CN116078334B - Paranitrophenol sodium apparatus for producing with automatic temperature control function - Google Patents
Paranitrophenol sodium apparatus for producing with automatic temperature control function Download PDFInfo
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- CN116078334B CN116078334B CN202310373544.1A CN202310373544A CN116078334B CN 116078334 B CN116078334 B CN 116078334B CN 202310373544 A CN202310373544 A CN 202310373544A CN 116078334 B CN116078334 B CN 116078334B
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- BTJIUGUIPKRLHP-UHFFFAOYSA-N 4-nitrophenol Chemical compound OC1=CC=C([N+]([O-])=O)C=C1 BTJIUGUIPKRLHP-UHFFFAOYSA-N 0.000 title claims abstract description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 title claims abstract description 6
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 6
- 239000011734 sodium Substances 0.000 title claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 21
- CURNJKLCYZZBNJ-UHFFFAOYSA-M sodium;4-nitrophenolate Chemical compound [Na+].[O-]C1=CC=C([N+]([O-])=O)C=C1 CURNJKLCYZZBNJ-UHFFFAOYSA-M 0.000 claims abstract description 15
- 230000008878 coupling Effects 0.000 claims abstract description 14
- 238000010168 coupling process Methods 0.000 claims abstract description 14
- 238000005859 coupling reaction Methods 0.000 claims abstract description 14
- 230000005611 electricity Effects 0.000 claims abstract description 11
- 239000012530 fluid Substances 0.000 claims abstract description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 174
- 239000000243 solution Substances 0.000 claims description 52
- 238000002156 mixing Methods 0.000 claims description 48
- 238000001125 extrusion Methods 0.000 claims description 30
- 238000003756 stirring Methods 0.000 claims description 29
- 238000001514 detection method Methods 0.000 claims description 27
- 238000002955 isolation Methods 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- CZGCEKJOLUNIFY-UHFFFAOYSA-N 4-Chloronitrobenzene Chemical compound [O-][N+](=O)C1=CC=C(Cl)C=C1 CZGCEKJOLUNIFY-UHFFFAOYSA-N 0.000 claims description 19
- 238000007789 sealing Methods 0.000 claims description 17
- 238000007599 discharging Methods 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 9
- 230000008859 change Effects 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 230000007246 mechanism Effects 0.000 claims description 7
- 239000012528 membrane Substances 0.000 claims description 5
- 238000005260 corrosion Methods 0.000 claims description 4
- 230000007797 corrosion Effects 0.000 claims description 4
- 238000009826 distribution Methods 0.000 claims description 4
- 239000013013 elastic material Substances 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 14
- 239000005992 Sodium p-nitrophenolate Substances 0.000 abstract description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 14
- 238000006243 chemical reaction Methods 0.000 description 6
- OORLTLMFPORJLV-UHFFFAOYSA-N 4-nitrophenol;sodium Chemical compound [Na].OC1=CC=C([N+]([O-])=O)C=C1 OORLTLMFPORJLV-UHFFFAOYSA-N 0.000 description 4
- 230000036632 reaction speed Effects 0.000 description 4
- 230000001105 regulatory effect Effects 0.000 description 4
- IQUPABOKLQSFBK-UHFFFAOYSA-N 2-nitrophenol Chemical compound OC1=CC=CC=C1[N+]([O-])=O IQUPABOKLQSFBK-UHFFFAOYSA-N 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- PLIKAWJENQZMHA-UHFFFAOYSA-N 4-aminophenol Chemical compound NC1=CC=C(O)C=C1 PLIKAWJENQZMHA-UHFFFAOYSA-N 0.000 description 2
- 238000006482 condensation reaction Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- LCCNCVORNKJIRZ-UHFFFAOYSA-N parathion Chemical compound CCOP(=S)(OCC)OC1=CC=C([N+]([O-])=O)C=C1 LCCNCVORNKJIRZ-UHFFFAOYSA-N 0.000 description 1
- RLBIQVVOMOPOHC-UHFFFAOYSA-N parathion-methyl Chemical compound COP(=S)(OC)OC1=CC=C([N+]([O-])=O)C=C1 RLBIQVVOMOPOHC-UHFFFAOYSA-N 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000000844 transformation Methods 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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
-
- 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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/002—Avoiding undesirable reactions or side-effects, e.g. avoiding explosions, or improving the yield by suppressing side-reactions
-
- 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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
- B01J19/0066—Stirrers
-
- 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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00054—Controlling or regulating the heat exchange system
- B01J2219/00056—Controlling or regulating the heat exchange system involving measured parameters
- B01J2219/00058—Temperature measurement
-
- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00162—Controlling or regulating processes controlling the pressure
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a device for producing sodium paranitrophenolate with an automatic temperature control function, and relates to the technical field of sodium paranitrophenolate production. The utility model provides a paranitrophenol sodium apparatus for producing with automatic temperature control function, includes the landing leg, and the landing leg is provided with control terminal, and the landing leg rigid coupling has mixed casing, and mixed casing is provided with inlet and leakage fluid dram, all is provided with the solenoid valve of being connected with control terminal electricity in inlet and the leakage fluid dram, and mixed casing is provided with discharge valve, temperature sensor and the pressure sensor of being connected with control terminal electricity. The invention can regulate and control the temperature and the pressure in the production process of the sodium p-nitrophenolate, and avoid the generation of black material phenomenon.
