CN213085852U - Production device of poly 2-hydroxy acrylic acid - Google Patents
Production device of poly 2-hydroxy acrylic acid Download PDFInfo
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- CN213085852U CN213085852U CN202021041486.0U CN202021041486U CN213085852U CN 213085852 U CN213085852 U CN 213085852U CN 202021041486 U CN202021041486 U CN 202021041486U CN 213085852 U CN213085852 U CN 213085852U
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Abstract
The utility model provides a gather 2-hydroxyacrylic acid's apparatus for producing mainly includes: a mixing kettle, a tubular reactor, an external steaming kettle, a pyruvic acid transfer tank, an ethanol transfer tank and a catalyst module. The device of the utility model adopts pyruvic acid as the main production raw material, the whole reaction process is mild and stable, and the safety factor is high; the device can continuously produce the poly 2-hydroxy acrylic acid; the solvent and unreacted raw materials used by the device can be recycled, the cost is reduced, no waste acid is generated, and the device is green and environment-friendly.
Description
Technical Field
The utility model relates to a chemical industry equipment technical field, in particular to gather apparatus for producing of 2-hydroxyacrylic acid.
Background
Poly 2-hydroxy acrylic acid is used as a novel important industrial raw material, is widely applied to industries such as paper making industry, coating, graphite, dyeing auxiliary agents and the like, has excellent chemical characteristics due to structural hydroxy and carboxyl groups, and can be used for preparing auxiliary agents such as chelating agents, plasticizers, coupling agents and the like.
Japanese patent CN1260270C proposes a method for preparing an aqueous solution of poly-alpha-hydroxyacrylate. In particular, a polylactone compound of poly-alpha-hydroxy acrylic acid and alkali are subjected to hydrolysis reaction to generate a poly-alpha-hydroxy acrylic acid salt aqueous solution. The method does not involve monomer synthesis and cannot meet the requirement of industrial production. DE2061584 proposes a process for obtaining poly-alpha-hydroxyacrylic acids by polymerization of monomeric alpha-haloacrylic acids in the presence of organic solvents and free-radically active catalysts. The alpha-halogenated acrylic acid for polymerization by the method is difficult to exist in a pure form, the dihalopropionic acid is usually used for reaction, the dihalopropionic acid is expensive, a large amount of halogen simple substances are consumed in the self-manufacturing process, a large amount of acid is generated, the process danger coefficient is large, the environmental protection cost is high, the requirement on the strength of a corresponding production device is high, and the industrial popularization is not facilitated.
Aiming at the defects of the problems, the invention provides a device for continuously producing poly 2-hydroxy acrylic acid by using acrylic acid as a monomer.
Disclosure of Invention
The utility model provides a poly 2-hydroxyacrylic acid's apparatus for producing realizes using pyruvic acid as the raw materials, realizes serialization production under the alkaline catalyst condition.
The utility model adopts the technical proposal that:
the invention has the beneficial effects that:
an apparatus for producing poly-2-hydroxyacrylic acid, comprising: a mixing kettle, a tubular reactor, an external steaming kettle, a pyruvic acid transfer tank and an ethanol transfer tank;
the upper end of the mixing kettle is provided with an ethanol inlet and a pyruvic acid inlet, the lower end of the mixing kettle is provided with a discharge hole of the mixing kettle, and the outer wall of the mixing kettle is provided with a first shell-and-tube type constant temperature heat exchanger;
the tubular reactor comprises a reactor feed inlet and a reactor discharge outlet, a second shell-and-tube type constant temperature heat exchanger is arranged on the outer wall of the tubular reactor, the reactor feed inlet is connected with the discharge outlet of the mixing kettle, a catalyst module is arranged in the tubular reactor, and the catalyst module is tightly combined with a tubular reactor pipeline in an embedded mode;
the outer steaming kettle is at least one group, an outer steaming kettle feed port, an outer steaming kettle gas outlet and an outer steaming kettle water inlet are arranged at the upper end of the outer steaming kettle, an outer steaming kettle discharge port is arranged at the lower end of the outer steaming kettle, a third shell-and-tube type constant temperature heat exchanger is arranged on the outer wall of the outer steaming kettle, the outer steaming kettle feed port is connected with a reactor discharge port through a pipeline, the outer steaming kettle water inlet is connected with a pure water pipeline, and the outer steaming kettle discharge port is connected with;
the pyruvic acid transfer tank is provided with an pyruvic acid transfer tank outer steaming inlet, a pyruvic acid transfer tank discharge port and a pyruvic acid transfer tank feed inlet, the pyruvic acid transfer tank outer steaming inlet is connected with an outer steaming kettle gas outlet of the outer steaming kettle through a pipeline, the pyruvic acid transfer tank discharge port is connected with a mixing kettle pyruvic acid inlet through a pipeline, and the pyruvic acid transfer tank feed inlet is connected with a pyruvic acid storage tank;
the device comprises an ethanol transfer tank, an ethanol mixing kettle, an ethanol transfer tank, an absolute ethanol storage tank and a water tank, wherein the ethanol transfer tank is provided with an ethanol transfer tank outer steaming inlet, an ethanol transfer tank discharge port and an ethanol transfer tank feed port, the ethanol transfer tank outer steaming inlet is connected with an outer steaming kettle gas outlet of the outer steaming kettle through a pipeline, the ethanol transfer tank discharge port is connected with a mixing kettle ethanol inlet through a pipeline, and the.
