CN117126057B - Synthesis process and synthesis system for continuously synthesizing paranitroaniline - Google Patents
Synthesis process and synthesis system for continuously synthesizing paranitroaniline Download PDFInfo
- Publication number
- CN117126057B CN117126057B CN202311091352.8A CN202311091352A CN117126057B CN 117126057 B CN117126057 B CN 117126057B CN 202311091352 A CN202311091352 A CN 202311091352A CN 117126057 B CN117126057 B CN 117126057B
- Authority
- CN
- China
- Prior art keywords
- stirring
- barrel
- paranitroaniline
- synthesis
- baffle plate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- TYMLOMAKGOJONV-UHFFFAOYSA-N 4-nitroaniline Chemical compound NC1=CC=C([N+]([O-])=O)C=C1 TYMLOMAKGOJONV-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 34
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 34
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 16
- 230000008569 process Effects 0.000 title claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 58
- 238000006243 chemical reaction Methods 0.000 claims abstract description 44
- 230000007246 mechanism Effects 0.000 claims abstract description 32
- 238000001914 filtration Methods 0.000 claims abstract description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000004140 cleaning Methods 0.000 claims abstract description 9
- 239000000047 product Substances 0.000 claims abstract description 9
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- CZGCEKJOLUNIFY-UHFFFAOYSA-N 4-Chloronitrobenzene Chemical compound [O-][N+](=O)C1=CC=C(Cl)C=C1 CZGCEKJOLUNIFY-UHFFFAOYSA-N 0.000 claims abstract description 7
- 208000005156 Dehydration Diseases 0.000 claims abstract description 6
- 230000018044 dehydration Effects 0.000 claims abstract description 6
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 6
- 238000005576 amination reaction Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 4
- 239000006227 byproduct Substances 0.000 claims abstract description 4
- 230000005540 biological transmission Effects 0.000 claims description 24
- 238000007789 sealing Methods 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 5
- 238000004806 packaging method and process Methods 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 230000000903 blocking effect Effects 0.000 claims description 3
- 230000006698 induction Effects 0.000 claims description 3
- 238000000926 separation method Methods 0.000 abstract description 7
- 230000033001 locomotion Effects 0.000 description 5
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005915 ammonolysis reaction Methods 0.000 description 2
- 229920006231 aramid fiber Polymers 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 239000004760 aramid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 210000001503 joint Anatomy 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/04—Preparation of compounds containing amino groups bound to a carbon skeleton by substitution of functional groups by amino groups
- C07C209/06—Preparation of compounds containing amino groups bound to a carbon skeleton by substitution of functional groups by amino groups by substitution of halogen atoms
- C07C209/10—Preparation of compounds containing amino groups bound to a carbon skeleton by substitution of functional groups by amino groups by substitution of halogen atoms with formation of amino groups bound to carbon atoms of six-membered aromatic rings or from amines having nitrogen atoms bound to carbon atoms of six-membered aromatic rings
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/82—Purification; Separation; Stabilisation; Use of additives
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention discloses a synthesis process and a synthesis system for continuously synthesizing paranitroaniline, which comprise the following steps: s2, amination: p-nitrochlorobenzene is added into a high-pressure reaction kettle, and stirring and mixing are carried out. S3, stirring and washing: adding condensed water into the high-pressure reaction kettle, and stirring and cleaning; s4, filtering: the stirring mechanism arranged in the internal high-pressure reaction kettle reversely rotates to realize that the filter holes of the bearing cylinder are opened to filter condensed water and byproducts ammonium chloride; s5, centrifuging: reversely rotating the stirring mechanism, and increasing the rotating speed to carry out centrifugal dehydration treatment; according to the synthesis process and the synthesis system for continuously synthesizing the paranitroaniline, provided by the invention, by adding the separation device, the synthesized paranitroaniline can be immediately subjected to centrifugal treatment after being washed, and the product can be dehydrated more quickly, namely, the synthesis quality and the synthesis efficiency of the paranitroaniline can be greatly improved.
