CN216039342U - Continuous reaction device for preparing methyl formate by one-step oxidation of methanol - Google Patents
Continuous reaction device for preparing methyl formate by one-step oxidation of methanol Download PDFInfo
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- CN216039342U CN216039342U CN202120640852.2U CN202120640852U CN216039342U CN 216039342 U CN216039342 U CN 216039342U CN 202120640852 U CN202120640852 U CN 202120640852U CN 216039342 U CN216039342 U CN 216039342U
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Abstract
The utility model discloses a continuous reaction device for preparing methyl formate by one-step oxidation of methanol, which comprises a methanol buffer tank, a methanol feed pump, a methanol preheater, a methanol reaction kettle, a circulating compressor system, a condenser, a gas-liquid separation tank, a first stripping tank, a second stripping tank, a product fractionating tower, a tower top condenser, a product buffer tank, a methyl formate discharge pump and a wastewater pump, wherein the methanol feed pump is connected with the methanol preheater; according to the utility model, the two-stage gas stripping tank is arranged to extract the residual oxygen in the crude reaction product, so that the concentration range of the oxygen in the subsequent treatment is controlled below the lower explosion limit, the explosion risk can be avoided, the reaction can be continuously carried out, the long-period stable operation can be realized, and the method has good economic benefit; according to the utility model, the gas circulating compressor is arranged, and unreacted oxygen can be returned to the reactor for continuous cycle use after being pressurized by the circulating compressor, so that the material consumption and the energy consumption can be effectively reduced.
Description
Technical Field
The utility model relates to a continuous reaction device for preparing methyl formate by one-step oxidation of methanol, belonging to the technical field of organic synthesis.
Background
Methanol is an important chemical basic raw material and a clean liquid fuel, the methanol production capacity of China enters a high-speed development period from 2003, the yield of the methanol in China reaches 6216 ten thousand tons in 2019, the yield of the methanol is increased by 640 ten thousand tons in 2018, the yield is increased by 11.48% on year-to-year basis, and the methanol market tends to be saturated day by day along with the continuous arrival of methanol devices in China, so that the methanol conversion method has extremely important significance in realizing the efficient conversion of the methanol.
Methyl formate (hereinafter referred to as "MF") is an important organic synthesis intermediate, and downstream industries based on methyl formate are numerous, the product coverage is wide, and by 2016 years, the annual output of methyl formate industry in China is 49 million tons; the yield reaches 75 ten thousand tons in 2018. With the development of industrialization and urbanization in China and the improvement of the living standard of people, methyl formate is used as an important basic chemical raw material, the overall demand of methyl formate keeps a stable growth trend in the traditional downstream application, including the increase of social demands of medicines, pesticides and the like, and the demand of 2025 years is expected to reach 97 ten thousand tons, so that the methyl formate industry faces a wider development space in China.
The prior MF synthesis processes mainly comprise the following steps: (1) a formic acid esterification method; (2) a methanol carbonylation process; (3) a methanol dehydrogenation process; (4) a direct synthesis method of synthesis gas; (5) formaldehyde dimerization condensation method. Commonly used industrial production processes are methanol carbonylation and methanol dehydrogenation. In the methanol carbonylation method, the conversion rate of methanol is low and the equipment investment is high, while the catalyst of the methanol dehydrogenation method has short service life and poor economic benefit. The method for preparing MF by the methanol oxidation method has the advantages of mild synthesis conditions, high yield, low equipment investment, less three wastes in the product and the like, and is widely valued by people; however, the oxidation method adopted in the industry is a two-step operation, the production process is long, the process is complex, and the equipment investment is large, so that the development of a safe device and process for continuously preparing MF by the methanol one-step catalytic oxidation method has very important significance.
