CN212128029U - Formaldehyde pyridine hydrogen peroxide coproduction device - Google Patents
Formaldehyde pyridine hydrogen peroxide coproduction device Download PDFInfo
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- CN212128029U CN212128029U CN202020439035.6U CN202020439035U CN212128029U CN 212128029 U CN212128029 U CN 212128029U CN 202020439035 U CN202020439035 U CN 202020439035U CN 212128029 U CN212128029 U CN 212128029U
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Abstract
The utility model discloses a formaldehyde pyridine hydrogen peroxide solution coproduction device belongs to formaldehyde production field. The co-production device is composed of a methanol oxidation unit, a purification and separation unit, a pyridine production unit and a hydrogen peroxide production unit, wherein a formaldehyde mixed gas outlet of the methanol oxidation unit is connected with a material inlet of the purification and separation unit, a formaldehyde outlet of the purification and separation unit is connected with a formaldehyde inlet of the pyridine production unit, and a hydrogen outlet of the purification and separation unit is connected with a hydrogen inlet of the hydrogen peroxide production unit. Compared with the prior art, the utility model discloses a formaldehyde pyridine hydrogen peroxide solution coproduction device has overcome that current formaldehyde apparatus for producing investment is big, the technological process is long, hydrogen burning causes extravagant etc. not enough, can realize formaldehyde, pyridine and hydrogen peroxide solution coproduction, has fine popularization and application and worth.
Description
Technical Field
The utility model relates to a formaldehyde, pyridine, hydrogen peroxide solution production field specifically provides a formaldehyde pyridine hydrogen peroxide solution coproduction device.
Background
The formaldehyde, the pyridine and the hydrogen peroxide are chemical basic raw materials, and the application amount is large. In the prior art, a methanol oxidation method is mainly adopted for producing formaldehyde, and methanol, air and water are directly oxidized in an oxidizer to generate a mixed gas containing formaldehyde through catalysts such as silver, copper or vanadium pentoxide at 600-700 ℃. The mixed gas is then passed through first, second and third absorption towers, counter-current contacted with soft water and dilute formaldehyde solution, and progressively concentrated to obtain about 37% formaldehyde solution. The tail gas (containing 18% of hydrogen) is sent to a combustion boiler for incineration, and steam is produced as a byproduct. Not only the investment is large and the process flow is long, but also a great deal of hydrogen is wasted.
On the other hand, in the prior art, when pyridine is produced, the formaldehyde solution needs to be sent to the reactor to participate in the pyridine generation reaction through units such as pump pressurization, steam heating gasification, steam overheating temperature raising and the like, and the defects of low raw material utilization rate, low product purity, high energy consumption and the like exist.
Disclosure of Invention
The utility model provides a formaldehyde pyridine hydrogen peroxide coproduction device aiming at the defects of the prior art.
The utility model provides a technical scheme that its technical problem adopted is: the device comprises a methanol oxidation unit, a purification and separation unit, a pyridine production unit and a hydrogen peroxide production unit, wherein a formaldehyde mixed gas outlet of the methanol oxidation unit is connected with a material inlet of the purification and separation unit, a formaldehyde outlet of the purification and separation unit is connected with a formaldehyde inlet of the pyridine production unit, and a hydrogen outlet of the purification and separation unit is connected with a hydrogen inlet of the hydrogen peroxide production unit.
After the formaldehyde mixed gas obtained by the methanol oxidation unit is separated by the purification and separation unit, high-concentration formaldehyde gas (the volume percentage concentration is not lower than 98%) and high-concentration hydrogen gas (the volume percentage concentration is not lower than 99%) are obtained. Sending the formaldehyde gas to a pyridine production unit to produce pyridine; hydrogen is sent to a hydrogen peroxide production unit to produce hydrogen peroxide.