Description
Technical Field
The invention relates to the technical field of paranitroaniline production, in particular to a synthesis process and a synthesis system for continuously synthesizing paranitroaniline.
Background
Along with the development of technology, the p-nitroaniline is an important organic chemical raw material in the aspect of chemical industry, and can be used as an intermediate of an anti-aging agent, a dye and a pesticide, wherein the p-phenylenediamine is also an important function, and then the p-phenylenediamine is used for synthesizing novel high-tech synthetic fibers, aramid fibers, and the demand of the p-nitroaniline is also kept to be rapidly increased along with the production of the aramid fiber project. The synthesis method of the paranitroaniline has various synthesis modes, wherein the paranitroaniline is synthesized by ammonia amination in common use, and the method has high efficiency and high yield.
The patent issued to China has publication No. CN109516921B, and is named as a method for preparing paranitroaniline, and the patent adopts a twice ammonolysis mode to completely react paranitrochlorobenzene to obtain the paranitroaniline of which the purity is more than 99.90 percent, so that the preparation purity of the paranitroaniline is integrally improved.
The prior art has the following defects: in the prior art, when synthesizing paranitroaniline, for example, the above patent, although the reaction completion degree of paranitroaniline is improved by synthesizing through two ammonolysis reactions, when specifically using, in order to improve the purity, the product is required to be washed with water, so that the water content of the product is increased, which affects the subsequent use and the subsequent efficiency and purity of paraphenylenediamine.
Disclosure of Invention
The invention aims to provide a synthesis process and a synthesis system for continuously synthesizing paranitroaniline, which solve the defects in the prior art.
In order to achieve the above object, the present invention provides the following technical solutions:
a synthesis process and a synthesis system for continuously synthesizing paranitroaniline: the method comprises the following steps:
s1, preparing ammonia water: adding liquid ammonia water and condensed water into a bearing cylinder of a high-pressure reaction kettle, and mixing;
s2, amination: adding p-nitrochlorobenzene in a high-pressure reaction kettle, stirring and mixing at 180-200 ℃.
S3, stirring and washing: adding condensed water into the high-pressure reaction kettle, and stirring and cleaning;
s4, filtering: the stirring mechanism arranged in the internal high-pressure reaction kettle reversely rotates to realize that the filter holes of the bearing cylinder are opened to filter condensed water and byproducts ammonium chloride;
s5, centrifuging: reversely rotating the stirring mechanism, and increasing the rotating speed to carry out centrifugal dehydration treatment;
s6, drying: drying the generated paranitroaniline;
s7, packaging: the resulting product is individually packaged.
In a further preferable embodiment of the present invention, in the step S2, p-nitrochlorobenzene is added and stirred for a period of 12 to 14 hours.
In a further preferable embodiment of the present invention, in the step S3, the pressure relief treatment is performed on the autoclave.
The synthesis system for continuously synthesizing the paranitroaniline is applied to the synthesis process for continuously synthesizing the paranitroaniline, and comprises a reaction cylinder, wherein the reaction cylinder is internally provided with the stirring mechanism;
a bearing mechanism is further arranged in the reaction cylinder, and the bearing mechanism is provided with a first stroke and a second stroke;
on the first stroke, the bearing mechanism rotates to be matched with stirring for stirring;
and on the second stroke, the bearing mechanism reversely rotates to realize filtration.
In a further preferable scheme of the invention, the bearing mechanism comprises a second barrel rotatably arranged in the reaction barrel, a first barrel is rotatably arranged in the second barrel, a first filtering hole is formed in the first barrel, a second filtering hole is formed in the second barrel, and the first filtering hole and the second filtering hole are correspondingly arranged;
an elastic piece is arranged between the first barrel and the second barrel, and the second barrel seals each first filtering hole under the elasticity of the elastic piece.