Description
Technical Field
The invention relates to the technical field of sodium paranitrophenolate production, in particular to a sodium paranitrophenolate production device with an automatic temperature control function.
Background
The p-nitrophenol sodium is an important fine chemical intermediate, is used as a raw material for preparing pesticides such as parathion, methyl parathion and the like, and can be prepared into p-aminophenol through acidification and reduction, wherein the p-nitrophenol sodium is an important intermediate of developer, medicine and dye, and the production process of the p-nitrophenol sodium is as follows: adding a certain volume of sodium hydroxide solution with the concentration of 133-136g/L into a hydrolysis kettle, adding para-nitrochlorobenzene, heating the temperature in the reaction kettle to 157 ℃, stopping heating, naturally raising the temperature and the pressure to 168 ℃ and 0.75Mpa by the heat release of the hydrolysis reaction, maintaining for 35h, cooling to 120 ℃, pressing the material to a crystallizer for cooling crystallization by using the residual pressure in the kettle, and carrying out vacuum suction filtration to obtain the product.
In the traditional industrial production, excessive sodium hydroxide is required to be added to ensure that high conversion rate and faster reaction speed are obtained, so that by-products are increased, hydrolysis reaction of p-nitrochlorobenzene and sodium hydroxide is exothermic, the concentration of sodium hydroxide participating in the hydrolysis reaction is not too high, the alkali concentration is increased, the reaction speed is increased exponentially, a large amount of heat is instantaneously released, the temperature and the pressure in a kettle are excessively fast to control, and meanwhile, reduction condensation reaction of p-nitrophenol sodium generated under high-temperature, pressure and alkaline conditions can occur to form black materials.
Disclosure of Invention
In order to solve the technical problems, the invention provides a device for producing sodium paranitrophenolate with an automatic temperature control function by pressure detection.
The technical proposal is as follows: the utility model provides a paranitrophenol sodium apparatus for producing with automatic temperature control function, which comprises supporting legs, the landing leg is provided with control terminal, the landing leg rigid coupling has mixed casing, mixed casing is provided with inlet and leakage fluid dram, all be provided with the solenoid valve of being connected with control terminal electricity in inlet and the leakage fluid dram, mixed casing is provided with discharge valve that is connected with control terminal electricity, temperature sensor and pressure sensor, the inside of mixed casing inlays the heating part of being connected with control terminal electricity, there is reinforced casing through the backup pad rigid coupling in the mixed casing, mixed casing rigid coupling has the communicating pipe with reinforced casing intercommunication, one side that the communicating pipe was kept away from to reinforced casing is provided with the outlet of circumference equidistant distribution, the landing leg is provided with the rabbling mechanism that is used for accelerating paranitrochlorobenzene and sodium hydroxide mixed speed, through communicating pipe, reinforced casing and outlet add a small amount of sodium hydroxide solution gradually in to mixed casing, temperature and pressure maintain at 168 ℃,0.75Mpa in the mixed casing.
Preferably, the stirring mechanism comprises a servo motor fixedly connected to the supporting leg, the servo motor is electrically connected with the control terminal, an output shaft of the servo motor is fixedly connected with a rotating shaft rotationally connected with the mixing shell, stirring blades distributed at equal intervals in the circumferential direction are fixedly connected with the rotating shaft, and the stirring blades distributed at equal intervals in the circumferential direction are all provided with a discharging part for quantitatively discharging sodium hydroxide solution in the feeding shell.
Preferably, the stirring blade is provided with a porous support rod for increasing the contact area of the stirring blade with the solution.
Preferably, the discharging part comprises a gear ring, the gear ring is fixedly connected with stirring blades distributed at equal intervals in the circumferential direction, the mixing shell is rotationally connected with a reciprocating screw, the reciprocating screw is fixedly connected with a gear meshed with the gear ring, the reciprocating screw is in threaded connection with a sliding plate, the sliding plate is provided with an adjusting component, and the adjusting component is used for adjusting the discharging speed of sodium hydroxide solution in the feeding shell.
Preferably, the adjusting component comprises a sliding rod fixedly connected to a sliding plate, the sliding rod is in sliding connection with a feeding shell, a limiting pipe is in sliding connection with the feeding shell, a spring is fixedly connected between the limiting pipes of the sliding plate, a pushing disc fixedly connected with the limiting pipe is in sliding connection with the feeding shell, the pushing disc is in sliding connection with the sliding rod, the pushing disc is divided into a first cavity and a second cavity in the feeding shell, the second cavity is communicated with the water outlet, the longitudinal length of the pushing disc is greater than that of the water outlet, a through hole is formed in the pushing disc, a one-way valve is arranged in the through hole of the pushing disc, a plugging component for sealing the water outlet is arranged in the feeding shell, and a detecting component for detecting pressure change in the mixing shell is arranged in the feeding shell.
Preferably, the shutoff subassembly is including the swivel becket, the swivel becket rotates to be connected in reinforced casing, the swivel becket rigid coupling has L shape pole, the slide bar is provided with the spout with L shape pole sliding connection, the lower part of spout is vertical, the upper portion of spout is the slope, reinforced casing rigid coupling has the stopper of circumference equidistant distribution, one side that reinforced casing was kept away from to the stopper sets up to the arcwall face, the stopper is provided with the through-hole that communicates with adjacent outlet, the swivel becket rigid coupling has the extrusion piece of circumference equidistant distribution, extrusion piece and the arcwall face sealing fit of adjacent stopper.
