coupling reboiler, the atmospheric tower bottom coupling reboiler and the recovery tower bottom coupling reboiler are respectively connected with the tower top of the first pressurized rectifying tower and the methanol product extraction pipeline;
the top of the second pressurized rectifying tower is connected with an inflow pipeline of a coupling reboiler at the bottom of the pre-rectifying tower, and an outflow pipeline of the coupling reboiler at the bottom of the pre-rectifying tower is respectively connected with the top of the second pressurized rectifying tower and a methanol product extraction pipeline.
8. The five-tower five-effect methanol rectification process unit as claimed in claim 7, wherein the reflux inlet of the condenser at the top of the pre-rectification tower is also connected with the extraction water pipeline.
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