In a further preferable scheme of the invention, the elastic pieces are multiple in number and uniformly distributed on the first barrel, the elastic pieces comprise fixed blocks fixedly arranged on the first barrel and third elastic pieces, one ends of the third elastic pieces are fixedly connected to the fixed blocks, and the other ends of the third elastic pieces are arranged on the groove walls of the guide grooves formed in the second barrel.
In a further preferable scheme of the invention, the stirring mechanism is fixedly arranged on a fixed column in the reaction cylinder and is used for stirring the materials in the first barrel when the stirring mechanism is in a vertical state.
In a further preferable scheme of the invention, a sealing cover is movably arranged on the induction cylinder, the shifting baffle is connected to a rotating shaft of the sealing cover through a transmission piece in a transmission way, when the sealing cover is opened, the shifting baffle is driven to be in a horizontal state through the transmission piece, a flow hole is formed in the shifting baffle, a sliding baffle for blocking the flow hole is arranged on the shifting baffle in a sliding way, and a plurality of holes matched with the flow hole are formed in the sliding baffle; when the poking baffle is in a horizontal state, the sliding baffle is extruded by the extrusion piece so that the holes on the sliding baffle correspond to the flow holes.
In a further preferable aspect of the present invention, the pressing member includes a protruding shaft fixedly provided on the fixing column, and one end of the sliding damper is fixedly provided with a fixing stopper, and one end of the fixing stopper abuts against a side wall of the protruding shaft.
In a further preferred scheme of the invention, the transmission member comprises a plurality of transmission belts fixedly arranged in the reaction cylinder, wherein one transmission belt is sleeved on the rotating shaft of the sealing cover, and the other transmission belt is sleeved on a belt pulley arranged on the rotating shaft.
In the technical scheme, the synthesis process and the synthesis system for continuously synthesizing the paranitroaniline have the beneficial effects that:
according to the invention, the separation step is added in the synthesis step, and the separation device is added, so that the synthesized paranitroaniline can be immediately subjected to centrifugal treatment without independently arranging the dehydration device after being washed, and the product can be dehydrated more quickly and rapidly, namely, the synthesis quality and the synthesis efficiency of the paranitroaniline can be greatly improved.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the disclosure.
This document provides an overview of various implementations or examples of the technology described in this disclosure, and is not a comprehensive disclosure of the full scope or all of the features of the disclosed technology.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments described in the present invention, and other drawings may be obtained according to these drawings for a person having ordinary skill in the art.
FIG. 1 is a schematic flow chart of a synthetic process for synthesizing paranitroaniline according to an embodiment of the present invention;
FIG. 2 is a schematic structural view of a reaction cylinder according to an embodiment of the present invention;
FIG. 3 is a schematic structural diagram of a reaction cylinder and a carrying mechanism according to an embodiment of the present invention;
FIG. 4 is a schematic cross-sectional view of a reaction cartridge according to an embodiment of the present invention;
FIG. 5 is a schematic view of the internal structure of a reaction cylinder according to an embodiment of the present invention;
FIG. 6 is a schematic diagram of the structure of a first barrel and a second barrel according to an embodiment of the present invention;
fig. 7 is an enlarged schematic view of a structure at a according to an embodiment of the present invention;
fig. 8 is a schematic structural view of a fixing post and a poking baffle according to an embodiment of the present invention;
FIG. 9 is a schematic diagram of a structure of a shifting plate and a rotating shaft according to an embodiment of the present invention;
FIG. 10 is a schematic cross-sectional view of a baffle plate according to an embodiment of the present invention;
FIG. 11 is a schematic view of a sliding panel according to an embodiment of the present invention;
FIG. 12 is a schematic cross-sectional view of a second barrel and a first barrel according to an embodiment of the present invention;
fig. 13 is an enlarged schematic view of a B-site structure according to an embodiment of the present invention.