The purification and separation unit is used for separating and purifying the formaldehyde mixed gas to obtain high-concentration formaldehyde gas and hydrogen which can be used for producing pyridine and hydrogen peroxide. Preferably, the purification and separation unit comprises a compressor, a cooler, a gas-liquid separator, a membrane separator and a pressure swing adsorption purification assembly, wherein an air inlet of the compressor is connected with a formaldehyde mixed gas outlet pipeline of the methanol oxidation unit, an air outlet of the compressor is connected with the cooler and the gas-liquid separator in series through pipelines and then is connected with a feed inlet of the membrane separator, a hydrogen outlet (permeation gas outlet) of the membrane separator is connected with a hydrogen inlet of the hydrogen peroxide production unit, a tail gas outlet of the membrane separator is connected with an air inlet of the pressure swing adsorption purification assembly, and an air outlet of the pressure swing adsorption purification assembly is connected with a formaldehyde inlet pipeline.
After the formaldehyde mixed gas from the methanol oxidation unit is subjected to pressure raising, cooling and gas-liquid separation, the generated gas obtained by separation enters a membrane separator, hydrogen is subjected to permeation and concentration by utilizing the permeation selectivity of the membrane separation to obtain high-concentration hydrogen, and the tail gas obtained by the membrane separator enters a pressure swing adsorption purification assembly to be subjected to adsorption and removal of ineffective gas to obtain high-concentration formaldehyde gas.
In order to promote the recycling of heat energy, the purification and separation unit can also comprise a heat exchanger, a heat medium inlet of the heat exchanger is connected with an air outlet of the compressor, a heat medium outlet of the heat exchanger is connected with the cooler, a cold medium inlet of the heat exchanger is connected with an air outlet of the pressure swing adsorption purification assembly, and a cold medium outlet of the heat exchanger is connected with a formaldehyde inlet of the pyridine production unit. The formaldehyde gas pressurized by the compressor enters the cooler after passing through the heat exchanger, and the formaldehyde gas output by the pressure swing adsorption purification component is sent to the pyridine production unit after absorbing the heat of the formaldehyde gas through the heat exchanger.
In order to ensure the stability of hydrogen supply of the hydrogen peroxide production unit, the purification and separation unit also comprises a buffer tank, and a hydrogen outlet of the membrane separator is connected with a hydrogen inlet of the hydrogen peroxide production unit through the buffer tank. And the hydrogen output by the membrane separator is buffered by a buffer tank and then sent to a hydrogen peroxide production unit.
Preferably, the pressure swing adsorption purification assembly comprises a first-stage adsorption tank and a second-stage adsorption tank, wherein the first-stage adsorption tank is filled with a common carbon molecular sieve for adsorbing nitrogen, and the second-stage adsorption tank is filled with an MH-317 type efficient carbon molecular sieve for adsorbing carbon dioxide, carbon monoxide and methane.
The first-stage adsorption tank preferably consists of 5-8 adsorption tanks; the secondary adsorption tank preferably consists of 5 to 8 adsorption tanks.
Preferably, the methanol oxidation unit comprises an evaporator, a superheater, a filter and an oxidation reactor, wherein an air outlet of the evaporator is connected with the superheater and the filter in series through pipelines and then is connected with an air inlet of the oxidation reactor, a mixed gas outlet of the oxidation reactor is connected with an evaporator heat medium inlet, and an evaporator heat medium outlet is connected with the purification and separation unit. After passing through the evaporator, methanol and air pass through the superheater and the filter together with steam and enter the oxidation reactor for oxidative dehydrogenation reaction, and the formaldehyde mixed gas output by the oxidation reactor returns to the evaporator to release heat and cool and then is sent to the purification and separation unit.
