CN112479821A - Method and system for reducing fusel oil production in crude methanol refining process - Google Patents
Method and system for reducing fusel oil production in crude methanol refining process Download PDFInfo
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Abstract
The invention relates to the field of crude methanol refining, and discloses a method and a system for reducing fusel oil production in a crude methanol refining process. By improving the temperature of condensation treatment after pre-rectification, condensing the non-condensable gas for recycling and adjusting the overflow amount of the fusel oil of the pre-rectification tower and the optimized normal pressure tower, under the condition of ensuring the quality of the refined methanol, the extraction of the fusel oil is greatly reduced, and even the effect of near-zero extraction can be realized.
Description
Technical Field
The invention relates to the field of crude methanol refining, in particular to a method and a system for reducing fusel oil extraction in a crude methanol refining process.
Background
The crude methanol is refined to obtain a methanol product, and for example, the methanol product can be refined by adopting a three-tower rectification process, wherein the three towers are a pre-rectification tower, a pressurization tower and an atmospheric tower respectively.
The removal of fusel oil from crude methanol is a key factor affecting the quality of refined methanol products, and the extraction process of fusel oil inevitably extracts part of methanol. The fusel oil extracted by a measuring line of the recovery tower contains about 50 percent of methanol and other components which are easy to form binary and multi-component azeotropes, so the recovery of the methanol in the fusel oil is difficult, and in order to reduce the cost of further treatment, the methanol is often treated in the form of the fusel oil, such as being directly sold or discharged into waste water, thereby causing resource waste.
Disclosure of Invention
The invention aims to solve the problems of large methanol proportion and low methanol yield in fusel oil removed in the process of refining the existing crude methanol to obtain a methanol product, and provides a method and a system for reducing the extraction of the fusel oil in a crude methanol refining process.
In order to achieve the above object, a first aspect of the present invention provides a method for reducing fusel oil production in a crude methanol refining process, the method comprising: refining the crude methanol by adopting a three-tower rectification process, wherein,
(1) pre-rectifying crude methanol to obtain a first light component and a bottom liquid of a pre-rectifying tower, carrying out first condensation treatment on the first light component to obtain a second light component and a first condensate, carrying out second condensation treatment on the second light component to obtain non-condensable gas and a second condensate, carrying out third condensation treatment on the non-condensable gas to obtain a third condensate, and recycling the third condensate for pre-rectifying;
(2) the first condensate is subjected to first overflow to obtain a first overflow material, and the second condensate is subjected to second overflow to obtain a second overflow material; separating the first overflowing material and the second overflowing material to obtain waste liquid and recovery liquid; refluxing the recovery solution for the pre-rectification in the step (1);
wherein the temperature of the first condensation is 68-72 ℃, the temperature of the second condensation is 47-50 ℃, and the temperature of the third condensation is 25-35 ℃.
Preferably, the frequency of the first overflow is 10 times per month or less; and/or
Preferably, the frequency of the second flooding is 10 or less per month.
Preferably, the total overflow amount of the first overflow and the second overflow is 0.04-0.2 vol% of the methanol production per month.
Preferably, the method further comprises: and (3) sequentially carrying out pressure rectification and normal pressure rectification on the bottom liquid of the pre-rectifying tower to obtain a fusel oil material, and separating the fusel oil material.
Preferably, the amount of fusel oil material withdrawn is 0.05-0.1% by volume based on the volume of pre-rectifying column feed per month.
The second aspect of the present invention provides a system for reducing fusel oil extraction in a crude methanol refining process, wherein the system is a three-tower rectification system, and comprises:
the pre-rectifying tower is used for carrying out pre-rectifying treatment on the crude methanol to obtain a first light component and a pre-rectifying tower bottom liquid;
the pre-tower top primary condenser is used for carrying out first condensation treatment on the first light component to obtain a second light component and first condensate;
the pre-tower top secondary condenser is used for carrying out secondary condensation treatment on the second light component to obtain non-condensable gas and second condensate;
the pre-tower reflux tank is used for performing first overflow on the first condensate to obtain a first overflow material;
the methanol analyzer is used for carrying out second overflow on the second condensate to obtain a second overflow material;
the separation unit is used for separating the first overflow material from the second overflow material to obtain waste liquid and recovery liquid;
the condensing device is used for carrying out third condensation treatment on the non-condensable gas to obtain third condensate;
the separation unit is communicated with the pre-rectifying tower through a pipeline and is used for refluxing the recovery liquid to the pre-rectifying tower for pre-rectification;
the condensing device is communicated with the pre-rectifying tower through a pipeline and is used for refluxing the third condensate to the pre-rectifying tower for pre-rectification.
