CN110681314A - High-pressure production high-solid low-viscosity acrylic acid preparation device for laboratory and production process thereof - Google Patents
High-pressure production high-solid low-viscosity acrylic acid preparation device for laboratory and production process thereof Download PDFInfo
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- CN110681314A CN110681314A CN201911004014.XA CN201911004014A CN110681314A CN 110681314 A CN110681314 A CN 110681314A CN 201911004014 A CN201911004014 A CN 201911004014A CN 110681314 A CN110681314 A CN 110681314A
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 38
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 title claims abstract description 31
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 239000007787 solid Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 90
- 238000003756 stirring Methods 0.000 claims abstract description 23
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 238000010992 reflux Methods 0.000 claims abstract description 19
- 239000002904 solvent Substances 0.000 claims abstract description 17
- 239000000047 product Substances 0.000 claims abstract description 16
- 230000008878 coupling Effects 0.000 claims abstract description 13
- 238000010168 coupling process Methods 0.000 claims abstract description 13
- 238000005859 coupling reaction Methods 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 238000007599 discharging Methods 0.000 claims abstract description 12
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims abstract description 11
- 230000001276 controlling effect Effects 0.000 claims abstract description 11
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 7
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 6
- 239000007810 chemical reaction solvent Substances 0.000 claims abstract description 4
- 230000001105 regulatory effect Effects 0.000 claims abstract description 4
- 239000012535 impurity Substances 0.000 claims abstract description 3
- 238000001816 cooling Methods 0.000 claims description 26
- 239000000203 mixture Substances 0.000 claims description 9
- 238000001514 detection method Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 244000261422 Lysimachia clethroides Species 0.000 claims description 5
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- 239000003999 initiator Substances 0.000 claims description 4
- 239000000178 monomer Substances 0.000 claims description 4
- 238000005516 engineering process Methods 0.000 claims 1
- 238000007789 sealing Methods 0.000 abstract description 14
- 230000000694 effects Effects 0.000 description 3
- 230000009351 contact transmission Effects 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/04—Pressure vessels, e.g. autoclaves
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/002—Component parts of these vessels not mentioned in B01J3/004, B01J3/006, B01J3/02 - B01J3/08; Measures taken in conjunction with the process to be carried out, e.g. safety measures
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/02—Feed or outlet devices therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/03—Pressure vessels, or vacuum vessels, having closure members or seals specially adapted therefor
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation device for producing high-solid low-viscosity acrylic acid at high pressure in a laboratory and a production process thereof, and relates to the technical field of high-solid low-viscosity acrylic acid production, wherein the preparation device comprises a reaction kettle for containing a reaction solvent, a feeding device for adding raw materials, a stirring device for reaction stirring, a reflux device for carrying out reflux on reaction liquid, a discharging device for removing impurities and outputting reaction products, a pressure regulating device for regulating pressure and a heating device for controlling reaction temperature; the feeding device, the stirring device, the reflux device and the discharging device are respectively arranged on the reaction kettle. According to the invention, the magnetic coupling stirrer which has good sealing performance with the reaction kettle and can provide effective stirring in a high-pressure environment is adopted, the pressure is fully adjusted, butyl acetate with better solubility and purity can be used as a solvent, the use amount of the solvent is reduced, and meanwhile, the quality of an acrylic acid finished product can be obviously improved.
Description
Technical Field
The invention relates to the technical field of high-pressure production of high-solid low-viscosity acrylic acid, in particular to a preparation device for high-pressure production of high-solid low-viscosity acrylic acid for a laboratory and a use method thereof.
Background
At present, the preparation of acrylic acid usually adopts a normal pressure process, the equipment is simple, xylene is used as a solvent, a dripping tank is used, and the solvent is sublimated and recovered. The finished product prepared by the method has high impurity, large solvent consumption and long process route, and the automatic control of PLC is not realized.
Disclosure of Invention
The invention aims to provide a preparation device for producing high-solid low-viscosity acrylic acid at high pressure in a laboratory, which has high product quality, and a use method thereof.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a laboratory high-pressure production high-solid low-viscosity acrylic acid preparation device comprises a reaction kettle for containing a reaction solvent, a feeding device for adding raw materials, a stirring device for reaction stirring, a reflux device for feeding back reaction liquid and a discharging device for outputting reaction products; the feeding device, the stirring device, the reflux device and the discharging device are respectively arranged on the reaction kettle.
Preferably, the reaction kettle further comprises a heating and cooling device for heating and cooling the reaction liquid, and the heating and cooling device is installed at the outer wall of the reaction kettle.