Compared with the prior art, the utility model discloses a formaldehyde pyridine hydrogen peroxide solution coproduction device has following outstanding beneficial effect:
the defects of large investment, long process flow, waste caused by hydrogen combustion and the like of the existing formaldehyde production device are overcome, the formaldehyde gas can be used for producing pyridine by adding a membrane separation and pressure swing adsorption device, and the recovered hydrogen is used for producing hydrogen peroxide;
secondly, co-production of formaldehyde and hydrogen peroxide solves the problem of hydrogen peroxide project in areas without hydrogen sources;
the formaldehyde gas is directly cooled to the required reaction temperature for pyridine production, so that the equipment investment is saved, the steam consumption is reduced, and the operation cost is greatly reduced;
and fourthly, co-production of formaldehyde and pyridine is carried out, because the water content of formaldehyde gas is extremely low, the purity of the generated pyridine crude material is high, the rectification load is light, the byproduct wastewater is reduced, the steam consumption of a rectification tower is saved, and the investment and the operation cost of a thermal oxidation furnace of an environmental protection facility are reduced.
Drawings
FIG. 1 is a schematic structural diagram of a formaldehyde, pyridine and hydrogen peroxide co-production device in an embodiment;
FIG. 2 is a schematic diagram of the structure of a methanol oxidation unit of an embodiment;
FIG. 3 is a schematic structural diagram of a purification and separation unit of an embodiment;
FIG. 4 is a schematic diagram of the unit structure for pyridine production in accordance with an embodiment;
FIG. 5 is a schematic diagram of a hydrogen peroxide production unit according to an embodiment.
The reference numerals in the drawings denote:
1. methanol evaporator, 2, superheater, 3, filter, 4, oxidation reactor, 5, compressor, 6, heat exchanger, 7, cooler, 8, gas-liquid separator, 9, membrane separator, 10, buffer tank, 11, pressure swing adsorption purification component, 12.1, fluidized bed reactor, 12.2, regenerator, 12.3, crude material stripper, 12.4, ammonia absorption tower, 12.5, ammonia stripper, 12.6, extraction tower, 12.7, benzene stripper, 12.8, rectification component, 12.81, rectification tower, 12.82, rectification tower, 12.83, finished product rectification tower, 12.9, crude material storage tank, 13.1, hydrogenation tower, 13.2, oxidation tower, 13.3, separator, 13.4, extraction tower, 13.5, purifier, 13.6, hydrogenation liquid-gas-liquid separation and hydrogenation liquid regeneration coalescence bed, 13.7, vacuum separator, 13.8, vacuum separator, 13.9, 13.4, extraction tower, 13.5, working liquid storage tank, 13.6, hydrogenation liquid preheater, 13.7, 13.8, working liquid storage tank, 13.9, 13.10.9, 13.10.13.13.10, 13.6, 13.7, 13.13, a hydrogenated liquid cooler, 13.14, a centrifugal air compressor, 13.15 and an oxidizing liquid storage tank.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and specific examples, which are not intended to limit the present invention.
Example (b):
[ Main Equipment ]
As shown in attached figure 1, the device for co-producing formaldehyde, pyridine and hydrogen peroxide comprises a methanol oxidation unit, a purification and separation unit, a pyridine production unit and a hydrogen peroxide production unit. The formaldehyde mixed gas outlet of the methanol oxidation unit is connected with the material inlet of the purification and separation unit, the formaldehyde outlet of the purification and separation unit is connected with the formaldehyde inlet of the pyridine production unit, and the hydrogen outlet of the purification and separation unit is connected with the hydrogen inlet of the hydrogen peroxide production unit.
As shown in fig. 2, the methanol oxidation unit mainly comprises a methanol evaporator 1, a superheater 2, a filter 3 and an oxidation reactor 4. The air outlet of the evaporator 1 is connected with the air inlet of the oxidation reactor 4 after being connected with the superheater 2 and the filter 3 in series through pipelines. The mixed gas outlet of the oxidation reactor 4 is connected with the heat medium inlet of the methanol evaporator 1. The outlet of the heat medium of the methanol evaporator 1 is connected with the air inlet of a purification and separation unit compressor 5.