By adopting the method of the invention to further adjust the overflow amount of the fusel oil of the pre-rectifying tower and the optimized normal pressure tower, the extraction of the fusel oil is greatly reduced under the condition of ensuring the quality of the refined methanol, and even the effect of near-zero extraction can be realized.
Drawings
FIG. 1 is a schematic diagram of a system for reducing fusel oil production in a crude methanol refining process according to the present invention.
Description of the reference numerals
T1001, pre-rectifying tower E1002, pre-tower top first-stage condenser E1003 and pre-tower top second-stage condenser
D1009, pre-tower reflux tank D1010, methanol analyzer D1014 and fusel oil storage tank
D1004, blowdown storage tank D1005, collecting tank T1002, pressurized column
T1003, atmospheric tower L1001 and condensing unit
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
In the present invention, fusel oil mainly refers to isoamyl alcohol, butanol and propanol. It should be understood that the fusel oil of the present invention also contains methanol and the like.
The invention provides a method for reducing fusel oil extraction in a crude methanol refining process, which comprises the following steps: refining the crude methanol by adopting a three-tower rectification process, wherein,
(1) pre-rectifying crude methanol to obtain a first light component and a bottom liquid of a pre-rectifying tower, carrying out first condensation treatment on the first light component to obtain a second light component and a first condensate, carrying out second condensation treatment on the second light component to obtain non-condensable gas and a second condensate, carrying out third condensation treatment on the non-condensable gas to obtain a third condensate, and recycling the third condensate for pre-rectifying;
(2) the first condensate is subjected to first overflow to obtain a first overflow material, and the second condensate is subjected to second overflow to obtain a second overflow material; separating the first overflowing material and the second overflowing material to obtain waste liquid and recovery liquid; refluxing the recovery solution for the pre-rectification in the step (1);
wherein the temperature of the first condensation is 68-72 ℃, the temperature of the second condensation is 47-50 ℃, and the temperature of the third condensation is 25-35 ℃.
Through improving first condensing temperature and second condensing temperature for noncondensable gas extraction volume increases, and then improves the quality of thick methyl alcohol after the tower processing in advance, guarantees under the condition that fusel oil subtracts the production that the fine methyl alcohol quality is qualified, can not produce negative effects.
In the present invention, the conditions of the pre-rectification may be those conventional in the art, and may include, for example: the temperature is 65-85 deg.C, and the pressure is 0.025-0.06 MPa.
More specifically, preferably, the conditions of the pre-rectification include: the temperature of the tower bottom is 70-74 ℃, and the pressure is 0.043-0.045 MPa; the temperature at the top of the tower is 69-72 ℃, and the pressure is 0.029-0.031 MPa.
The pre-rectification may be performed in a pre-rectification column.
In the present invention, the first condensate is subjected to the first overflow to obtain the first overflow material, and for the purpose of reducing the fusel oil production amount, preferably, the first overflow is performed less than 10 times per month, such as 10 times per month, 9 times per month, 8 times per month, 7 times per month, 6 times per month, 5 times per month, 4 times per month, 3 times per month, 2 times per month, 1 time per month, and any range between any two values. More preferably, the frequency of the first flooding is 4 or less per month.
In the present invention, the second condensate is subjected to a second overflow to obtain a second overflow material, and the second overflow is frequently less than 10 times per month for the purpose of reducing the fusel oil production amount, and may be, for example, 10 times per month, 9 times per month, 8 times per month, 7 times per month, 6 times per month, 5 times per month, 4 times per month, 3 times per month, 2 times per month, 1 time per month, and any range between any two values. More preferably, the frequency of the second flooding is 4 or less per month.
Preferably, the total overflow volume of the first overflow and the second overflow is 0.04-0.2 vol% of the methanol production, such as may be 0.1, 0.12, 0.14, 0.16, 0.18, 0.2 and any range of compositions between any two values, in monthly units of time.
Preferably, the volume ratio of the overflow amount of the first overflow to the overflow amount of the second overflow is 1: 0.3-0.5.
In the present invention, if the overflow frequency is adjusted from a higher overflow frequency to a lower overflow frequency, the adjustment can be performed in a stepwise decreasing manner, such as decreasing from the regular once a day to 10 times a month, decreasing again to 4 times a month, and finally decreasing to 1 time a month.
The first overflow and the second overflow may or may not be performed simultaneously, and for convenience of operation, the first overflow and the second overflow are performed simultaneously.
In the present invention, the material may be subjected to condensation treatment using process water such as desalted water and cold seal water.
The third condensate contains mainly methanol. The non-condensable gas after the third condensation treatment mainly contains aldehyde, ketone, ether, alkane and the like, and can be directly incinerated.