Disclosure of Invention
The technical problem to be solved by the utility model is as follows: in the prior art, a two-step oxidation method is adopted to prepare methyl formate, so that the problems of long production period, complex process, environmental pollution, high energy consumption and large equipment investment exist, and the problems of explosion risk, potential safety hazard and the like exist in the one-step oxidation preparation of methyl formate.
In order to solve the technical problem, the utility model provides a continuous reaction device for preparing methyl formate by one-step oxidation of methanol, which comprises a gas inlet system for providing synthesis gas for reaction, a feeding system for providing methanol raw material for reaction, a reaction system for reaction, a product separation system for product separation and purification and a collection system for collecting product and waste liquid;
the reaction system comprises a methanol reaction kettle (4) for methanol one-step oxidation, a first condenser (6) for condensing gas generated by the reaction and a gas-liquid separation tank (7) for separating the condensed gas from the liquid, wherein the gas obtained by the gas-liquid separation tank (7) is circulating gas, and the liquid is a crude product;
two or more than two gas stripping tanks are arranged between the reaction system and the product separation system and are used for extracting residual oxygen in the crude product so that the concentration range of the oxygen in the subsequent product separation and purification process is below the lower explosion limit.
Preferably, the gas inlet system comprises a gas supplementing system for supplementing fresh gas and a compressor circulating system (5), the circulating gas enters the compressor circulating system (5) for pressurization, and the fresh gas is depressurized by a pressure reducing valve and then enters the compressor circulating system (5) to be used as synthesis gas together with the circulating gas to enter the reaction system.
Preferably, the feed system comprises a methanol buffer tank (1) for storing methanol, a methanol preheater (3) and a methanol feed pump (2) for transporting methanol from the methanol buffer tank (1) to the methanol preheater (3) and the methanol reactor (4).
Preferably, the product separation system comprises a product fractionating tower (10) for rectifying the crude product, an overhead condenser (11) for condensing the gas phase components obtained from the rectification, and a product buffer tank (12) for storing the methyl formate product obtained after the condensation.
Preferably, the bottom of the product fractionating tower (10) is provided with a waste liquid outlet.
Preferably, the molar ratio of the synthetic gas in the air inlet system to the methanol in the air inlet system is 10-35: 1, and the synthetic gas is oxygen.
Preferably, the molar ratio of the synthesis gas in the air inlet system to the methanol in the air inlet system is 24-35: 1, so that the explosion limit of oxygen in the reaction and air inlet system can be avoided.
Preferably, the process conditions in the methanol reaction kettle (4) are as follows: the temperature is 100-250 ℃, the pressure is 0.1-1.5 MPa, and the liquid hourly space velocity of the methanol is 0.1-2.5 h-1The yield of the methyl formate is more than or equal to 90 percent, and the pressure is absolute pressure.
Preferably, the process conditions in the product fractionation column (10) are: the number of theoretical plates is 5-20, the operating temperature is 5-100 ℃, the operating pressure is 0.1MPa, and the reflux ratio is 0.5-2; the operating pressure is absolute pressure.
Compared with the prior art, the utility model has the beneficial effects that:
1. according to the continuous reaction device for preparing methyl formate through one-step oxidation of methanol, the two-stage gas stripping tank is arranged between the reaction system and the product separation system and is used for extracting residual oxygen in the reaction crude product, so that the concentration range of the oxygen in the subsequent product separation and purification process is below the lower explosion limit, the explosion risk can be avoided, the reaction can be continuously carried out, the long-period stable operation can be realized, and good economic benefits are achieved.
2. The continuous reaction device for preparing the methyl formate by oxidizing the methanol in one step is provided with the gas circulating compressor, and unreacted oxygen can be returned to the reactor for continuous recycling after being pressurized by the circulating compressor, so that the material consumption and the energy consumption can be effectively reduced.