As shown in fig. 3, the purification and separation unit is composed of a compressor 5, a heat exchanger 6, a cooler 7, a gas-liquid separator 8, a membrane separator 9, a buffer tank 10, and a pressure swing adsorption purification unit 11.
The compressor 5 is connected with the heat exchanger 6, the cooler 7 and the gas-liquid separator 8 in series, and a gas outlet of the gas-liquid separator 8 is connected with a feed inlet of the membrane separator 9. The hydrogen outlet of the membrane separator 9 is connected with a hydrogenation tower 13.1 of a hydrogen peroxide production unit through a buffer tank 10. The tail gas outlet of the membrane separator 9 is connected with the gas inlet of the pressure swing adsorption purification component 11. The air outlet of the pressure swing adsorption purification component 11 is connected with the cold medium inlet of the heat exchanger 6. The cold medium outlet of the heat exchanger 6 is connected to the fluidized bed reactor 12.1 of the pyridine production unit.
The membrane separator 9 adopts a hollow fiber membrane, such as a H _2/N _2 separation and hydrogen recovery device of large connected substances.
The pressure swing adsorption purification component adopts two-stage pressure swing adsorption. The first-stage pressure swing adsorption adopts six tanks filled with common carbon molecular sieves; the two-stage pressure swing adsorption adopts six tanks filled with MH-317 type high-efficiency carbon molecular sieves.
As shown in fig. 4, the pyridine production unit mainly comprises a fluidized bed reactor 12.1, a regenerator 12.2, a crude material stripper 12.3, an ammonia absorption tower 12.4, an ammonia stripper 12.5, an extraction tower 12.6, a benzene stripper 12.7 and a rectification component 12.8, and the structure and the pipeline connection of the pyridine production unit are in the prior art.
As shown in the attached figure 5, the hydrogen peroxide production unit mainly comprises a hydrogenation tower 13.1, an oxidation tower 13.2, a separator 13.3, an extraction tower 13.4, a purifier 13.5, a hydrogenation liquid gas-liquid separation and hydrogenation liquid regeneration bed 13.6, a coalescence separator 13.7, a vacuum dehydrator 13.8 and a drying tower 13.9, and the structure and pipeline connection of the hydrogen peroxide production unit are the prior art.
[ Process flow ]
Unless otherwise specified, the concentrations in the process flow are mass percent concentrations.
(I) methanol oxidation unit
Methanol is pressurized from a methanol metering tank through a methanol pump, the flow rate of the methanol is controlled by an adjusting valve, and then the methanol enters the bottom of the methanol evaporator 1 and is indirectly heated through reaction gas (formaldehyde mixed gas). The methanol in the methanol evaporator 1 is mixed with a certain amount of air sent by the Roots blower to form binary mixed gas, and a certain amount of saturated water vapor is added to form ternary mixed gas. The ternary mixed gas is sent into a superheater 2, is indirectly heated by steam, is sent into an oxidation reactor 4 filled with a catalyst through a flame retardant device and a filter 3 from top to bottom, passes through a catalyst layer from top to bottom, and is subjected to oxidation and dehydrogenation reactions of methanol at the high temperature of 640 ℃, the generated formaldehyde mixed gas quickly passes through a quenching section of the oxidation reactor 4 to heat soft water, and 0.4Mpa steam is byproduct. The cooled formaldehyde mixed gas is indirectly heated by the formaldehyde evaporator 1 and then sent to the purification and recovery unit.
(2) Purification and recovery unit
The formaldehyde mixed gas from the formaldehyde device is pressurized to 2.0Mpa by a compressor 5, then exchanges heat with the formaldehyde gas output by a pressure swing adsorption purification component 11 by a heat exchanger 5, and enters a separator 8 after being cooled by a cooler 7. Gas-liquid separation is performed in the separator 8. The separated condensed water contains a small amount of formaldehyde which can be recycled. The separated generated gas enters a membrane separator 9, hydrogen in the generated gas is subjected to permeation and concentration through the permeation selectivity of membrane separation to obtain 99.5% high-concentration hydrogen with the pressure of 0.5MPa, and the hydrogen is sent to a hydrogen peroxide production unit 13 through a buffer tank 10 to react.