In the invention, the crude methanol is subjected to pre-rectification treatment to obtain a first light component and a pre-rectification tower bottom liquid, the pre-rectification tower bottom liquid can be subjected to rectification treatment, and fusel oil is extracted from a side line, so that the purity of the methanol is improved, and the purpose of refining the methanol is realized. Preferably, the method further comprises: and (3) sequentially carrying out pressure rectification and normal pressure rectification on the bottom liquid of the pre-rectifying tower to obtain a fusel oil material, and separating the fusel oil material.
It will be appreciated that in a three column rectification process, the pre-rectification bottoms are sequentially rectified in a pressurized column and an atmospheric column, respectively, and the fusel oil feed is taken off the side stream of the atmospheric column.
In order to reduce the fusel oil extraction and meet the quality of a methanol product, preferably, the extraction amount of the fusel oil material is 0.05-0.1% by volume by taking the volume of the feeding amount of the pre-rectifying tower as a reference in unit time every month; more preferably 0.05 to 0.08 vol%. That is, the volume of fusel oil material produced in a month is 0.05-0.1% by volume, compared to the total volume of pre-rectification column bottoms in that month; more preferably 0.05 to 0.08 vol%.
It should be understood that in actual operation, as the performance of the methanol synthesis catalyst changes, the content of the by-products changes correspondingly, and the side-draw amount of the fusel oil needs to be adjusted. For example, in the initial stage of catalyst operation, the byproduct is less, the extraction amount can be in a lower range, and as the operation time is prolonged, the proportion of the byproduct is increased, and at this time, the side extraction amount of the fusel oil needs to be increased.
If the side-draw amount of the fusel oil is adjusted to be lower than the side-draw amount of the fusel oil, the side-draw amount of the fusel oil can be adjusted in a gradually decreasing mode, for example, the side-draw amount of the fusel oil is adjusted to be 0.16m3Reduction of the reaction time/h to 0.1m3At the time of/h, can be from 0.16m3The volume/h is reduced to 0.15m3H, finally reduced to 0.1m3/h。
Preferably, the frequency of side draws is 2-4 times per month, such as may be 4 times per month, 3 times per month, 2 times per month, and any range between any two values.
In the present invention, the conditions for rectification may be those conventional in the art, for example, in pressure rectification, the conditions include: the temperature is 100 ℃ and 140 ℃, and the pressure is 0.27-0.8 MPa; in atmospheric distillation, the conditions include: the temperature is 60-110 ℃, and the pressure is 0-0.06 MPa.
More specifically, preferably, the conditions of the pressure distillation include: the temperature at the bottom of the tower is 120 ℃ and 128 ℃, and the pressure is 0.45-0.55 MPa; the temperature at the top of the tower is 110 ℃ and 120 ℃, and the pressure is 0.48-0.57 MPa.
More specifically, preferably, the conditions of the atmospheric distillation include: the temperature of the tower bottom is 96-103 ℃, and the pressure is 0.02-0.03 MPa; the temperature at the top of the tower is 61-64 ℃ and the pressure is 0.005-0.01 MPa.
In the present invention, preferably, the method of separation comprises: performing first separation on the first overflow material and the second overflow material to obtain a first recovery liquid and a first waste liquid, and performing second separation on the first waste liquid to obtain a second recovery liquid and a second waste liquid; and (3) refluxing the first recovery liquid and the second recovery liquid for the pre-rectification in the step (1).
In a preferred embodiment of the invention, the method of separation comprises: performing first separation on the first overflowing material, the second overflowing material and the fusel oil material to obtain a first recovery liquid and a first waste liquid, and performing second separation on the first waste liquid to obtain a second recovery liquid and a second waste liquid; and (3) refluxing the first recovery liquid and the second recovery liquid for the pre-rectification in the step (1).
Preferably, the first separation is performed in a fusel oil reservoir and the second separation is performed in a blowdown reservoir. And when the material in the fusel oil storage tank reaches 50-70% of the volume of the fusel oil storage tank and no new material is input for 20-50h, performing first separation to obtain a first recovery liquid and a first waste liquid. Under the condition that no new material is input, the material in the fusel oil storage tank can be automatically layered, wherein the upper material and the bottom material are first waste liquid and are conveyed to a pollution discharge storage tank; and (3) taking the middle material as a first recovery liquid, recovering and returning to the pre-rectification in the step (1).
Preferably, after the material in the blowdown storage tank reaches 70-90 vol% of the volume of the blowdown storage tank and no new material is input for 20-50h, performing second separation to obtain a second recovery liquid and a second waste liquid. Under the condition that no new material is input, the material in the blowdown storage tank can be automatically layered, wherein the upper material (generally about 10 volume percent of the total volume of the material) and the bottom material (generally about 10 volume percent of the total volume of the material) are second waste liquid and are conveyed to the blowdown storage tank; and (3) taking the middle material as a second recovery liquid, recovering and returning to the pre-rectification in the step (1).