Preferably, the reaction kettle further comprises a pressure sensing device for detecting the reaction pressure, a pressure adjusting device for adjusting the pressure and a control device for controlling the pressure adjusting device, wherein the pressure sensing device and the pressure adjusting device are arranged on the reaction kettle, the pressure sensing device is electrically connected with a signal input end of the control device, and the pressure adjusting device is electrically connected with a signal output end of the control device.
Preferably, the feeding device is a dosing metering pump.
Preferably, the stirring device is a magnetic coupling stirrer.
Preferably, the reflux device is a combination of a gooseneck and a tubular condenser.
Preferably, the pressure sensing device is a pressure sensor.
Preferably, the pressure regulating device is a back pressure valve.
Preferably, the heating and cooling device is a heat conducting oil heater.
A production process of a high-solid low-viscosity acrylic acid preparation device for laboratory production comprises the following steps:
(1) adding an initiator, a monomer raw material and a butyl acetate solvent into a reaction kettle through a feeding device;
(2) heating the mixture in the reaction kettle by a heating and cooling device; simultaneously stirring and reacting the mixture by a stirring device;
(3) hot steam of a butyl acetate solvent generated in the reaction kettle is subjected to reflux condensation through a reflux device;
(4) detecting the pressure in the reaction kettle in the reaction process through a pressure sensing device, transmitting detection data to a control device, controlling a pressure adjusting device to open to release the pressure when the pressure in the reaction kettle reaches a preset upper limit, and controlling the pressure adjusting device to close to maintain the pressure when the pressure in the reaction kettle reaches a preset lower limit;
(5) after the reaction is finished, cooling the product in the reaction kettle by the heating and cooling device;
(6) and after cooling is finished, outputting a high-solid low-viscosity acrylic acid product through a discharging device.
By adopting the technical scheme, the magnetic coupling stirrer which has good sealing performance with the reaction kettle and can provide effective stirring in a high-pressure environment is adopted, butyl acetate with better solubility and higher purity can be used as a solvent, the use amount of the solvent is reduced, and meanwhile, the quality of an acrylic acid finished product can be obviously improved; meanwhile, the magnetic coupling stirrer has better sealing performance compared with a conventional stirrer, is a non-contact transmission torque, replaces dynamic sealing with static sealing, can thoroughly solve the problem of pressure release which cannot be solved by the conventional mechanical sealing, can ensure the effective pressure in the reaction kettle, improves the reaction effect and further improves the quality of finished products; because high-pressure reaction is dangerous than ordinary pressure reaction, in high-pressure reaction, the dropwise addition of raw materials, the leakproofness of reation kettle and the regulation and control of reation kettle internal pressure all have important influence to reaction product nature and the security of whole reaction, can effectively detect the pressure in the reation kettle through pressure detection and pressure release system, prevent that pressure is too big and cause danger, can accurately regulate and control raw materials dropwise add volume through adding the medicine measuring pump, control reation kettle internal pressure size.
Drawings
FIG. 1 is a block diagram showing the construction of a manufacturing apparatus according to the present invention;
FIG. 2 is a schematic structural view of a production apparatus in example 3 of the present invention.
In the figure, 1-frame, 2-high pressure resistant reaction kettle, 3-magnetic coupling stirrer, 4-sealing shock pad, 5-tubular condenser and 6-plunger type sampling valve.
Detailed Description
The following further describes embodiments of the present invention with reference to the drawings. It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example 1
As shown in fig. 1, a laboratory high-pressure production high-solid low-viscosity acrylic acid preparation device comprises a reaction kettle for containing a reaction solvent, a feeding device for adding raw materials, a stirring device for reaction stirring, a reflux device for feeding back a reaction liquid, and a discharging device for outputting a reaction product; the feeding device, the stirring device, the reflux device and the discharging device are respectively arranged on the reaction kettle.
In order to heat or cool the mixture in the reaction kettle, the preparation device also comprises a heating and cooling device for heating and cooling the reaction liquid, and the heating and cooling device is arranged on the outer wall of the reaction kettle.
In order to facilitate the monitoring of the pressure in the reaction kettle and prevent the danger caused by overlarge pressure, the preparation device also comprises a pressure sensing device for detecting the reaction pressure, a pressure adjusting device for adjusting the pressure and a control device for controlling the pressure adjusting device, wherein the pressure sensing device and the pressure adjusting device are arranged on the reaction kettle, the pressure sensing device is electrically connected with the signal input end of the control device, and the pressure adjusting device is electrically connected with the signal output end of the control device.
In order to further ensure the safety of the reaction kettle, a safety relief device is arranged on the reaction kettle.