Drawings
FIG. 1 is a schematic diagram of a continuous reaction apparatus for preparing methyl formate by one-step oxidation of methanol according to the present invention;
reference numerals: 1. a methanol buffer tank; 2. a methanol feed pump; 3. a methanol preheater; 4. a methanol reaction kettle; 5. a recycle compressor system; 6. a first condenser; 7. a gas-liquid separation tank; 8. a first stripping tank; 9. a second stripping tank; 10. a product fractionation column; 11. a tower top condenser; 12. a product buffer tank; 13. a methyl formate discharge pump; 14. a waste water pump.
Detailed Description
In order to make the utility model more comprehensible, preferred embodiments are described in detail below with reference to the accompanying drawings.
Examples
The embodiment provides a continuous reaction device for preparing methyl formate by one-step oxidation of methanol, which comprises an air inlet system for providing synthesis gas for reaction, a feeding system for providing methanol raw materials for reaction, a reaction system for reaction, a product separation system for product separation and purification and a collection system for collecting products and waste liquid, wherein the air inlet system is used for providing synthesis gas for reaction; in particular, the intake system comprises a gas make-up system for supplementing fresh oxygen and a recycle compressor system 5; the feeding system comprises a methanol buffer tank 1 for storing methanol, a methanol preheater 3 and a methanol feeding pump 2 for conveying the methanol from the methanol buffer tank 1 to the methanol preheater 3 and a methanol reaction kettle 4; the reaction system comprises a methanol reaction kettle 4 for methanol one-step oxidation, a first condenser 6 for condensing gas generated by the reaction and a gas-liquid separation tank 7 for separating gas from liquid after condensation, wherein the gas obtained by separation of the gas-liquid separation tank 7 is circulating gas, and the liquid is crude product; the product separation system comprises a product fractionating tower 10 for rectifying a crude product, a tower top condenser 11 for condensing a gas-phase product obtained by rectification and a product buffer tank 12 for storing a methyl formate product obtained after condensation, wherein a waste liquid outlet is formed in the bottom of the product fractionating tower 10; a first gas stripping tank 8 and a second gas stripping tank 9 are arranged between the reaction system and the product separation system and are used for extracting residual oxygen in the crude product so that the concentration range of the oxygen in the subsequent product separation and purification process is below the lower explosion limit; the collection system comprises a product storage tank for collecting products, a waste water treatment system for collecting waste liquid, a methyl formate discharge pump 13 for conveying methyl formate products from the product buffer tank 12 to the product storage tank, and a waste water pump 14 for conveying waste liquid obtained by rectifying the product fractionating tower 10 to the waste water treatment system.
During reaction, synthesis gas (oxygen) and methanol are respectively provided for the methanol reaction kettle 4 through an air inlet system and a feeding system, the molar ratio of the synthesis gas in the air inlet system to the methanol in the feeding system is set to be 24-35: 1, and the concentration range of the oxygen in the reaction system and the air inlet system can be below the lower explosion limit; the synthesis gas comprises fresh oxygen and circulating gas, the circulating gas is recycled in a methanol reaction kettle 4, a first condenser 6 and a gas-liquid separation tank 7 in the reaction system after being pressurized by a circulating compressor system 5, and the fresh O2The methanol is supplemented to a compressor circulating system 5 through a pressure control system and mixed with circulating gas, the mixture is fed into a methanol reaction kettle 4 to participate in reaction, the methanol is subjected to further oxidation reaction in the methanol reaction kettle 4 to generate methyl formate, the mixed gas obtained by the reaction is condensed by a first condenser 6, gas and liquid are separated in a gas-liquid separation tank 7, the separated gas is the circulating gas and fed into the compressor circulating system 5, the separated liquid (crude product) is subjected to gas stripping by nitrogen in a first gas stripping tank 8 and a second gas stripping tank 9 to extract oxygen remained in the crude product, the gas obtained by the gas stripping is fed into a waste gas treatment system, the concentration range of the oxygen can be below the lower explosion limit when the crude product subjected to the two-stage gas stripping treatment is fed into a product fractionating tower 10 for separation and purification so as to avoid explosion risks, a gas-phase product obtained by rectification in the product fractionating tower 10 is condensed by a tower top condenser 11 and then fed into a product buffer tank 12, the product buffer tank 12 is connected with the product storage tank through a methyl formate discharge pump 13; the liquid phase waste liquid obtained by rectification is introduced into a waste water treatment system from a waste liquid outlet at the bottom of the tower through a waste liquid pump 14.