Reference numerals illustrate:
1. a reaction cylinder; 11. sealing cover; 101. a liquid container; 111. a drive belt; 12. fixing the column; 21. a first barrel; 2101. a first filter aperture; 2201. a second filter aperture; 22. a second tub; 221. a sliding guide wheel; 222. a guide post; 2221. a first elastic member; 2222. a locking block; 223. a tightening block; 2231. a second elastic member; 224. a third elastic member; 1111. a transmission guide groove; 13. a support frame; 131. a carrying groove; 211. a fixed block; 2202. a guide groove; 2203. a locking hole; 4. a baffle plate; 41. a sliding baffle; 4101. a flow hole; 42. a rotating shaft; 401. a flow channel; 411. a fixed stop block; 121. a protruding shaft; 4011. and (3) a hole.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present disclosure more apparent, the technical solutions of the embodiments of the present disclosure will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present disclosure. It will be apparent that the described embodiments are some, but not all, of the embodiments of the present disclosure. All other embodiments, which can be made by one of ordinary skill in the art without the need for inventive faculty, are within the scope of the present disclosure, based on the described embodiments of the present disclosure.
1-13, a synthesis process for continuously synthesizing paranitroaniline comprises the following steps:
s1, preparing ammonia water: adding liquid ammonia water and condensed water into a bearing cylinder of a high-pressure reaction kettle, and mixing;
s2, amination: adding p-nitrochlorobenzene in a high-pressure reaction kettle, stirring and mixing at 180-200 ℃.
S3, stirring and washing: adding condensed water into the high-pressure reaction kettle, and stirring and cleaning;
in this step, stir the pressure release, then wash through the comdenstion water, and when wasing, the material is in motion all the time, promptly, the material that is in dynamic state can carry out more even and comdenstion water and contact, can wash more even.
S4, filtering: the stirring mechanism arranged in the internal high-pressure reaction kettle reversely rotates to realize that the filter holes of the bearing cylinder are opened to filter condensed water and byproducts ammonium chloride;
s5, centrifuging: reversely rotating the stirring mechanism, and increasing the rotating speed to carry out centrifugal dehydration treatment;
s6, drying: and drying the generated paranitroaniline.
S7, packaging: packaging the formed products individually;
according to the invention, the separation step is added in the synthesis step, and the separation device is added, so that the synthesized paranitroaniline can be immediately subjected to centrifugal treatment without independently arranging the dehydration device after being washed, and the product can be dehydrated more quickly and rapidly, namely, the synthesis quality and the synthesis efficiency of the paranitroaniline can be greatly improved.
In a further embodiment of the present invention, in step S2, p-nitrochlorobenzene is added for a stirring and mixing time of 12 to 14 hours.
In a further embodiment of the present invention, in step S3, the pressure relief treatment is performed on the autoclave. Specifically, after stirring is finished and cleaning is needed, the pressure relief treatment is needed for the high-pressure reaction kettle, and then the cleaning and filtering are performed by spraying condensed water, so that the cleaning effect can be greatly improved.
Furthermore, the invention also provides a synthesis system which is applied to the synthesis process and the synthesis system for continuously synthesizing the paranitroaniline, and comprises a reaction cylinder 1, wherein a stirring mechanism is arranged in the reaction cylinder 1;
a bearing mechanism is also arranged in the reaction cylinder 1 and is provided with a first stroke and a second stroke;
on the first stroke, the bearing mechanism rotates to stir in cooperation with stirring;
on the second stroke, the bearing mechanism rotates reversely to realize filtration. According to the invention, through the arrangement of the bearing mechanism and the stirring mechanism, two strokes can be provided in the movement stroke, namely, the effects of continuous stirring and filtering centrifugation can be respectively realized, and the steps of stirring, filtering washing centrifugation and the like can be realized without changing the barrel body, so that the functionality of the device is greatly improved.