In the invention, the first recovery liquid, the second recovery liquid and the third condensate all belong to materials with higher methanol content and all belong to reflux liquid, and the reflux is carried out for pre-rectification.
The main components of the first waste liquid and the second waste liquid are methanol and fusel oil, wherein the content of the methanol is controlled within the range of 40-50% by volume, and the balance is the fusel oil which can be sold for treatment.
In the present invention, the pressure means a gauge pressure.
The second aspect of the present invention provides a system for reducing fusel oil extraction in a crude methanol refining process, wherein the system is a three-tower rectification system, and comprises:
the pre-rectifying tower is used for carrying out pre-rectifying treatment on the crude methanol to obtain a first light component and a pre-rectifying tower bottom liquid;
the pre-tower top primary condenser is used for carrying out first condensation treatment on the first light component to obtain a second light component and first condensate;
the pre-tower top secondary condenser is used for carrying out secondary condensation treatment on the second light component to obtain non-condensable gas and second condensate;
the pre-tower reflux tank is used for performing first overflow on the first condensate to obtain a first overflow material;
the methanol analyzer is used for carrying out second overflow on the second condensate to obtain a second overflow material;
the separation unit is used for separating the first overflow material from the second overflow material to obtain waste liquid and recovery liquid;
the condensing device is used for carrying out third condensation treatment on the non-condensable gas to obtain third condensate;
the separation unit is communicated with the pre-rectifying tower through a pipeline and is used for refluxing the recovery liquid to the pre-rectifying tower for pre-rectification;
the condensing device is communicated with the pre-rectifying tower through a pipeline and is used for refluxing the third condensate to the pre-rectifying tower for pre-rectification.
Preferably, the system further comprises:
the pressurizing tower is used for performing pressurized rectification treatment on the bottom liquid of the pre-rectifying tower to obtain bottom liquid of the pressurizing tower and a product methanol at the top of the pressurizing tower;
the atmospheric tower is used for carrying out atmospheric rectification treatment on the tower bottom liquid from the pressurizing tower to obtain fusel oil materials and methanol products at the top of the atmospheric tower;
the normal pressure tower is connected with the separation unit through a pipeline and is used for separating the fusel oil material.
Preferably, the separation unit comprises:
the fusel oil storage tank is used for carrying out first separation on the first overflowing material and the second overflowing material to obtain a first recovery liquid and a first waste liquid; and
the blowdown storage tank is used for carrying out second separation on the first waste liquid to obtain a second recovery liquid and a second waste liquid;
and the fusel oil storage tank and/or the blowdown storage tank are/is connected with the pre-rectifying tower through a pipeline and used for refluxing the recovery liquid to the pre-rectifying tower for pre-rectification.
In the present invention, the materials (i.e., the recovered liquids, such as the first recovered liquid, the second recovered liquid and the third condensed liquid) to be refluxed to the pre-rectification column for pre-rectification may be temporarily stored and then refluxed to the pre-rectification column.
In the present invention, preferably, the system further comprises a collecting tank for collecting the recovery liquid, and the collecting tank is connected with the fusel oil storage tank, the blowdown storage tank, the leaching unit and the pre-rectifying tower through pipelines for refluxing the recovery liquid to the pre-rectifying tower for pre-rectification.
The equipment included in the system is commercially available.
In a preferred embodiment of the present invention, as shown in fig. 1, the system for reducing fusel oil production in a crude methanol refining process comprises:
the pre-rectifying tower T1001 is used for carrying out pre-rectifying treatment on the crude methanol to obtain a first light component and a pre-rectifying tower bottom liquid;
the pressurizing tower T1002 is used for performing pressurized rectification treatment on the bottom liquid of the pre-rectifying tower to obtain bottom liquid of the pressurizing tower and a product methanol at the top of the pressurizing tower;
the atmospheric tower T1003 is used for carrying out atmospheric rectification treatment on the tower bottom liquid from the pressurizing tower T1002 to obtain fusel oil materials and methanol which is a product at the top of the atmospheric tower;
the pre-tower top primary condenser E1002 is used for carrying out first condensation treatment on the first light component to obtain a second light component and first condensate;
the pre-tower top secondary condenser E1003 is used for carrying out second condensation treatment on the second light component to obtain non-condensable gas and second condensate;
the pre-tower reflux groove D1009 is used for performing first overflow on the first condensate to obtain a first overflow material;
a methanol analyzer D1010, configured to perform a second overflow on the second condensate to obtain a second overflow material;
the fusel oil storage tank D1014 is connected with the pre-tower reflux tank D1009, the methanol analyzer D1010 and the atmospheric tower T1003 through pipelines and is used for carrying out first separation on the first overflow material, the second overflow material and the fusel oil material to obtain a first recovery liquid and a first waste liquid;
a blowdown storage tank D1004 for performing a second separation on the first waste liquid to obtain a second recovered liquid and a second waste liquid;
the collecting tank D1005 is used for collecting the recovered liquid, is connected with the fusel oil storage tank D1014, the blowdown storage tank D1004 and the pre-rectifying tower T1001 through pipelines, and is used for refluxing the recovered liquid to the pre-rectifying tower for pre-rectification;
the condensing device L1001 is used for carrying out third condensation treatment on the non-condensable gas to obtain third condensate;
wherein the condensing device L1001 is communicated with a collecting tank D1005 through a pipeline and is used for refluxing the third condensate to a pre-rectifying tower for pre-rectification.