Preferably, the extrusion block is made of elastic material and used for increasing the contact area between the extrusion block and the limiting block.
Preferably, the detection assembly comprises a guide pipe fixedly connected to the feeding shell and communicated with the second cavity, the guide pipe is communicated with the detection shell, a first push plate is slidably connected in the second cavity, the first push plate, the push plate and the feeding shell are matched to form a quantitative cavity, a connecting rod located in the guide pipe is fixedly connected to the first push plate, a second push plate fixedly connected with the connecting rod is slidably connected in the detection shell, an isolation diaphragm located on the lower side of the second push plate is arranged in the detection shell, the second push plate and the detection shell are matched to form a third cavity, and the second push plate, the isolation diaphragm and the detection shell are matched to form a fourth cavity.
Preferably, the protection assembly is arranged on the detection shell and used for protecting the isolation diaphragm, the protection assembly comprises a sliding disc, the detection shell is provided with an annular groove, the sliding disc is connected in the annular groove of the detection shell in a sliding mode, the isolation diaphragm and the sliding disc are matched to form a fifth cavity, and the fifth cavity is filled with protection liquid.
Preferably, the sliding plate is made of corrosion-resistant materials, so as to prolong the service life of the sliding plate.
1. By adding a certain amount of sodium hydroxide solution and paranitrochlorobenzene into the mixed shell, the exothermic temperature of the hydrolysis reaction of the sodium hydroxide solution and the paranitrochlorobenzene tends to 168 ℃,0.75Mpa, and a small amount of sodium hydroxide solution is gradually added in the follow-up process to maintain the temperature and the pressure in the mixed shell at 168 ℃ and 0.75Mpa, the temperature and the pressure in the production process of producing paranitrosodium phenolate are regulated and controlled, and the black material phenomenon is avoided.
2. The stirring blade drives the porous supporting rod to rotate, so that the contact area between the stirring blade and materials is increased, the reaction speed of the paranitrochlorobenzene and sodium hydroxide solution is accelerated, and the production efficiency of the paranitrosodium nitrophenolate is improved.
3. The amount of sodium hydroxide in the mixing shell is reduced by detecting the pressure change in the mixing shell, so that the pressure and the temperature in the mixing shell are dynamically adjusted, the problem that the temperature sensor cannot detect the temperature change in real time is solved, and the pressure and the temperature in the mixing shell are further regulated and controlled by a small extent.
Drawings
Fig. 1 is a schematic perspective view of the present invention.
Fig. 2 is a schematic perspective view of the stirring mechanism of the present invention.
Fig. 3 is a schematic perspective view of a discharging part of the present invention.
Fig. 4 is a schematic perspective view of an adjusting assembly according to the present invention.
Fig. 5 is a schematic perspective view of a plugging assembly according to the present invention.
Fig. 6 is a schematic perspective view of a detection assembly according to the present invention.
Fig. 7 is a schematic perspective view of a protective assembly according to the present invention.
The marks of the components in the drawings are as follows: 1-supporting leg, 2-mixing shell, 201-liquid inlet, 202-liquid outlet, 203-exhaust valve, 3-temperature sensor, 4-charging shell, 401-water outlet, 402-first cavity, 403-second cavity, 4031-dosing cavity, 404-limiting block, 5-communicating pipe, 601-servo motor, 602-rotating shaft, 603-stirring blade, 701-gear ring, 702-reciprocating screw, 703-gear, 704-sliding plate, 801-sliding rod, 8011-sliding groove, 802-limiting tube, 803-spring, 804-pushing disc, 901-rotating ring, 902-L-shaped rod, 903-extrusion block, 1001-conduit, 1002-detecting shell, 10021-third cavity, 10022-fourth cavity, 10023-fifth cavity, 1003-first pushing plate, 1004-connecting rod, 1005-second pushing plate, 1006-isolating membrane, 1007-sliding disc.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
Example 1: the utility model provides a paranitrophenol sodium apparatus for producing with automatic temperature control function, as shown in fig. 1-3, including landing leg 1, landing leg 1 is provided with control terminal (not shown in the figure), landing leg 1 rigid coupling has hybrid housing 2, the right side on hybrid housing 2 upper portion is provided with inlet 201, the right side of hybrid housing 2 lower part is provided with fluid outlet 202, all be provided with the solenoid valve that is connected with control terminal electricity in inlet 201 and the fluid outlet 202, the left side of hybrid housing 2 is provided with discharge valve 203 that is connected with control terminal electricity, temperature sensor 3 and pressure sensor (not shown in the figure), the inside of hybrid housing 2 is inlayed and is had the heating part (not shown in the figure) that is connected with control terminal electricity, there is reinforced housing 4 through the backup pad rigid coupling in hybrid housing 2, hybrid housing 2 rigid coupling has communicating pipe 5 with reinforced housing 4 intercommunication, communicating pipe 5 is used for adding sodium hydroxide solution to reinforced housing 4, the lower part of reinforced housing 4 lateral surface is provided with circumference equidistant 401, landing leg 1 is provided with the rabbling mechanism that is used for accelerating the mixed speed of paranitrochlorobenzene and sodium hydroxide, be provided with the discharge outlet, firstly with quantitative sodium hydroxide and mix the housing and temperature sensor 3 and pressure sensor (not shown in the figure) is carried out in the hybrid housing 2, the mixed housing 2 and the mixed temperature of a small amount of temperature and the mixed housing is kept at 75, the mixed temperature sensor is added in the continuous temperature sensor 2 and the mixed temperature sensor is 75, the mixed temperature sensor is added in the mixed housing 2 and the temperature sensor is 75, and the mixed temperature sensor is added in the continuous temperature sensor is 75 in the production process of the mixed temperature sensor.