In the scheme provided by the invention, the bearing mechanism comprises a second barrel 22 rotatably arranged in the reaction barrel 1, a first barrel 21 is rotatably arranged in the second barrel 22, a first filter hole 2101 is formed in the first barrel, a second filter hole 2201 is formed in the second barrel 22, and the first filter hole 2101 and the second filter hole 2201 are correspondingly arranged;
in a further embodiment of the present invention, an elastic member is disposed between the first tub 21 and the second tub 22, and the second tub 22 seals each of the first filtering holes 2101 under the elastic force of the elastic member. Specifically, the second barrel 22 seals each of the first filtering holes 2101 under the elastic force of the elastic member, that is, in the initial state, the first filtering holes 2101 are in a sealed state and cannot circulate.
In a further embodiment of the present invention, the number of elastic members is plural and is uniformly distributed on the first barrel 21, the elastic members include a fixed block 211 fixedly disposed on the first barrel 21 and a third elastic member 224, one end of the third elastic member 224 is fixedly connected to the fixed block 211, and the other end is disposed on a groove wall of the guide groove 2202 formed in the second barrel 22.
Further, a sliding guide wheel 221 is fixedly disposed on the outer wall of the second barrel 22, and one end of the sliding guide wheel 221 abuts against a transmission guiding groove 1111 formed on the inner wall of the reaction barrel 1.
In a further embodiment of the present invention, the stirring mechanism is fixedly arranged on the fixed column 12 in the reaction cylinder 1 and rotates the stirring baffle 4 arranged on the fixed column 12, so as to stir the material in the first barrel 21 when the stirring baffle 4 is in a vertical state. In particular, the deflector 4 may be substantially vertical, with a certain angular deviation being equally suitable, as long as it forms an angle in contact with the material.
In a further provided embodiment of the present invention, a sealing cover 11 is movably disposed on the induction cylinder, and the stirring baffle 4 is connected to a rotating shaft of the sealing cover 11 through a transmission member in a transmission manner, when the sealing cover 11 is opened, the stirring baffle 4 is driven to be in a horizontal state through the transmission member, a circulation channel 401 is disposed on the stirring baffle 4, a flow hole 4011 is disposed on the circulation channel 401, a sliding baffle 41 for blocking the flow hole 4011 is slidingly disposed on the stirring baffle 4, and a plurality of holes 4101 adapted to the flow hole 4011 are disposed on the sliding baffle 41; when the toggle plate 4 is in the horizontal state, the slide damper 41 is pressed by the pressing member so that the hole 4101 on the slide damper 41 corresponds to the flow hole 4011. Specifically, a spring is disposed between the sliding baffle 41 and the toggle baffle 4, and the elastic force of the spring makes the sliding baffle 41 and the flow hole 4011 on the toggle baffle 4 staggered when the fixed baffle 411 does not contact the protruding portion, so that the sliding baffle 41 blocks the fixed baffle 411, and the flow hole 4011 is blocked, that is, when stirring, materials can be prevented from entering the flow hole 4011, and the functionality of the device is improved.
In a further embodiment of the present invention, the pressing member includes a protruding shaft 121 fixedly disposed on the fixed column 12, and one end of the sliding damper 41 is fixedly provided with a fixed stop 411, and one end of the fixed stop 411 abuts against a side wall of the protruding shaft 121.
Specifically, when the dial plate 4 is in a horizontal state, the sliding plate 41 and the flow hole 4011 can be made to flow through the extrusion of the protruding shaft 121 and the fixed stopper 411, and then the flow hole 4011 is communicated with the condensate water inlet pipe in a butt joint manner, so that the functionality of the device can be improved. When the baffle plate 4 is in a horizontal state, condensed water flows into the first barrel 21 through the flow holes 4011, so that the cleaning of products is facilitated.