Preferably, the tubular reactor is made of graphite, the inner wall of the tube has a diameter of 10-20 cm and a total length of 50-150 m.
Preferably, the catalyst module is formed by sequentially combining a sodium alkoxide catalyst component and a metallocene catalyst component, the two components in each module are sequentially and alternately arranged for 3-5 groups, the components are of a leakage net-shaped structure, the cross section of each component is equivalent to the cross section of the pipe diameter of the tubular reactor, and the thickness of each component is 1-2 cm.
Preferably, the carrier material of the sodium alkoxide component is mesoporous molecular sieve SBA-15, and the catalyst main body is solid sodium methoxide and sodium hydroxide, and is physically fixed with the carrier material.
Preferably, the carrier material of the metallocene catalyst component is mesoporous molecular sieve SBA-15, the main catalyst is fixedly connected with the carrier material through a cocatalyst, the central metal of the main catalyst is one of iron, titanium and zirconium, and the cocatalyst can be alkylaluminoxane.
Preferably, the water inlet of the first heat exchanger is connected with a hot water inlet pipeline and is connected with a valve and a circulating pump in series, the water outlet of the first heat exchanger is connected with a hot water return pipeline and is connected with the valve in series, the steam inlets at the upper ends of the other shell-and-tube type constant temperature heat exchangers are connected with a steam supply pipeline and are connected with the valve in series, and the steam outlets at the lower ends of the shell-and-tube type constant temperature heat exchangers are connected with a steam return pipeline and are connected with the valve in series.
Preferably, a valve, a material beating pump and an electronic flow meter are connected in series on pipelines connected with the reactor feed inlet and the material mixing kettle discharge outlet, the outer steaming kettle water inlet and a pure water pipeline, the pyruvic acid transfer tank discharge outlet and a pyruvic acid inlet of the material mixing kettle, and the ethanol transfer tank discharge outlet and an ethanol inlet of the material mixing kettle, a valve, a diaphragm pump and an electronic flow meter are connected in series on a pipeline connected with the tubular reactor discharge outlet and the outer steaming kettle feed inlet, a valve and a negative pressure pump are connected in series on a pipeline connected in parallel with the pyruvic acid transfer tank and the ethanol transfer tank at the outer steaming kettle gas outlet, and the rest pipelines are connected in series with valves.
Preferably, the external steaming kettles are connected with the tanks in parallel when the number of the external steaming kettles is more than two.
The device of the utility model adopts pyruvic acid as the main production raw material, the whole reaction process is mild and stable, and the safety factor is high; the device can continuously produce the poly 2-hydroxy acrylic acid; the solvent and unreacted raw materials used by the device can be recycled, the cost is reduced, no waste acid is generated, and the device is green and environment-friendly.
Drawings
FIG. 1 is a schematic view of the structure of the present invention.
FIG. 2 is a cross-sectional view of a tubular reactor tube and catalyst module.
Reference numerals: 1. a mixing kettle, 101, an ethanol inlet, 102, an pyruvic acid inlet, 103 a discharge hole, 2, a tubular reactor, 201, a reactor feed inlet, 202, a reactor discharge hole, 3, an external steaming kettle, 301, an external steaming kettle feed inlet, 302, an air outlet, 303, a water inlet, 304, an external steaming kettle discharge hole, 4, an pyruvic acid transfer tank, 401 an pyruvic acid transfer tank external steaming material inlet, 402, an pyruvic acid transfer tank discharge hole, 403, an pyruvic acid transfer tank feed inlet, 5, an ethanol transfer tank, 501 an ethanol transfer tank external steaming material inlet, 502, an ethanol transfer tank discharge hole, 503, an ethanol transfer tank feed inlet, 6, a first shell-and-tube type constant temperature heat exchanger, 601, a first heat exchanger water inlet, 802, a first heat exchanger water outlet, 7, a second shell-and-tube type constant temperature heat exchanger, 701, a second heat exchanger steam inlet, 702, a second heat exchanger steam outlet, 8 and a third shell-and-tube type constant temperature heat, 801. a third heat exchanger steam inlet, 802, a third heat exchanger steam outlet, 9 and a catalyst module.