The process conditions adopted in this example are as follows:
reaction temperature: the reaction pressure is 0.7MPa at 160 ℃;
reactor feed inlet conditions:
methanol feed flow rate: 15-70 mL/h;
o2 feed streamQuantity: 0.2 to 0.95Nm3Hour/hour;
effective volumetric loading of methanol reactor (4): 30-100 ml;
volume ratio of oxygen to methanol: 24:1
Discharging results at the discharging port:
conversion rate of methanol: 98 percent;
methyl formate selectivity: more than or equal to 97 percent;
in the embodiment, the production process of preparing methyl formate by one-step oxidation of methanol is realized by 98% of methanol conversion rate and more than or equal to 97% of selectivity of a main product.
The above-described embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way and substantially, it should be noted that those skilled in the art may make several modifications and additions without departing from the scope of the present invention, which should also be construed as a protection scope of the present invention.
Claims (6)
1. A continuous reaction device for preparing methyl formate by one-step oxidation of methanol is characterized by comprising a gas inlet system for providing synthesis gas for reaction, a feeding system for providing methanol raw material for reaction, a reaction system for reaction, a product separation system for product separation and purification and a collection system;
the reaction system comprises a methanol reaction kettle (4) for methanol one-step oxidation, a first condenser (6) for condensing gas generated by the reaction and a gas-liquid separation tank (7) for separating the condensed gas from the liquid, wherein the gas obtained by the gas-liquid separation tank (7) is circulating gas, and the liquid is a crude product;
two or more than two gas stripping tanks are arranged between the reaction system and the product separation system and are used for extracting residual oxygen in the crude product so that the concentration range of the oxygen in the subsequent product separation and purification process is below the lower explosion limit.
2. A continuous reaction unit for the one-step oxidation of methanol to methyl formate according to claim 1, wherein said gas inlet system comprises a gas make-up system for making up fresh gas and a compressor recycle system (5), and said recycle gas is pressurized by entering the compressor recycle system (5).
3. A continuous reaction unit for the one-step oxidation of methanol to methyl formate according to claim 1, characterized in that the feed system comprises a methanol buffer tank (1) for storing methanol, a methanol preheater (3) and a methanol feed pump (2) for transferring methanol from the methanol buffer tank (1) to the methanol preheater (3) and the methanol reactor (4).
4. A continuous reaction apparatus for the one-step oxidation of methanol to produce methyl formate according to claim 1, wherein said product separation system comprises a product fractionation column (10) for rectifying a crude product, an overhead condenser (11) for condensing a gas phase component obtained by the rectification, and a product surge tank (12) for storing a methyl formate product obtained after the condensation.
5. A continuous reaction unit for the one-step oxidation of methanol to methyl formate according to claim 4, characterized in that the bottom of said product fractionation column (10) is provided with a waste liquid outlet for discharging the liquid waste liquid obtained by rectification.
6. The continuous reaction device for preparing methyl formate by one-step oxidation of methanol according to claim 4, wherein the number of theoretical plates of the product fractionating tower (10) is 5-20.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112939777A (en) * | 2021-03-30 | 2021-06-11 | 上海簇睿低碳能源技术有限公司 | Continuous reaction device and process for preparing methyl formate through one-step oxidation of methanol |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112939777A (en) * | 2021-03-30 | 2021-06-11 | 上海簇睿低碳能源技术有限公司 | Continuous reaction device and process for preparing methyl formate through one-step oxidation of methanol |
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