As shown in fig. 1 and 2, the stirring mechanism comprises a servo motor 601, the servo motor 601 is fixedly connected to a supporting leg 1, the servo motor 601 is electrically connected with a control terminal, an output shaft of the servo motor 601 is fixedly connected with a rotating shaft 602 which is rotationally connected with a mixing shell 2, stirring blades 603 which are distributed at equal intervals circumferentially are fixedly connected to the upper end of the rotating shaft 602, the stirring blades 603 are positioned in the mixing shell 2, the stirring blades 603 are provided with porous supporting rods, the stirring blades 603 drive the porous supporting rods to rotate, the contact area between the stirring blades 603 and materials is increased, the reaction speed of paranitrochlorobenzene and sodium hydroxide solution is accelerated, the production efficiency of paranitrosodium nitrophenolate is improved, and the stirring blades 603 which are distributed at equal intervals circumferentially are all provided with discharging components for quantitatively discharging sodium hydroxide solution in a charging shell 4.
As shown in fig. 2 and fig. 3, the discharging component comprises a gear ring 701, the gear ring 701 is fixedly connected to the upper end of stirring blades 603 distributed at equal intervals in the circumferential direction, a reciprocating screw 702 is rotatably connected to the right side of the upper portion in the mixing shell 2, a gear 703 engaged with the gear ring 701 is fixedly connected to the lower end of the reciprocating screw 702, the reciprocating screw 702 is in threaded connection with a sliding plate 704, the reciprocating screw 702 rotates to drive the sliding plate 704 to reciprocate up and down, and the sliding plate 704 is provided with an adjusting component for adjusting the discharging speed of the sodium hydroxide solution in the feeding shell 4.
As shown in fig. 3 and 4, the adjusting component comprises a sliding rod 801, the sliding rod 801 is fixedly connected to the left side of a sliding plate 704, the sliding rod 801 is slidably connected with the lower portion of a charging shell 4, a limiting pipe 802 is slidably connected to the upper portion of the charging shell 4, a spring 803 is fixedly connected between the sliding plate 704 and the upper surface of the limiting pipe 802, a push plate 804 fixedly connected with the limiting pipe 802 is slidably connected in the charging shell 4, the push plate 804 is slidably connected with the sliding rod 801, the charging shell 4 is divided into a first cavity 402 and a second cavity 403, the first cavity 402 is located on the upper side of the second cavity 403, the second cavity 403 is communicated with the drain outlet 401, the longitudinal length of the push plate 804 is larger than the longitudinal length of the drain outlet 401, the push plate 804 moves downwards to drain sodium hydroxide solution in the second cavity 403, the push plate 804 is slidably connected with the drain outlet 401, a through hole is formed in the right side of the push plate 804, a one-way valve is arranged in the through hole of the push plate 804, the one-way valve is used for conveying sodium hydroxide solution into the second cavity 403, the first cavity 402 is arranged in the second cavity 403, the charging shell 4 is arranged in a sealing component 401, the pressure in the plugging component is arranged in the charging shell 4 is used for detecting the change of the mixing component 2, and the pressure in the mixing shell is detected.
As shown in fig. 4 and 5, the plugging assembly comprises a rotating ring 901, the rotating ring 901 is rotatably connected to the lower part of the outer side surface of the charging shell 4, an L-shaped rod 902 is fixedly connected to the lower surface of the rotating ring 901, a sliding groove 8011 which is slidably connected with the lower part of the L-shaped rod 902 is arranged on the sliding rod 801, the lower part of the sliding groove 8011 is vertical, the upper part of the sliding groove 8011 is inclined, the sliding rod 801 moves downwards, when the lower part of the L-shaped rod 902 is matched with the inclined part of the sliding groove 8011, the sliding rod 801 drives the L-shaped rod 902 to rotate anticlockwise, a limiting block 404 which is distributed at equal intervals in circumferential direction is fixedly connected to one side of the charging shell 4 close to the water outlet 401, one side of the limiting block 404 far away from the charging shell 4 is provided with an arc surface, the stopper 404 is provided with the through-hole that communicates with adjacent outlet 401, the upper surface rigid coupling of swivel ring 901 has circumferentially equidistant extrusion piece 903 that distributes, extrusion piece 903 and the arcwall face sealing fit of adjacent stopper 404, when extrusion piece 903 and stopper 404 contact, extrusion piece 903 is the through-hole shutoff with stopper 404, the interior sodium hydroxide solution of reinforced casing 4 can't follow outlet 401 and discharge, extrusion piece 903's material is elastic material, when extrusion piece 903 and stopper 404 contact, extrusion piece 903 receives the extrusion and takes place deformation, increased the area of contact of extrusion piece 903 and stopper 404, the leakproofness between improvement extrusion piece 903 and the stopper 404.