In a further embodiment of the present invention, the transmission member includes a plurality of transmission belts 111 fixedly disposed in the reaction cylinder 1, wherein one transmission belt 111 is sleeved on the rotating shaft of the sealing cover 11, and the other transmission belt 111 is sleeved on a pulley disposed on the rotating shaft 42.
Specifically, the driving belt 111 that this application set up is at its main power of transmission, and the power of rotation of sealed lid 11 is carried to the power of rotation on the baffle plate 4 through driving belt 111 to drive baffle plate 4 and take place to rotate, and the redest rotates to the horizontality.
In order to improve the stability of the first barrel 21 and the second barrel 22 during separation, in this embodiment, an elastic fixing member is further provided, the elastic fixing member includes a locking block 2222 slidably disposed in the guide post 222, a locking hole 2203 is formed in an inner wall of the guide groove 2202, the locking hole 2203 is adapted to the locking block 2222, a second elastic member 2231 is further provided in the locking hole 2203, one end of the second elastic member 2231 is fixedly connected with a tightening block 223, the tightening block 223 is slidably disposed in the locking hole 2203, and an inclined surface is formed at one end of the tightening block 223.
Specifically, when in use, firstly liquid ammonia water and condensed water are added into a bearing cylinder of a high-pressure reaction kettle to be mixed, then stirring is carried out, at this time, a reaction cover of the reaction cylinder 1 is in a closed state, then the interior is vacuumized, at this time, a baffle plate 4 is basically in a vertical state, then a driving device is started, specifically, the driving device is a driving motor arranged on a supporting frame 13, an output shaft of the driving motor is fixedly arranged on a second cylinder, then the driving motor is arranged in a bearing groove 131 formed on the supporting frame 13, then the driving motor drives the second cylinder 22 and the first cylinder 21 to start rotating, when in rotation, the first cylinder 21 and the second cylinder 22 are relatively fixed, namely, as shown in fig. 12, the rotation direction is to the left, the rotation direction is to the direction of a third elastic piece 224, a guide post 222 is abutted against the side wall of the guide groove 2202, the first filter holes 2101 and the second filter holes 2201 are staggered at this time, namely, the first filter holes 2101 can be plugged by the second barrel 22, so that the material is always in the first barrel 21, then the material is matched with the baffle plate 4, stirring is realized, after stirring for a certain time, the material is decompressed and cleaned, then the sealing cover 11 is opened, the sealing cover 11 drives the driving belt 111 to move, the driving belt 111 drives the baffle plate 4 to be in a basically horizontal state, then after being in the horizontal state, the fixed stop blocks 411 arranged on the sliding baffle plate 41 are abutted against the protruding parts on the protruding shafts 121, then the holes on the sliding baffle plate 41 are corresponding to the flow holes 4011, so that the sliding baffle plate 41 is communicated with the flow holes 4011, then the flow holes 4011 are communicated with the condensed water inlet pipe, and then condensed water can be introduced for cleaning, then, when the filtering separation is performed, the driving motor is rotated reversely, as shown in fig. 12, with the third elastic member 224 and the guide post 222 as reference, to rotate in the direction of the guide post 222, and then the first barrel 21 and the second barrel 22 are rotated relatively under the action of inertia, that is, the guide post 222 is driven to rotate relative to the second barrel 22, and then the guide post 222 is gradually moved in the direction of the third elastic member 224, and then the guide post 222 is gradually driven to move in the direction of the locking hole 2203 during the movement, finally, the locking block 2222 is moved towards the direction corresponding to the locking hole 2203, then falls into the locking hole 2203, then the locking block 2222 is moved downwards under the elastic force of the first elastic member 2221, and is inserted into the locking hole 2203, that is, the movement of the locking block 2222 can be limited, that is, the movement of the guide post 222 can be limited, at this time, the first barrel 21 and the second barrel 22 are relatively fixed, the first filtering holes 2101 and the second filtering holes 2201 formed in the first barrel 21 and the second barrel 22 correspond to each other, that is, the first filtering circulation can be achieved, then the first barrel 21 and the second barrel 22 synchronously and rapidly rotate under high-speed rotation, then the moisture in the first barrel 21 is centrifuged out, the moisture of paranitroaniline is greatly reduced, the synthetic quality and the synthetic efficiency are greatly improved, then after centrifugation is finished, the driving device stops rotating, after rotation is stopped on the first barrel 21 and the second barrel 22, due to the effect of inertia, the abutting block 223 is made to have inertia, then the abutting block 223 is driven to move towards the opening of the locking hole 2203, then the inclined surface formed on the abutting block 223 can press the locking block 2222, the inclined surface of the locking block 2222 presses the locking block 2222, the locking block 2222 gradually protrudes out of the locking hole 2203, then, under the elastic force of the second elastic member 2231, the locking block 2222 rotates relative to the second barrel 22, that is, drives the first barrel 21 to rotate, so that the first barrel 21 and the filtration Kong Xiangxiang on the second barrel 22 are staggered, so that the second barrel 22 seals the first filtration hole 2101, and finally the filtrate falls into the liquid containing tank 101.