The system can adopt the method of the first aspect to realize the effect of reducing fusel oil production in the crude methanol refining process.
The present invention will be described in detail below by way of examples.
The crude methanol material is crude methanol prepared by a methanol synthesis process.
In the following examples, crude methanol was refined by a two-column refining process.
In the following examples, the content of fusel oil was measured by the GB/T6283-; the content of methanol was measured by the method of Q/SNCC-J-05-2014-4020.
In the following examples, unless otherwise specified, a system for reducing fusel oil production in a crude methanol refining process is shown in fig. 1, and specifically, the system comprises:
the pre-rectifying tower T1001 is used for carrying out pre-rectifying treatment on the crude methanol to obtain a first light component and a pre-rectifying tower bottom liquid;
the pressurizing tower T1002 is used for performing pressurized rectification treatment on the bottom liquid of the pre-rectifying tower to obtain bottom liquid of the pressurizing tower and a product methanol at the top of the pressurizing tower;
the atmospheric tower T1003 is used for carrying out atmospheric rectification treatment on the tower bottom liquid from the pressurizing tower T1002 to obtain fusel oil materials and methanol which is a product at the top of the atmospheric tower;
the pre-tower top primary condenser E1002 is used for carrying out first condensation treatment on the first light component to obtain a second light component and first condensate;
the pre-tower top secondary condenser E1003 is used for carrying out second condensation treatment on the second light component to obtain non-condensable gas and second condensate;
the pre-tower reflux groove D1009 is used for performing first overflow on the first condensate to obtain a first overflow material;
a methanol analyzer D1010, configured to perform a second overflow on the second condensate to obtain a second overflow material;
the fusel oil storage tank D1014 is connected with the pre-tower reflux tank D1009, the methanol analyzer D1010 and the normal pressure tower through pipelines and is used for carrying out first separation on the first overflow material, the second overflow material and the fusel oil material of the normal pressure tower to obtain a first recovery liquid and a first waste liquid;
a blowdown storage tank D1004 for performing a second separation on the first waste liquid to obtain a second recovered liquid and a second waste liquid;
the collecting tank D1005 is used for collecting the recovered liquid, is connected with the fusel oil storage tank D1014, the blowdown storage tank D1004 and the pre-rectifying tower through pipelines, and is used for refluxing the recovered liquid to the pre-rectifying tower for pre-rectifying;
the condensing device L1001 is used for carrying out third condensation treatment on the non-condensable gas to obtain third condensate;
wherein the condensing device L1001 is communicated with a collecting tank D1005 through a pipeline and is used for refluxing the third condensate to a pre-rectifying tower for pre-rectification.
The process is a crude methanol refining process of 25 ten thousand tons/year, wherein the volume of the pre-rectifying tower is 15.27m3The volume of the pressurized column was 16.48m3The volume of the atmospheric tower is 27.68m3. The working conditions of the pre-rectifying tower comprise: the temperature of the tower bottom is 70-74 ℃, and the pressure is 0.043-0.045 MPa; the temperature at the top of the tower is 69-72 ℃, and the pressure is 0.029-0.031 MPa; the operating conditions of the pressurized column include: the temperature at the bottom of the tower is 120 ℃ and 128 ℃, and the pressure is 0.45-0.55 MPa; the temperature at the top of the tower is 110-120 ℃, the pressure is 0.48-0.57MPa, and the working conditions of the atmospheric tower comprise: the temperature of the tower bottom is 96-103 ℃, and the pressure is 0.02-0.03 MPa; the temperature at the top of the tower is 61-64 ℃ and the pressure is 0.005-0.01 MPa.
The material used for condensation is, unless otherwise specified, desalted water at 25-35 ℃.
The methanol content of the export product of fusel oil is about 45 vol%.