Detailed Description
The invention will be further described with reference to the following description of specific embodiments and the accompanying drawings.
The production device of poly 2-hydroxy acrylic acid has a structure shown in figure 1, and comprises a mixing kettle 1, a tubular reactor 2, an external steaming kettle 3, a pyruvic acid transfer tank 4 and an ethanol transfer tank 5;
the upper end of the mixing kettle is provided with an ethanol inlet 101 and a pyruvic acid inlet 102, the lower end of the mixing kettle is provided with a mixing kettle discharge hole 103, and the outer wall of the mixing kettle is provided with a first shell-and-tube type constant temperature heat exchanger 6;
the tubular reactor comprises a reactor feed inlet port 201 and a reactor discharge port 202, a second shell-and-tube type constant temperature heat exchanger 7 is arranged on the outer wall of the tubular reactor, the reactor feed inlet port 201 is connected with the discharge port 103 of the mixing kettle, a catalyst module is arranged in the tubular reactor, and the catalyst module is tightly combined with a pipeline of the tubular reactor in an embedded mode;
outer steaming still is a set of at least, evaporates the cauldron upper end outward and is equipped with outer steaming still feed inlet 301, outer steaming still gas outlet 302 and outer steaming still water inlet 303, and the lower extreme is equipped with outer steaming still discharge gate 304, and the outer wall is equipped with third shell and tube formula constant temperature heat exchanger 8, outer steaming still feed inlet 301 passes through the pipeline connection with reactor discharge gate 202, outer steaming still water inlet 303 connects the pure water pipeline, outer steaming still discharge gate 304 connects the finished product storage tank. When the number of the outer steaming kettles is more than two, the material inlet and the material outlet of each outer steaming kettle are connected with the corresponding tank body in parallel through pipelines.
The pyruvic acid transfer tank is provided with an pyruvic acid transfer tank outer steaming material inlet 401, a pyruvic acid transfer tank discharge port 402 and a pyruvic acid transfer tank feed inlet 403, the pyruvic acid transfer tank outer steaming material inlet 401 is connected with the outer steaming kettle gas outlet 302 through a pipeline, the pyruvic acid transfer tank discharge port 402 is connected with the mixing kettle pyruvic acid inlet 102 through a pipeline, and the pyruvic acid transfer tank feed inlet 403 is connected with a pyruvic acid storage tank;
the ethanol transfer tank is provided with an ethanol transfer tank outer steaming material inlet 501, an ethanol transfer tank discharge port 502 and an ethanol transfer tank feed inlet 503, the ethanol transfer tank outer steaming material inlet 501 is connected with the outer steaming kettle gas outlet 302 through a pipeline, the ethanol transfer tank discharge port 502 is connected with the mixing kettle ethanol inlet 101 through a pipeline, and the ethanol transfer tank feed inlet 503 is connected with an absolute ethanol storage tank.
A water inlet 701 of the first heat exchanger is connected with a hot water inlet pipeline and is connected with a valve and a circulating pump in series, a water outlet 702 of the first heat exchanger is connected with a hot water return pipeline and is connected with the valve in series, steam inlets at the upper ends of other shell-and-tube type constant temperature heat exchangers are connected with a steam supply pipeline and are connected with the valve in series, and a steam outlet at the lower end is connected with a steam return pipeline and is connected with the valve in series.
The pipeline connecting the reactor feed inlet and the mixing kettle discharge port, the outer steaming kettle water inlet and the pure water pipeline, the pyruvic acid transfer tank discharge port and the pyruvic acid inlet of the mixing kettle, and the ethanol transfer tank discharge port and the ethanol inlet of the mixing kettle are all connected in series with a valve, a material beating pump and an electronic flow meter, the pipeline connecting the tubular reactor discharge port and the outer steaming kettle feed inlet is connected in series with a valve, a diaphragm pump and an electronic flow meter, the pipeline connecting the outer steaming kettle gas outlet and the pyruvic acid transfer tank and the ethanol transfer tank in parallel is connected in series with a valve and a negative pressure pump, and the rest of the pipelines are all connected in series with valves.