While certain exemplary embodiments of the present invention have been described above by way of illustration only, it will be apparent to those of ordinary skill in the art that modifications may be made to the described embodiments in various different ways without departing from the spirit and scope of the invention. Accordingly, the drawings and description are to be regarded as illustrative in nature and not as restrictive of the scope of the invention, which is defined by the appended claims.
Claims (4)
1. A synthesis system for continuously synthesizing paranitroaniline, which is applied to a synthesis process for continuously synthesizing paranitroaniline, comprises the following steps:
s1, preparing ammonia water: adding liquid ammonia water and condensed water into a bearing cylinder of a high-pressure reaction kettle for mixing;
s2, amination: adding p-nitrochlorobenzene in a high-pressure reaction kettle, stirring and mixing at 180-200 ℃;
s3, stirring and washing: adding condensed water into the high-pressure reaction kettle, and stirring and cleaning;
s4, filtering: the stirring mechanism arranged in the internal high-pressure reaction kettle reversely rotates to realize that the filter holes of the bearing cylinder are opened to filter condensed water and byproducts ammonium chloride;
s5, centrifuging: reversely rotating the stirring mechanism, and increasing the rotating speed to carry out centrifugal dehydration treatment;
s6, drying: drying the generated paranitroaniline;
s7, packaging: the formed product is individually packaged and is characterized by comprising a reaction cylinder (1), wherein the stirring mechanism is arranged in the reaction cylinder (1);
a bearing mechanism is further arranged in the reaction cylinder (1), and the bearing mechanism is provided with a first stroke and a second stroke;
on the first stroke, the bearing mechanism rotates to be matched with stirring for stirring;
on the second stroke, the bearing mechanism reversely rotates to realize filtration;
the bearing mechanism comprises a second barrel (22) rotatably arranged in the reaction barrel (1), a first barrel (21) is rotatably arranged in the second barrel (22), a first filtering hole (2101) is formed in the first barrel (21), a second filtering hole (2201) is formed in the second barrel (22), and the first filtering hole (2101) and the second filtering hole (2201) are correspondingly arranged;
an elastic piece is arranged between the first barrel (21) and the second barrel (22), and the second barrel (22) seals each first filtering hole (2101) under the elastic force of the elastic piece;
the elastic pieces are uniformly distributed on the first barrel (21), each elastic piece comprises a fixed block (211) and a third elastic piece (224) which are fixedly arranged on the first barrel (21), one end of each third elastic piece (224) is fixedly connected to the corresponding fixed block (211), and the other end of each third elastic piece is arranged on the groove wall of a guide groove (2202) formed in the second barrel (22); the stirring mechanism is fixedly arranged on a fixed column (12) in the reaction cylinder (1) and is used for rotating a stirring baffle plate (4) arranged on the fixed column (12), and the stirring baffle plate (4) is used for stirring materials in the first barrel (21) when in a vertical state.