Example 1
This example illustrates the reduction of fusel oil production in a crude methanol refining process according to the present invention.
And (3) feeding the crude methanol into a pre-rectifying tower for pre-rectifying, extracting a first light component from the tower top, and extracting a bottom liquid of the pre-rectifying tower from the tower bottom. And conveying the bottom liquid of the pre-rectifying tower to a pressurized rectifying tower for pressurized rectification, conveying the bottom liquid of the pressurized rectifying tower to an atmospheric rectifying tower for atmospheric rectification, and collecting fusel oil materials at the side line of the atmospheric rectifying tower. Wherein, each month, the extraction frequency of the fusel oil is 1 time, and the extraction amount of the fusel oil material is 0.05-0.08 volume percent of the volume of the feed amount of the pre-rectification.
Carrying out first condensation treatment on the first light component to obtain a second light component and a first condensate; carrying out second condensation treatment on the second light component to obtain non-condensable gas and second condensate; and carrying out third condensation treatment on the non-condensable gas to obtain third condensate and the non-condensable gas subjected to the third condensation treatment, conveying the third condensate to the collecting tank, and incinerating the non-condensable gas subjected to the third condensation treatment. Wherein the temperature of the first condensation is 70 ℃, the temperature of the second condensation is 48 ℃, and the temperature of the third condensation is 30 ℃.
And carrying out first overflow on the first condensate in a pre-tower reflux tank to obtain a first overflow material, carrying out second overflow on the second condensate in a methanol analyzer to obtain a second overflow material, conveying the first overflow material, the second overflow material and the fusel oil material to a fusel oil storage tank, and carrying out first separation in the fusel oil storage tank to obtain a first recovery liquid and a first waste liquid.
Wherein, the frequency of the first overflow is gradually adjusted from 10 times per month to 4 times per month, and finally to 1 time per month; and the frequency control of the second overflow is synchronous with the frequency control of the first overflow. The total overflow was controlled to be 0.04-0.08 vol% of methanol production per month. The volume ratio of the overflow quantity of the first overflow to the overflow quantity of the second overflow is about 1: 0.4.
wherein the first separation method comprises the following steps: when the material in the fusel oil storage tank reaches 60 volume percent of the volume of the fusel oil storage tank and no new material is input for 24 hours, the material in the fusel oil storage tank can be automatically layered, and the upper material (about 10 volume percent of the total volume of the material) and the bottom material (about 10 volume percent of the total volume of the material) are first waste liquid and are conveyed to a pollution discharge storage tank; the middle material is first recovery liquid and is conveyed to the collecting tank for temporary storage.
And carrying out second separation on the first waste liquid to obtain a second recovery liquid and a second waste liquid. Wherein the second separation method comprises: when the volume of the materials in the blowdown storage tank reaches 80% of the volume of the blowdown storage tank and no new materials are input for 24 hours, the materials in the fusel oil storage tank can be automatically layered, and the upper materials (about 10% of the total volume of the materials) and the bottom materials (about 10% of the total volume of the materials) are second waste liquid and are discharged as fusel oil products to be sold; and the middle material is a second recovery liquid and is conveyed to the collecting tank for temporary storage.
And refluxing the recovery liquid in the collecting tank to a pre-rectifying tower for pre-rectification.
The yield of the refined methanol is 21.8 ten thousand tons/year after the operation for one year, the yield of the fusel oil product for export sales is about 15 tons, and the qualification rate of the refined methanol is about 98 percent.
Example 2
This example illustrates the reduction of fusel oil production in a crude methanol refining process according to the present invention.
The operation was carried out in the same manner as in example 1 except that the frequency of the first flooding was gradually adjusted from 10 times per month to 4 times per month, the frequency control of the second flooding was synchronized with the frequency control of the first flooding, and the total flooding amount was controlled to be 0.08 to 0.15 vol% based on the methanol production.
The yield of the refined methanol is 21.8 ten thousand tons/year after the operation for one year, the yield of the fusel oil product for export sales is about 30 tons, and the qualification rate of the refined methanol is about 98 percent.
Example 3
This example illustrates the reduction of fusel oil production in a crude methanol refining process according to the present invention.
The operation was carried out in the same manner as in example 1 except that the frequency of the first and second overflows was 10 times per month, and the overflows were synchronized, and the total overflow amount was controlled to be 0.1 to 0.2 vol% of the methanol production.
The yield of the refined methanol is 21.8 ten thousand tons/year after the operation for one year, the yield of the fusel oil product for export sales is about 50 tons, and the qualification rate of the refined methanol is about 98 percent.
Example 4
This example illustrates the reduction of fusel oil production in a crude methanol refining process according to the present invention.