Example 2
A production process of a high-solid low-viscosity acrylic acid preparation device for laboratory production comprises the following steps:
(1) adding an initiator, a monomer raw material and a butyl acetate solvent into a reaction kettle through a feeding device;
(2) heating the mixture in the reaction kettle by a heating and cooling device; simultaneously, stirring the mixture by a stirring device for reaction;
(3) hot steam of a butyl acetate solvent generated in the reaction kettle is subjected to reflux condensation through a reflux device;
(4) the pressure in the reaction kettle in the reaction process is detected through the pressure sensing device, the detection data are transmitted to the control device, when the pressure in the reaction kettle reaches a preset upper limit, the control device controls the pressure adjusting device to open to release the pressure, and when the pressure in the reaction kettle reaches a preset lower limit, the control device controls the pressure adjusting device to close to maintain the pressure;
(5) after the reaction is finished, cooling the product in the reaction kettle by a heating and cooling device;
(6) and after cooling is finished, outputting a high-solid low-viscosity acrylic acid product through a discharging device.
Example 3
A laboratory is with high-pressure production high solid low glutinous acrylic acid preparation facilities, including the frame 1, fixedly mounted on the frame 1 has high pressure resistant reactor 2, the sealed installation has magnetic coupling agitator 3 on the high pressure resistant reactor 2, the (mixing) shaft of the magnetic coupling agitator 3 stretches into in the high pressure resistant reactor 2, still install the gooseneck (not shown) on the high pressure resistant reactor 2, gooseneck one end is linked together with high pressure resistant reactor 2, the other end of the gooseneck links together with tubular condenser 5, the reflux end of tubular condenser 5 is linked together with high pressure resistant reactor 2, still be equipped with the dosing pump (not shown) on the high pressure resistant reactor 2 and be used for adding the raw materials, the bottom of high pressure resistant reactor 2 is installed with plunger type sample valve 6, the product used for discharging after the reaction, still install the pressure sensor that is used for detecting reaction pressure on the high pressure resistant reactor 2, the backpressure valve used for adjusting pressure and the controller that is used for controlling the backpressure valve, the controller can adopt single chip microcomputer control, and pressure sensor is connected with the signal input part electricity of controller, and the signal output electricity of back pressure valve and controller is connected, and 2 outer walls of high pressure resistant reation kettle department still are equipped with the conduction oil heater, can heat the cooling to the reactant in the high pressure resistant reation kettle 2.
In order to further improve the sealing effect between the magnetic coupling stirrer 3 and the high-pressure resistant reaction kettle 2, a sealing shock pad 4 is arranged between the magnetic coupling stirrer 3 and the high-pressure resistant reaction kettle 2.
In order to further ensure the safety of the reaction kettle, an explosion-proof tank is arranged on the reaction kettle.
Example 4
A production process of a high-solid low-viscosity acrylic acid preparation device for laboratory production comprises the following steps:
(1) adding an initiator, a monomer raw material and a butyl acetate solvent into the high-pressure resistant reaction kettle 2 through a dosing metering pump;
(2) heating the mixture in the high-pressure resistant reaction kettle 2 by a heat-conducting oil heater; simultaneously, the mixture is stirred and reacted by a magnetic coupling stirrer 3;
(3) hot steam of butyl acetate solvent generated by the reaction in the high pressure resistant reaction kettle 2 is subjected to reflux condensation by a tubular condenser 5;
(4) detecting the pressure in the high-pressure resistant reaction kettle 2 in the reaction process through a pressure sensor, transmitting detection data to a controller, controlling a back pressure valve to open to release the pressure when the pressure in the high-pressure resistant reaction kettle 2 reaches a preset upper limit, and controlling the back pressure valve to close to maintain the pressure when the pressure in the high-pressure resistant reaction kettle 2 reaches a preset lower limit;
(5) after the reaction is finished, cooling the product in the high-pressure resistant reaction kettle 2 by a heat-conducting oil heater;
(6) after cooling, a high-solid low-viscosity acrylic acid product is output through a plunger type sampling valve 6.
According to the invention, the magnetic coupling stirrer 3 which has good sealing performance with the reaction kettle and can provide effective stirring in a high-pressure environment is adopted, butyl acetate with better solubility and purity can be used as a solvent, the use amount of the solvent is reduced, and meanwhile, the quality of an acrylic acid finished product can be obviously improved; meanwhile, compared with a conventional stirrer, the magnetic coupling stirrer 3 has better sealing performance and is a non-contact transmission torque, static sealing replaces dynamic sealing, the problem of pressure release which cannot be solved by the conventional mechanical sealing can be thoroughly solved, the effective pressure in the reaction kettle can be ensured, the reaction effect is improved, and the quality of a finished product is further improved; because high-pressure reaction is dangerous than ordinary pressure reaction, in high-pressure reaction, the dropwise addition of raw materials, the leakproofness of reation kettle and the regulation and control of reation kettle internal pressure all have important influence to reaction product nature and the security of whole reaction, can effectively detect the pressure in the reation kettle through pressure detection and pressure release system, prevent that pressure is too big and cause danger, can accurately regulate and control raw materials dropwise add volume through adding the medicine measuring pump, control reation kettle internal pressure size.