As shown in fig. 6 and 7, the detection assembly comprises a conduit 1001, the conduit 1001 is fixedly connected to the lower part of the charging housing 4 and is communicated with the second cavity 403, the lower end of the conduit 1001 is communicated with a detection housing 1002, the lower part in the second cavity 403 is slidably connected with a first push plate 1003, the first push plate 1003 is lower than the water outlet 401, the first push plate 1003 only slides on the lower side of the water outlet 401, the first push plate 1003, the push plate 804 and the charging housing 4 are matched to form a dosing cavity 4031, when the first push plate 1003 is matched with the bottom in the charging housing 4, the upper surface of the first push plate 1003 is aligned with the lower side of the water outlet 401 on the lowest side, the upper surface of the first push plate 1003 is aligned with the lower side of the dosing cavity 4031, so as to ensure that sodium hydroxide solution in the dosing cavity 4031 is completely discharged, the lower surface of the first push plate 1003 is fixedly connected with a connecting rod 1004 in the conduit 1001, a gap is reserved between the connecting rod 1004 and the conduit 1001, the detection housing 1002 is slidably connected with a second push plate 1006 fixedly connected with the lower end of the connecting rod 1004, an isolation membrane 1006 is arranged in the detection housing 1002, when the pressure in the mixing housing 2 changes, the second push plate 1002 and the detection housing 403 is matched with the third push plate 403 to form a third cavity 21, and the third cavity 1005 is matched with the fourth cavity 1005, and the third cavity 1005 is formed by the third membrane cavity 21 and the third cavity 1005.
Before the production of sodium paranitrophenolate by using the production device, an operator firstly communicates sodium hydroxide solution with the upper end of the communicating pipe 5, sodium hydroxide solution is stored in the first cavity 402 and the quantitative cavity 4031, when the production device is required to be used for producing sodium paranitrophenolate, the operator opens the electromagnetic valve in the liquid inlet 201 through the control terminal, the paranitrochlorobenzene, sodium hydroxide solution and other raw materials are added into the mixing shell 2 through the liquid inlet 201 (the quantity of the added sodium hydroxide solution is smaller at this time and only used for enabling the temperature and the pressure in the mixing shell 2 to reach the specified value), after the addition of the paranitrochlorobenzene, the sodium hydroxide solution and other raw materials is completed, the control terminal closes the electromagnetic valve in the liquid inlet 201 and starts the heating part, the materials in the mixing shell 2 are heated, the temperature of the materials in the mixing shell 2 is gradually increased, the temperature sensor 3 detects the temperature of the materials in the mixing shell 2 in real time, when the temperature of the materials reaches 157 ℃, the control terminal stops heating the heating part, the materials in the mixing shell 2 are stopped, the sodium hydroxide and the temperature of the paranitrochlorobenzene in the mixing shell 2 is increased to 0.168 MPa, the hydrolysis reaction is carried out, and the hydrolysis reaction of the paranitrochlorobenzene is carried out under the conditions that the temperature of the temperature reaches 0.168 MPa, and the hydrolysis reaction temperature in the mixing shell 2 is carried out under the conditions.
Then adding sodium hydroxide solution into the mixing shell 2 to ensure that the temperature and the pressure in the mixing shell 2 are maintained at 168 ℃ and 0.75Mpa, and in order to avoid the phenomenon that the produced sodium p-nitrophenolate undergoes a reduction condensation reaction to form a black material due to the rapid increase of the temperature and the pressure caused by the total addition of the sodium hydroxide solution, the following operations are carried out: the control terminal starts the servo motor 601, the output shaft of the servo motor 601 drives the rotating shaft 602 to rotate, the rotating shaft 602 drives the three stirring blades 603 to rotate, the three stirring blades 603 drive the gear ring 701 to rotate, the gear ring 701 drives the reciprocating screw 702 to rotate through the gear 703, the reciprocating screw 702 drives the sliding plate 704 to move downwards, as the extrusion block 903 seals the water outlet 401, therefore, sodium hydroxide solution in the quantitative cavity 4031 cannot be discharged, the one-way valve in the through hole of the push plate 804 is in a closed state, the push plate 804 cannot move downwards, the limiting pipe 802 cannot move downwards, in the process of downwards moving the sliding plate 704, the spring 803 is compressed, the sliding plate 704 drives the sliding rod 801 to move downwards, the lower end of the L-shaped rod 902 is located at the vertical part of the sliding groove 8011, when the lower end of the L-shaped rod 902 contacts with the inclined part of the sliding groove 8011, the sliding rod 801 continues to move downwards, the sliding groove 8011 limits the lower end of the L-shaped rod 902 and drives the L-shaped rod 902 to rotate, the L-shaped rod 902 drives the rotating ring 901 to rotate anticlockwise, the extrusion block 903 rotates anticlockwise and is far away from the adjacent limiting block 404, the extrusion block 903 seals the adjacent limiting block 404, the adjacent limiting block 802 cannot move downwards, the spring 802 moves downwards, the limiting block 802, the reset pipe 802 cannot move downwards, the temperature is kept by the volume of the sodium hydroxide solution in the volume of the cavity 402, the mixed solution is discharged into the cavity 402, the cavity is equal to the volume of the water outlet of the water, and the mixed solution is discharged by the volume of the water, and the sodium hydroxide solution is discharged by the temperature of the sealing agent, and the volume of the water in the 402, and the volume of the water is discharged by the water, and the water is discharged by the water, and has the concentration is discharged by the water, and has lower concentration, and has lower concentration.