The operation was carried out as described in example 1, except that the fusel oil feed was withdrawn from the atmospheric tower 4 times per month in an amount of 0.1 to 0.15% by volume based on the volume of the methanol-containing feed.
The yield of the refined methanol is 21.8 ten thousand tons/year after the operation for one year, the yield of the fusel oil product for export sales is about 18 tons, and the qualification rate of the refined methanol is about 98 percent.
Comparative example 1
This comparative example is presented to illustrate the method of reducing fusel oil production in a crude methanol refining process according to the present invention.
And (3) feeding the crude methanol into a pre-rectifying tower for pre-rectifying, extracting a first light component from the tower top, and extracting a bottom liquid of the pre-rectifying tower from the tower bottom. And conveying the bottom liquid of the pre-rectifying tower to a pressurized rectifying tower for pressurized rectification, conveying the bottom liquid of the pressurized rectifying tower to an atmospheric rectifying tower for atmospheric rectification, and collecting fusel oil materials at the side line of the atmospheric rectifying tower. Wherein the fusel oil is extracted for 1 time every day, and the amount of the fusel oil extracted from the lateral line every day is 0.2 volume percent of the volume of the feeding amount of the pre-rectifying tower.
Carrying out first condensation treatment on the first light component to obtain a second light component and a first condensate; carrying out second condensation treatment on the second light component to obtain non-condensable gas and second condensate; the non-condensable gas is directly incinerated. Wherein the temperature of the first condensation is 65 ℃ and the temperature of the second condensation is 45 ℃.
And carrying out first overflow on the first condensate in a pre-tower reflux tank to obtain a first overflow material, carrying out second overflow on the second condensate in a methanol analyzer to obtain a second overflow material, conveying the first overflow material, the second overflow material and the fusel oil material to a fusel oil storage tank, and carrying out first separation in the fusel oil storage tank to obtain a first recovery liquid and a first waste liquid.
Wherein the frequency of the first overflow and the second overflow is 1 time per day, the overflow is synchronous, and the total overflow amount is controlled to be 0.3-0.5 volume percent of the methanol yield. The volume ratio of the overflow quantity of the first overflow to the overflow quantity of the second overflow is about 1: 0.4.
wherein the first separation method comprises the following steps: when the material in the fusel oil storage tank reaches 60 volume percent of the volume of the fusel oil storage tank and no new material is input for 24 hours, the material in the fusel oil storage tank can be automatically layered, and the upper material (about 10 volume percent of the total volume of the material) and the bottom material (about 10 volume percent of the total volume of the material) are first waste liquid and are conveyed to a pollution discharge storage tank; the middle material is first recovery liquid and is conveyed to the collecting tank for temporary storage.
And carrying out second separation on the first waste liquid to obtain a second recovery liquid and a second waste liquid. Wherein the second separation method comprises: when the volume of the materials in the blowdown storage tank reaches 80% of the volume of the blowdown storage tank and no new materials are input for 24 hours, the materials in the fusel oil storage tank can be automatically layered, and the upper materials (about 10% of the total volume of the materials) and the bottom materials (about 10% of the total volume of the materials) are second waste liquid and are discharged as fusel oil products to be sold; and the middle material is a second recovery liquid and is conveyed to the collecting tank for temporary storage.
And refluxing the recovery liquid in the collecting tank to a pre-rectifying tower for pre-rectification.
The yield of the refined methanol is 21.8 ten thousand tons/year after the operation for one year, the yield of the fusel oil product for export sales is about 860 tons, and the qualification rate of the refined methanol is about 98 percent.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. A method for reducing fusel oil extraction in a crude methanol refining process is characterized by comprising the following steps: refining the crude methanol by adopting a three-tower rectification process, wherein,
(1) pre-rectifying crude methanol to obtain a first light component and a bottom liquid of a pre-rectifying tower, carrying out first condensation treatment on the first light component to obtain a second light component and a first condensate, carrying out second condensation treatment on the second light component to obtain non-condensable gas and a second condensate, carrying out third condensation treatment on the non-condensable gas to obtain a third condensate, and recycling the third condensate for pre-rectifying;
(2) the first condensate is subjected to first overflow to obtain a first overflow material, and the second condensate is subjected to second overflow to obtain a second overflow material; separating the first overflowing material and the second overflowing material to obtain waste liquid and recovery liquid; refluxing the recovery solution for the pre-rectification in the step (1);
wherein the temperature of the first condensation is 68-72 ℃, the temperature of the second condensation is 47-50 ℃, and the temperature of the third condensation is 25-35 ℃.
2. The method of claim 1, wherein the frequency of the first overflow is less than 10 times per month; and/or
The frequency of the second overflow is less than 10 times per month.