The 2.0MPa tail gas passing through the membrane separator 9 enters a pressure swing adsorption purification component 11, is subjected to two-stage pressure swing adsorption under 2.0MPa to adsorb nitrogen and other ineffective gases in the tail gas, finally obtains 98% high-concentration formaldehyde gas, and is sent to a pyridine production unit after heat exchange and temperature increase by a heat exchanger 6.
In two-stage pressure swing adsorption, one-stage pressure swing adsorption is used for adsorbing nitrogen. Other mixed gas enters a secondary pressure swing adsorption stage to be used for adsorbing and removing carbon dioxide, carbon monoxide and methane.
(3) Pyridine production unit
Pressurizing acetaldehyde to 0.6MPa by a pump, filtering, gasifying, mixing with formaldehyde gas from a purification and recovery unit, heating, feeding into the middle part of a fluidized bed reactor 12.1, gasifying and heating liquid ammonia, feeding from the bottom of the reactor 12.1, and reacting formaldehyde, acetaldehyde and ammonia gas on the surface of a catalyst in the fluidized bed reactor to generate crude material gas.
The crude material gas enters a crude material tower 12.3 for absorption, the absorbed crude material enters a crude material storage tank 12.9, and the unabsorbed gas phase sequentially enters an ammonia absorption tower 12.4 and an ammonia stripping tower 12.5 for ammonia recovery. The recovered ammonia is returned to the fluidized bed reactor 12.1 for reuse.
The crude material in the crude material storage tank 12.9 is pumped into the extraction column 12.6. The extraction column 12.6 separates pyridine, picoline and other by-products from the aqueous solution. The extract enters a benzene stripping tower 12.7 for separation of an extracting agent, pyridine and the like. The extractant is recycled, and the separated pyridine and the byproducts thereof enter a rectification component 12.8 (composed of a rectification tower 12.81, a rectification tower 12.82 and a finished product rectification tower 12.83) for product separation and refining. 99.9% of finished pyridine and 99% of finished 3-methylpyridine are obtained.
(4) Hydrogen peroxide production unit
The working fluid from the working fluid tank 13.10 is heated by the working fluid preheater 13.11, and then enters the hydrogenation tower 13.1 together with the high-concentration hydrogen gas of 0.5MPa and 99.5% from the purification and recovery unit. The working solution and hydrogen flow into the top of the upper tower to be mixed, flow downward and perform hydrogenation reaction through the catalyst layers of the upper tower and the lower tower to obtain hydrogenated liquid, then enter a hydrogenated liquid gas-liquid separation and hydrogenated liquid regeneration bed 13.6 to perform gas-liquid separation and regeneration, and then enter a hydrogenated liquid storage tank 13.12 after passing through a filter. The hydrogenated liquid in the hydrogenated liquid storage tank 13.12 is cooled by passing through the hydrogenated liquid cooler 13.13 by means of a hydrogenated liquid pump, and enters the oxidation tower 13.2 together with air sent by the centrifugal air compressor 13.14, and is oxidized. The oxidized liquid after oxidation passes through a separator 13.3 and then enters an oxidized liquid storage tank 13.15. Pumping the oxidizing solution into the bottom of an extraction tower 13.4 by an oxidizing solution pump to extract hydrogen peroxide, and extracting the oxidizing solution containing hydrogen peroxide by pure water to obtain crude hydrogen peroxide containing hydrogen peroxide. The raffinate flowing out from the top of the extraction tower 13.4 is sent to a circulating working solution storage tank 13.10 after passing through a raffinate coalescence separator 13.7, a vacuum dehydrator 13.8 and a drying tower 13.9. The crude hydrogen peroxide obtained by extraction flows out from the bottom of the extraction tower 13.4, and is purified by a purification tower 13.5 to obtain the hydrogen peroxide product with the mass percentage concentration of 27.5%.