In summary, a certain amount of sodium hydroxide solution and paranitrochlorobenzene are added into the mixing shell 2, so that the exothermic temperature of the hydrolysis reaction of the sodium hydroxide solution and paranitrochlorobenzene tends to 168 ℃,0.75Mpa, a small amount of sodium hydroxide solution is gradually added subsequently to maintain the temperature and pressure in the mixing shell 2 at 168 ℃,0.75Mpa, the excess pressure is discharged through the exhaust valve 203, the temperature and pressure in the production process of paranitrosodium phenolate are regulated and controlled, the generation of black material phenomenon is avoided, the pressure in the first cavity 402 is reduced in the downward moving process of the pushing disc 804, and the sodium hydroxide solution in the communicating pipe 5 is replenished into the first cavity 402.
When the lower side of the push plate 804 is in contact with the upper side of the first push plate 1003, the first push plate 1003 is not positioned at the lowest side of the second cavity 403, the push plate 804 moves downwards to press the first push plate 1003, the first push plate 1003 drives the second push plate 1005 to move downwards through the connecting rod 1004, the isolation diaphragm 1006 deforms, the upward bulge amplitude of the isolation diaphragm 1006 decreases, when the lower surface of the first push plate 1003 is in contact with the bottom in the charging shell 4, the first push plate 1003 does not move downwards any more, sodium hydroxide solution in the dosing cavity 4031 is completely discharged, the spring 803 is still in a compressed state, the push plate 804 seals the water outlet 401, the sliding plate 704 is positioned at the lower side of the reciprocating screw 702, the sliding plate 704 starts to move upwards along with the continuous rotation of the reciprocating screw 702, the sliding plate 704 drives the sliding rod 801 to move upwards, the sliding groove 8011 makes the L-shaped rod 902 rotate clockwise, the extrusion block 903 gradually approaches to the adjacent 404, when the extrusion block 903 is in contact with the limiting block 404, and the extrusion block 903 is made of elastic material, therefore the extrusion block 903 deforms due to extrusion deformation when the extrusion block 903 is in contact with the limiting block 404, the contact area between the extrusion block 903 and the limiting block 903 is increased, the sealing performance between the extrusion block 903 and the lower side of the limiting block 404 is kept in contact with the sealing state, and the upper side of the sealing plate 404 is kept in contact with the sealing state, and the upper side of the sealing part of the sliding plate 804 is kept in contact with the sealing plate 404, and the upper side of the sealing plate 2, and the upper side of the sealing plate is kept in contact with the sealing position with the sealing plate 404.
When the push plate 804 moves upwards, the first push plate 1003 moves upwards in synchronization with the push plate 804, and the reason why the first push plate 1003 moves upwards: because the pressure in the mixed shell 2 causes the isolation diaphragm 1006 to deform, the isolation diaphragm 1006 extrudes the second push plate 1005 through the fourth cavity 10022, the second push plate 1005 drives the first push plate 1003 to move upwards through the connecting rod 1004, the middle part of the isolation diaphragm 1006 gradually bulges upwards, when the isolation diaphragm 1006 deforms and recovers (deformation under the pressure of 0.75 Mpa), the first push plate 1003 does not move upwards any more, after the spring 803 resets, the sliding plate 704 drives the push plate 804 to move upwards through the spring 803, the pressure between the push plate 804 and the first push plate 1003 is reduced, the one-way valve in the through hole of the push plate 804 is opened, sodium hydroxide solution in the first cavity 402 enters the quantitative cavity 4031 through the through hole of the push plate 804, when the sliding plate 704 moves to the upper side of the reciprocating screw 702, the push plate 804 returns to the initial position, and the steps are repeated continuously to supplement the sodium hydroxide solution into the mixed shell 2 along with the rotation of the reciprocating screw 702, and the content of the sodium hydroxide solution in the mixed shell 2 is equal to the volume of the quantitative cavity 4031 every time.
Along with the rotation of stirring leaf 603, stirring leaf 603 drives porous bracing piece and rotates, has increased the area of contact of stirring leaf 603 with the material, accelerate the reaction rate of paranitrochlorobenzene and sodium hydroxide solution, improve the production efficiency of paranitrosodium nitrophenolate, because sodium hydroxide solution and paranitrochlorobenzene can't guarantee even mixed speed, consequently, hydrolysis reaction is not at uniform velocity, lead to sodium hydroxide solution and paranitrochlorobenzene to appear intermittent type reaction, cause temperature and pressure in mixing housing 2 to increase suddenly or suddenly drop (when sodium hydroxide solution and paranitrochlorobenzene are unreactive, the temperature can slowly drop in the mixing housing 2), the instantaneous temperature variation when temperature sensor 3 can't directly detect the material reaction, the reason has two: firstly, the temperature after the reaction of the materials needs to be conducted to the temperature sensor 3 after a period of time, secondly, the temperature in the mixing shell 2 is suddenly increased to be increased in a small extent, and the accuracy of the temperature sensor 3 is limited, so that when the temperature in the mixing shell 2 is suddenly increased, the temperature in the mixing shell 2 is required to be reduced in a small extent, and the temperature and the pressure in the mixing shell 2 are in a linear relation, and therefore, when the pressure in the mixing shell 2 is increased, the temperature is reduced, and the specific operation is as follows:
when the pressure in the mixing housing 2 suddenly increases, the isolating diaphragm 1006 senses the pressure change of the solution in the mixing housing 2, the isolating diaphragm 1006 protrudes upward to press the gas in the fourth cavity 10022, the gas in the fourth cavity 10022 moves upward to press the second push plate 1005, the second push plate 1005 moves upward to enable the gas in the third cavity 10021 to enter the lower side of the first push plate 1003 in the second cavity 403 through the guide tube 1001, the second push plate 1005 drives the first push plate 1003 to move upward (to be offset from the position at the pressure of 0.75 Mpa) through the connecting rod 1004, when the push plate 804 and the first push plate 1003 move upward to reset at the same time, the distance of the upward movement of the first push plate 1003 is further, therefore, the volume of the dosing cavity 4031 is reduced, the content of the sodium hydroxide solution entering the second cavity 403 from the first cavity 402 is reduced, when the push plate 804 moves downward again, the sodium hydroxide solution in the quantitative cavity 4031 is discharged, so that the content of sodium hydroxide participating in the hydrolysis reaction is reduced, the heat released by the hydrolysis reaction is reduced, because the temperature in the mixing shell 2 is in a state of being temporarily increased, the temperature in the mixing shell 2 is not reduced before the sodium hydroxide solution is added for the second time, therefore, the temperature in the mixing shell 2 is ensured to be stable before the sodium hydroxide solution is added for the third time through the neutralization of the two times, and similarly, when the pressure in the mixing shell 2 is suddenly reduced, the deformation of the isolating diaphragm 1006 is reduced, the volume of the quantitative cavity 4031 is increased, so that the content of sodium hydroxide participating in the hydrolysis reaction is increased, the heat released by the hydrolysis reaction is increased, and in sum, the amount of sodium hydroxide added into the mixing shell 2 is reduced by detecting the pressure change in the mixing shell 2, so that the pressure and the temperature in the mixing shell 2 are dynamically adjusted, the temperature sensor 3 can not detect the temperature change in real time, and the pressure and the temperature in the mixed shell 2 can be regulated and controlled further in a small range.