3. The method of claim 1 or 2, wherein the total overflow of the first overflow and the second overflow is 0.04-0.2 vol% of methanol production per month.
4. The method of any of claims 1-3, wherein the method further comprises: and (3) sequentially carrying out pressure rectification and normal pressure rectification on the bottom liquid of the pre-rectifying tower to obtain a fusel oil material, and separating the fusel oil material.
5. The method of claim 4, wherein the frequency of side draws is 2-4 times per month.
6. A process according to claim 4 or 5, wherein the fusel oil feed is withdrawn in an amount of 0.05 to 0.1% by volume, based on the volume of pre-rectification column feed, per month; preferably 0.05 to 0.08 volume%.
7. The method of any one of claims 1-6, wherein the method of separating comprises: performing first separation on the first overflow material and the second overflow material to obtain a first recovery liquid and a first waste liquid, and performing second separation on the first waste liquid to obtain a second recovery liquid and a second waste liquid; and (3) refluxing the first recovery liquid and the second recovery liquid for the pre-rectification in the step (1).
8. A system for reducing fusel oil extraction in a crude methanol refining process is characterized in that the system is a three-tower rectification system and comprises:
the pre-rectifying tower is used for carrying out pre-rectifying treatment on the crude methanol to obtain a first light component and a pre-rectifying tower bottom liquid;
the pre-tower top primary condenser is used for carrying out first condensation treatment on the first light component to obtain a second light component and first condensate;
the pre-tower top secondary condenser is used for carrying out secondary condensation treatment on the second light component to obtain non-condensable gas and second condensate;
the pre-tower reflux tank is used for performing first overflow on the first condensate to obtain a first overflow material;
the methanol analyzer is used for carrying out second overflow on the second condensate to obtain a second overflow material;
the separation unit is used for separating the first overflow material from the second overflow material to obtain waste liquid and recovery liquid;
the condensing device is used for carrying out third condensation treatment on the non-condensable gas to obtain third condensate;
the separation unit is communicated with the pre-rectifying tower through a pipeline and is used for refluxing the recovery liquid to the pre-rectifying tower for pre-rectification;
the condensing device is communicated with the pre-rectifying tower through a pipeline and is used for refluxing the third condensate to the pre-rectifying tower for pre-rectification.
9. The system of claim 8, wherein the system further comprises:
the pressurizing tower is used for performing pressurized rectification treatment on the bottom liquid of the pre-rectifying tower to obtain bottom liquid of the pressurizing tower and a product methanol at the top of the pressurizing tower;
the atmospheric tower is used for carrying out atmospheric rectification treatment on the tower bottom liquid from the pressurizing tower to obtain fusel oil materials and methanol products at the top of the atmospheric tower;
the normal pressure tower is connected with the separation unit through a pipeline and is used for separating the fusel oil material.
10. The system of claim 8 or 9, wherein the separation unit comprises:
the fusel oil storage tank is used for carrying out first separation on the first overflowing material and the second overflowing material to obtain a first recovery liquid and a first waste liquid; and
the blowdown storage tank is used for carrying out second separation on the first waste liquid to obtain a second recovery liquid and a second waste liquid;
and the fusel oil storage tank and/or the blowdown storage tank are/is connected with the pre-rectifying tower through a pipeline and used for refluxing the recovery liquid to the pre-rectifying tower for pre-rectification.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114949905A (en) * | 2022-06-17 | 2022-08-30 | 贵州天福化工有限责任公司 | Device and method for recovering methanol in methanol rectification non-condensable gas |
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| CN204815742U (en) * | 2015-07-29 | 2015-12-02 | 兖矿国宏化工有限责任公司 | Methyl alcohol rectifier unit |
| CN208883743U (en) * | 2018-06-06 | 2019-05-21 | 天津奥展兴达化工技术有限公司 | A kind of refining crude methanol process system of three towers triple effect |
| CN211863899U (en) * | 2019-07-19 | 2020-11-06 | 张兵 | Improved three-tower three-effect crude methanol refining process system |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN204815742U (en) * | 2015-07-29 | 2015-12-02 | 兖矿国宏化工有限责任公司 | Methyl alcohol rectifier unit |
| CN208883743U (en) * | 2018-06-06 | 2019-05-21 | 天津奥展兴达化工技术有限公司 | A kind of refining crude methanol process system of three towers triple effect |
| CN211863899U (en) * | 2019-07-19 | 2020-11-06 | 张兵 | Improved three-tower three-effect crude methanol refining process system |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114949905A (en) * | 2022-06-17 | 2022-08-30 | 贵州天福化工有限责任公司 | Device and method for recovering methanol in methanol rectification non-condensable gas |
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