The above-mentioned embodiments are only preferred embodiments of the present invention, and the ordinary changes and substitutions performed by those skilled in the art within the technical scope of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. Formaldehyde pyridine hydrogen peroxide coproduction device which characterized in that: comprises a methanol oxidation unit, a purification and separation unit, a pyridine production unit and a hydrogen peroxide production unit,
the formaldehyde mixed gas outlet of the methanol oxidation unit is connected with the material inlet of the purification and separation unit, the formaldehyde outlet of the purification and separation unit is connected with the formaldehyde inlet of the pyridine production unit, and the hydrogen outlet of the purification and separation unit is connected with the hydrogen inlet of the hydrogen peroxide production unit.
2. The formaldehyde, pyridine and hydrogen peroxide co-production device as claimed in claim 1, wherein: the purification and separation unit comprises a compressor, a cooler, a gas-liquid separator, a membrane separator and a pressure swing adsorption purification assembly, wherein an air inlet of the compressor is connected with a formaldehyde mixed gas outlet pipeline of the methanol oxidation unit, an air outlet of the compressor is connected with a feed inlet of the membrane separator after being connected in series with the cooler and the gas-liquid separator through pipelines, a hydrogen outlet of the membrane separator is connected with a hydrogen inlet of the hydrogen peroxide production unit, a tail gas outlet of the membrane separator is connected with an air inlet of the pressure swing adsorption purification assembly, and an air outlet of the pressure swing adsorption purification assembly is connected with a formaldehyde inlet pipeline.
3. The formaldehyde, pyridine and hydrogen peroxide co-production device as claimed in claim 2, wherein: the purification and separation unit also comprises a heat exchanger, a heat medium inlet of the heat exchanger is connected with an air outlet of the compressor, a heat medium outlet is connected with the cooler, a cold medium inlet is connected with an air outlet of the pressure swing adsorption purification assembly, and a cold medium outlet is connected with a formaldehyde inlet of the pyridine production unit.
4. The formaldehyde, pyridine and hydrogen peroxide co-production device as claimed in claim 2 or 3, wherein: the purification and separation unit also comprises a buffer tank, and a hydrogen outlet of the membrane separator is connected with a hydrogen inlet of the hydrogen peroxide production unit through the buffer tank.
5. The formaldehyde, pyridine and hydrogen peroxide co-production device as claimed in claim 2 or 3, wherein: the pressure swing adsorption purification assembly comprises a first-stage adsorption tank and a second-stage adsorption tank, wherein the first-stage adsorption tank is filled with a common carbon molecular sieve, and the second-stage adsorption tank is filled with an MH-317 type high-efficiency carbon molecular sieve.
6. The formaldehyde, pyridine and hydrogen peroxide co-production device as claimed in claim 5, wherein: the first-stage adsorption tank consists of 5-8 adsorption tanks; the second-stage adsorption tank consists of 5-8 adsorption tanks.
7. The formaldehyde, pyridine and hydrogen peroxide co-production device as claimed in claim 1, wherein: the methanol oxidation unit comprises an evaporator, a superheater, a filter and an oxidation reactor, wherein an air outlet of the evaporator is connected with the superheater and the filter in series through pipelines and then is connected with an air inlet of the oxidation reactor, a mixed gas outlet of the oxidation reactor is connected with an evaporator heat medium inlet, and an evaporator heat medium outlet is connected with the purification and separation unit.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115784855A (en) * | 2022-12-15 | 2023-03-14 | 山东明化新材料有限公司 | Novel process for coproducing acetaldehyde and pyridine and simplifying flow |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115784855A (en) * | 2022-12-15 | 2023-03-14 | 山东明化新材料有限公司 | Novel process for coproducing acetaldehyde and pyridine and simplifying flow |
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