Example 2: on the basis of embodiment 1, as shown in fig. 6 and 7, the device further comprises a protection component, the protection component is arranged on the detection housing 1002, the protection component is used for protecting the isolation diaphragm 1006, the protection component comprises a sliding disk 1007, an annular groove is arranged at the lower part in the detection housing 1002, the sliding disk 1007 is slidably connected in the annular groove of the detection housing 1002, the sliding disk 1007 is positioned at the lower side of the isolation diaphragm 1006, the sliding disk 1007 is made of a corrosion-resistant material and is used for prolonging the service life of the sliding disk 1007, the isolation diaphragm 1006 and the sliding disk 1007 are matched to form a fifth cavity 10023, and the fifth cavity 10023 is filled with a protection liquid, so that the isolation diaphragm 1006 is prevented from being in direct contact with a solution.
Because the solution in the mixing housing 2 is sodium hydroxide, and is in an alkaline environment, in order to avoid that the isolation diaphragm 1006 is directly contacted with the solution in the mixing housing 2, the service life of the isolation diaphragm 1006 in the alkaline environment is reduced for a long time, therefore, when the pressure in the mixing housing 2 changes, the sliding disk 1007 senses and slides up and down, the sliding disk 1007 drives the protective liquid in the fifth cavity 10023 to flow, so that the isolation diaphragm 1006 deforms, the isolation diaphragm 1006 is prevented from being directly contacted with the solution, the sliding disk 1007 is made of corrosion-resistant materials, the service life of the sliding disk 1007 is prolonged, the cost of the isolation diaphragm 1006 is high, the sliding disk 1007 is directly replaced when the sliding disk 1007 needs to be replaced, and the isolation diaphragm 1006 does not need to be replaced.
It will be appreciated by persons skilled in the art that the above embodiments are not intended to limit the invention in any way, and that all technical solutions obtained by means of equivalent substitutions or equivalent transformations fall within the scope of the invention.
Claims (5)
1. The utility model provides a paranitrophenol sodium apparatus for producing with automatic temperature control function, including landing leg (1), landing leg (1) are provided with control terminal, landing leg (1) rigid coupling has mixed casing (2), mixed casing (2) are provided with inlet (201) and leakage fluid dram (202), all be provided with the solenoid valve that is connected with control terminal electricity in inlet (201) and the leakage fluid dram (202), mixed casing (2) are provided with discharge valve (203) that are connected with control terminal electricity, temperature sensor (3) and pressure sensor, the inside of mixed casing (2) is inlayed and is had the heating part that is connected with control terminal electricity, characterized in that, through backup pad rigid coupling in mixed casing (2), mixed casing (2) rigid coupling has communicating pipe (5) with feed casing (4) intercommunication, one side that feed casing (4) kept away from communicating pipe (5) is provided with outlet (401) of equidistant distribution of circumference, landing leg (1) are provided with the rabbling mechanism that is used for accelerating the mixed speed of paranitrochlorobenzene and sodium hydroxide, through outlet (5), feed casing (4) and outlet (401) are added gradually to mixed casing (2) in the mixed casing temperature of sodium hydroxide at 75.168, mixed solution temperature is maintained at a small amount of temperature in mixed casing (2);
the stirring mechanism comprises a servo motor (601), the servo motor (601) is fixedly connected to the supporting leg (1), the servo motor (601) is electrically connected with the control terminal, an output shaft of the servo motor (601) is fixedly connected with a rotating shaft (602) which is rotationally connected with the mixing shell (2), the rotating shaft (602) is fixedly connected with stirring blades (603) which are distributed at equal intervals in the circumferential direction, and the stirring blades (603) which are distributed at equal intervals in the circumferential direction are all provided with discharging components for quantitatively discharging sodium hydroxide solution in the feeding shell (4);
the discharging part comprises a gear ring (701), the gear ring (701) is fixedly connected with stirring blades (603) distributed at equal intervals in the circumferential direction, the mixing shell (2) is rotationally connected with a reciprocating screw (702), the reciprocating screw (702) is fixedly connected with a gear (703) meshed with the gear ring (701), the reciprocating screw (702) is in threaded connection with a sliding plate (704), the sliding plate (704) is provided with an adjusting component, and the adjusting component is used for adjusting the discharging speed of sodium hydroxide solution in the feeding shell (4);
the adjusting component comprises a sliding rod (801), the sliding rod (801) is fixedly connected to a sliding plate (704), the sliding rod (801) is in sliding connection with a feeding shell (4), the feeding shell (4) is in sliding connection with a limiting pipe (802), the sliding rod (801) is in sliding connection with the limiting pipe (802), a spring (803) is fixedly connected between the sliding plate (704) and the limiting pipe (802), a pushing disc (804) fixedly connected with the limiting pipe (802) is in sliding connection with the feeding shell (4), the pushing disc (804) is in sliding connection with the sliding rod (801), the pushing disc (804) is used for dividing the feeding shell (4) into a first cavity (402) and a second cavity (403), the second cavity (403) is communicated with the water outlet (401), the longitudinal length of the pushing disc (804) is larger than that of the water outlet (401), a through hole is formed in the pushing disc (804), a one-way valve is formed in the through hole of the pushing disc (804), the feeding shell (4) is provided with a plugging component for sealing the water outlet (401), and the feeding shell (4) is provided with a detecting component for detecting pressure change in the mixing shell (2).