The tubular reactor is made of graphite, the diameter of the inner wall of the tube is 10-20 cm, the total length is 50-150 m, and 100-150m is preferred. The catalyst module structure is shown in figure 2 and is formed by sequentially combining two parts of a sodium alkoxide catalyst component and a metallocene catalyst component, wherein 3-5 groups of the two components are sequentially alternated in each module, the components are of a leakage net-shaped structure, the cross section of each component is equivalent to the cross section of the pipe diameter of the tubular reactor, and the thickness of each component is 1-2 cm.
The carrier material of the sodium alkoxide component is mesoporous molecular sieve SBA-15, the main body of the catalyst is sodium methoxide and sodium hydroxide solid, and the sodium methoxide and sodium hydroxide solid are fixed with the carrier material in a physical mode.
The carrier material of the metallocene catalyst component is mesoporous molecular sieve SBA-15, the main catalyst is fixedly connected with the carrier material through a cocatalyst, the central metal of the main catalyst is one of iron, titanium and zirconium, and the cocatalyst can be alkyl aluminoxane.
When the device is used for carrying out continuous production of poly 2-hydroxyacrylic acid, the operation process of each device is as follows:
the method comprises the following steps: pumping into a mixing kettle at a constant speed according to the flow of 177kg/h pyruvic acid and 18kg/h absolute ethyl alcohol, simultaneously starting stirring, controlling the temperature in the kettle to be 76 +/-2 ℃ through a first shell-and-tube type constant temperature heat exchanger, mixing the reaction materials for 1h, pumping into a tubular reactor at a constant speed through a discharge port of the mixing kettle according to the flow of 195L/h through a feed port, heating through water vapor by a second shell-and-tube type constant temperature heat exchanger, and controlling the boiling state in the tubular reactor.
Step two: after 4.03h, the reaction liquid begins to flow out of the tubular reactor, the reaction liquid is injected into an external steaming kettle after being filtered, the filtrate is collected for 5h, the ethanol is separated by distillation under the pressure of-0.05 MPa and then enters an ethanol transfer tank, the pressure is continuously reduced to-0.1 MPa, the pyruvic acid is separated by distillation and enters a pyruvic acid transfer tank, and 2467kg of poly 2-hydroxyacrylic acid aqueous solution with the mass fraction of 25.0 percent is obtained after the rest components are diluted by adding 1850kg of pure water.
Step three: and the ethanol and the pyruvic acid separated by distillation are recycled by repeating the second step, and the continuity is realized by repeating the second step by using the parallel outer steaming kettles in the outer steaming process.
Wherein the primary conversion rate of pyruvic acid is 71.2%, the chroma of the poly 2-hydroxy acrylic acid aqueous solution is 14, the average molecular weight is 2198, and the viscosity is 207.
The above-mentioned embodiments only express the embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for those skilled in the art, without departing from the spirit of the present invention, several variations and modifications can be made, which are within the scope of the present invention.
Claims (8)
1. A production device of poly 2-hydroxy acrylic acid is characterized by comprising: a mixing kettle (1), a tubular reactor (2), an external steaming kettle (3), a pyruvic acid transfer tank (4) and an ethanol transfer tank (5);
the upper end of the mixing kettle is provided with an ethanol inlet (101) and an pyruvic acid inlet (102), the lower end of the mixing kettle is provided with a mixing kettle discharge hole (103), and the outer wall of the mixing kettle is provided with a first shell-and-tube type constant temperature heat exchanger (6);
the tubular reactor comprises a reactor feeding hole (201) and a reactor discharging hole (202), a second shell-and-tube type constant temperature heat exchanger (7) is arranged on the outer wall of the tubular reactor, the reactor feeding hole (201) is connected with a mixing kettle discharging hole (103), a catalyst module is arranged in the tubular reactor, and the catalyst module is tightly combined with a tubular reactor pipeline in an embedded mode;
the device comprises at least one group of outer steaming kettles, wherein the upper ends of the outer steaming kettles are provided with an outer steaming kettle feed inlet (301), an outer steaming kettle gas outlet (302) and an outer steaming kettle water inlet (303), the lower ends of the outer steaming kettles are provided with an outer steaming kettle discharge outlet (304), the outer walls of the outer steaming kettles are provided with a third shell-and-tube type constant temperature heat exchanger (8), the outer steaming kettle feed inlet (301) is connected with a reactor discharge outlet (202) through a pipeline, the outer steaming kettle water inlet (303) is connected with a pure water pipeline, and the outer steaming kettle discharge;
the pyruvic acid transfer tank is provided with an pyruvic acid transfer tank outer steaming inlet (401), a pyruvic acid transfer tank discharge port (402) and a pyruvic acid transfer tank feed inlet (403), the pyruvic acid transfer tank outer steaming inlet (401) is connected with the outer steaming kettle gas outlet (302) through a pipeline, the pyruvic acid transfer tank discharge port (402) is connected with the mixing kettle pyruvic acid inlet (102) through a pipeline, and the pyruvic acid transfer tank feed inlet (403) is connected with a pyruvic acid storage tank;
the ethanol transfer tank is provided with an ethanol transfer tank outer steaming material inlet (501), an ethanol transfer tank discharge port (502) and an ethanol transfer tank feed inlet (503), the ethanol transfer tank outer steaming material inlet (501) is connected with an outer steaming kettle gas outlet (302) through a pipeline, the ethanol transfer tank discharge port (502) is connected with a mixing kettle ethanol inlet (101) through a pipeline, and the ethanol transfer tank feed inlet (503) is connected with an absolute ethanol storage tank.