The embodiments of the present invention have been described in detail with reference to the accompanying drawings, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, and the scope of protection is still within the scope of the invention.
Claims (10)
1. The utility model provides a laboratory is with high pressure production height solid low glutinous acrylic acid preparation facilities which characterized in that: the device comprises a reaction kettle for containing a reaction solvent, a feeding device for adding raw materials, a stirring device for reaction stirring, a reflux device for feeding back reaction liquid and a discharging device for outputting reaction products; the feeding device, the stirring device, the reflux device and the discharging device are respectively arranged on the reaction kettle.
2. The laboratory high pressure production high solid low viscosity acrylic acid production apparatus according to claim 1, characterized in that: the reaction kettle further comprises a heating and cooling device for heating and cooling the reaction liquid, and the heating and cooling device is installed on the outer wall of the reaction kettle.
3. The laboratory high pressure production high solid low viscosity acrylic acid production apparatus according to claim 1, characterized in that: the reaction kettle is characterized by further comprising a pressure sensing device for detecting reaction pressure, a pressure adjusting device for adjusting the pressure and a control device for controlling the pressure adjusting device, wherein the pressure sensing device and the pressure adjusting device are arranged on the reaction kettle, the pressure sensing device is electrically connected with a signal input end of the control device, and the pressure adjusting device is electrically connected with a signal output end of the control device.
4. The laboratory high pressure production high solid low viscosity acrylic acid production apparatus according to claim 1, characterized in that: the feeding device is a dosing metering pump.
5. The laboratory high pressure production high solid low viscosity acrylic acid production apparatus according to claim 1, characterized in that: the stirring device is a magnetic coupling stirrer.
6. The laboratory high pressure production high solid low viscosity acrylic acid production apparatus according to claim 1, characterized in that: the reflux device is a combination of a gooseneck tube and a tubular condenser.
7. The laboratory high pressure production high solid low viscosity acrylic acid production apparatus according to claim 3, characterized in that: the pressure sensing device is a pressure sensor.
8. The laboratory high pressure production high solid low viscosity acrylic acid production apparatus according to claim 3, characterized in that: the pressure regulating device is a backpressure valve.
9. The laboratory high pressure production high solid low viscosity acrylic acid production apparatus according to claim 2, characterized in that: the heating and cooling device is a heat conducting oil heater.
10. The utility model provides a production technology of high solid low glutinous acrylic acid preparation facilities of high pressure production is used in laboratory which characterized in that: the method comprises the following steps:
(1) adding an initiator, a monomer raw material and a butyl acetate solvent into a reaction kettle through a feeding device;
(2) heating the mixture in the reaction kettle by a heating and cooling device; simultaneously stirring and reacting the mixture by a stirring device;
(3) carrying out reflux condensation on hot steam of a butyl acetate solvent generated in the reaction kettle by using a reflux device to remove impurities;
(4) detecting the pressure in the reaction kettle in the reaction process through a pressure sensing device, transmitting detection data to a control device, controlling a pressure adjusting device to open to release the pressure when the pressure in the reaction kettle reaches a preset upper limit, and controlling the pressure adjusting device to close to maintain the pressure when the pressure in the reaction kettle reaches a preset lower limit;
(5) after the reaction is finished, cooling the product in the reaction kettle by the heating and cooling device;
(6) and after cooling is finished, outputting a high-solid low-viscosity acrylic acid product through a discharging device.
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US4185073A (en) * | 1976-07-26 | 1980-01-22 | Standard Oil Company (Indiana) | Apparatus for iso- or terephthalic acid production in and recovery from benzoic acid-water solvent system |
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CN204074008U (en) * | 2014-09-29 | 2015-01-07 | 山西同济药业有限公司 | Reactor magnetic couple agitator |
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-
2019
- 2019-10-22 CN CN201911004014.XA patent/CN110681314A/en active Pending
Patent Citations (6)
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Non-Patent Citations (1)
Title |
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孙志娟;张心亚;黄洪;陈焕钦;: "丙烯酸树脂合成工艺的正交优化", 合成树脂及塑料, no. 04, 25 July 2005 (2005-07-25), pages 26 - 29 * |
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