The plugging assembly comprises a rotating ring (901), the rotating ring (901) is rotationally connected to the charging shell (4), an L-shaped rod (902) is fixedly connected to the rotating ring (901), a sliding groove (8011) which is slidably connected with the L-shaped rod (902) is formed in the sliding rod (801), the lower portion of the sliding groove (8011) is vertical, and the upper portion of the sliding groove (8011) is inclined; the feeding shell (4) is fixedly connected with limiting blocks (404) which are distributed at equal intervals in the circumferential direction, one side, far away from the feeding shell (4), of each limiting block (404) is provided with an arc-shaped surface, each limiting block (404) is provided with a through hole communicated with an adjacent water outlet (401), the rotating ring (901) is fixedly connected with extrusion blocks (903) which are distributed at equal intervals in the circumferential direction, and the extrusion blocks (903) are in sealing fit with the arc-shaped surfaces of the adjacent limiting blocks (404);
the detection assembly comprises a guide pipe (1001), the guide pipe (1001) is fixedly connected to a feeding shell (4) and is communicated with a second cavity (403), the guide pipe (1001) is communicated with a detection shell (1002), a first push plate (1003) is connected in a sliding mode in the second cavity (403), the first push plate (1003), a push plate (804) and the feeding shell (4) are matched to form a quantitative cavity (4031), a connecting rod (1004) located in the guide pipe (1001) is fixedly connected to the first push plate (1003), a second push plate (1005) fixedly connected with the connecting rod (1004) is connected in a sliding mode in the detection shell (1002), an isolation membrane (1006) located on the lower side of the second push plate (1005) is arranged in the detection shell (1002), a third cavity (10021) is formed in a matching mode in the second push plate (1005), and the second push plate (1005), the isolation membrane (1006) and the detection shell (1002) are matched to form a fourth cavity (10022).
2. The device for producing sodium paranitrophenolate with automatic temperature control function according to claim 1, wherein the stirring blade (603) is provided with a porous supporting rod for increasing the contact area between the stirring blade (603) and the solution.
3. The device for producing sodium paranitrophenolate with automatic temperature control function according to claim 1, wherein the extrusion block (903) is made of an elastic material, so as to increase the contact area between the extrusion block (903) and the limiting block (404).
4. The device for producing sodium paranitrophenolate with automatic temperature control function according to claim 1, further comprising a protection component, wherein the protection component is arranged on the detection housing (1002), the protection component is used for protecting the isolation diaphragm (1006), the protection component comprises a sliding disk (1007), the detection housing (1002) is provided with an annular groove, the sliding disk (1007) is slidably connected in the annular groove of the detection housing (1002), the isolation diaphragm (1006) and the sliding disk (1007) are matched to form a fifth cavity (10023), and the fifth cavity (10023) is filled with a protection liquid.
5. The apparatus for producing sodium paranitrophenolate with automatic temperature control function according to claim 4, wherein the sliding plate (1007) is made of corrosion-resistant material for increasing the service life of the sliding plate (1007).
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Address after: No. 63, Mingyuan Road, Blue Economic Development Zone, Hekou District, Dongying City, Shandong Province 257200 Patentee after: SHANDONG GUANSEN POLYMERS MATERIALS SCIENCE AND TECHNOLOGY Inc. Address before: 257000 New Material Industrial Park, Dongying Port Economic Development Zone, Dongying City, Shandong Province Patentee before: SHANDONG GUANSEN POLYMERS MATERIALS SCIENCE AND TECHNOLOGY Inc. |
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Denomination of invention: A production device for sodium p-nitrophenol with automatic temperature control function Effective date of registration: 20231109 Granted publication date: 20230602 Pledgee: Dongying Hekou District sub branch of China Post Savings Bank Co.,Ltd. Pledgor: SHANDONG GUANSEN POLYMERS MATERIALS SCIENCE AND TECHNOLOGY Inc. Registration number: Y2023980065013 |