2. The apparatus for producing poly-2-hydroxyacrylic acid according to claim 1, wherein the tubular reactor is made of graphite, and has a tube inner wall diameter of 10-20 cm and a total length of 50-150 m.
3. The production device of poly (2-hydroxyacrylic acid) according to claim 1, wherein the catalyst module (9) is composed of sodium alkoxide catalyst component and metallocene catalyst component, wherein the two components are sequentially and alternately arranged in 3-5 groups, the components are of a grid structure, the cross section of the components is equivalent to the cross section of the pipe diameter of the tubular reactor, and the thickness of the components is 1-2 cm.
4. The apparatus of claim 3, wherein the carrier material of the sodium alkoxide module is mesoporous molecular sieve SBA-15, and the catalyst main body is solid sodium methoxide and sodium hydroxide, physically fixed to the carrier material.
5. The apparatus for producing poly-2-hydroxyacrylic acid as claimed in claim 3, wherein the carrier material of the metallocene catalyst component is mesoporous molecular sieve SBA-15, the main catalyst is fixedly connected with the carrier material through a cocatalyst, the central metal of the main catalyst is one of Fe, Ti and Zr, and the cocatalyst can be alkylaluminoxane.
6. The apparatus for producing poly-2-hydroxyacrylic acid according to claim 1, wherein the water inlet (701) of the first heat exchanger is connected to the hot water inlet pipe and is connected in series with a valve and a circulation pump, the water outlet (702) of the first heat exchanger is connected to the hot water return pipe and is connected in series with a valve, the steam inlets at the upper ends of the other shell-and-tube type constant temperature heat exchangers are connected to the steam supply pipe and are connected in series with a valve, and the steam outlets at the lower ends are connected to the steam return pipe and are connected in series with a valve.
7. The apparatus for producing poly (2-hydroxyacrylic acid) according to claim 1, wherein the pipelines connecting the feed inlet of the reactor and the discharge outlet of the mixing kettle, the water inlet of the outer steaming kettle and the pure water pipeline, the discharge outlet of the pyruvic acid transfer pot and the pyruvic acid inlet of the mixing kettle, and the discharge outlet of the ethanol transfer pot and the ethanol inlet of the mixing kettle are all connected in series with a valve, a material pumping pump and an electronic flow meter, the pipelines connecting the discharge outlet of the tubular reactor and the feed inlet of the outer steaming kettle are connected in series with a valve, a diaphragm pump and an electronic flow meter, the pipelines connecting the gas outlet of the outer steaming kettle, the pyruvic acid transfer pot and the ethanol transfer pot in parallel are connected in series with a valve, a negative pressure pump, and the rest pipelines are all connected in series.
8. The apparatus for producing poly-2-hydroxyacrylic acid according to claim 1, wherein the external steaming vessel has at least two tanks connected in parallel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021041486.0U CN213085852U (en) | 2020-06-09 | 2020-06-09 | Production device of poly 2-hydroxy acrylic acid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021041486.0U CN213085852U (en) | 2020-06-09 | 2020-06-09 | Production device of poly 2-hydroxy acrylic acid |
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| CN213085852U true CN213085852U (en) | 2021-04-30 |
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| CN202021041486.0U Active CN213085852U (en) | 2020-06-09 | 2020-06-09 | Production device of poly 2-hydroxy acrylic acid |
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