2. The synthesis system for continuously synthesizing paranitroaniline according to claim 1, wherein a sealing cover (11) is movably arranged on the induction cylinder, the stirring baffle plate (4) is connected to a rotating shaft of the sealing cover (11) through a transmission piece in a transmission way, when the sealing cover (11) is opened, the stirring baffle plate (4) is driven to be in a horizontal state through the transmission piece, a flow hole (4101) is formed in the stirring baffle plate (4), a sliding baffle plate (41) for blocking the flow hole is slidably arranged on the stirring baffle plate (4), and a plurality of holes matched with the flow hole (4101) are formed in the sliding baffle plate (41); when the toggle plate (4) is in a horizontal state, the slide damper (41) is pressed by the pressing member so that the hole on the slide damper (41) corresponds to the flow hole (4101).
3. A continuous synthesizing system for p-nitroaniline according to claim 2, wherein the pressing member includes a protruding shaft (121) fixedly provided on the fixed column (12), and one end of the sliding shutter (41) is fixedly provided with a fixed stopper (411), and one end of the fixed stopper (411) abuts against a side wall of the protruding shaft (121).
4. The system for continuously synthesizing paranitroaniline according to claim 1, wherein the transmission member comprises a plurality of transmission belts (111) fixedly arranged in the reaction cylinder (1), one transmission belt (111) is sleeved on a rotating shaft of the sealing cover (11), and the other transmission belt (111) is sleeved on a belt pulley arranged on the rotating shaft (42).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311091352.8A CN117126057B (en) | 2023-08-29 | 2023-08-29 | Synthesis process and synthesis system for continuously synthesizing paranitroaniline |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311091352.8A CN117126057B (en) | 2023-08-29 | 2023-08-29 | Synthesis process and synthesis system for continuously synthesizing paranitroaniline |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN117126057A CN117126057A (en) | 2023-11-28 |
| CN117126057B true CN117126057B (en) | 2024-03-15 |
Family
ID=88850433
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311091352.8A Active CN117126057B (en) | 2023-08-29 | 2023-08-29 | Synthesis process and synthesis system for continuously synthesizing paranitroaniline |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117126057B (en) |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2235376C1 (en) * | 2002-12-09 | 2004-08-27 | Государственное унитарное предприятие города Москвы - объединенный эколого-технологический и научно-исследовательский центр по обезвреживанию РАО и охране окружающей среды (ГУП МосНПО "Радон") | Thermochemical treatment plant for powdered and crushed combustible radioactive wastes |
| CN101343231A (en) * | 2008-08-21 | 2009-01-14 | 苏州市罗森助剂有限公司 | Production method of p-nitroaniline |
| CN102001952A (en) * | 2009-09-02 | 2011-04-06 | 南化集团研究院 | Preparation method of high-purity paranitroaniline |
| CN103420850A (en) * | 2013-07-19 | 2013-12-04 | 浙江闰土股份有限公司 | Continuous production method of paranitroaniline |
| CN106957231A (en) * | 2016-01-11 | 2017-07-18 | 江苏圣奥化学科技有限公司 | The preparation method of N, N '-bis- (alkyl)-p-phenylenediamine |
| CN107382747A (en) * | 2017-08-01 | 2017-11-24 | 安徽东至广信农化有限公司 | A kind of continuous ammonating process of phenyl amines organic intermediate |
| CN109516921A (en) * | 2018-11-12 | 2019-03-26 | 江苏扬农化工集团有限公司 | A method of preparing paranitroanilinum |
| CN210683725U (en) * | 2019-08-28 | 2020-06-05 | 兴国红天下山茶油有限公司 | Concentrated extraction equipment of camellia oil |
| CN215137394U (en) * | 2020-10-27 | 2021-12-14 | 贵州瓮福开磷氟硅新材料有限公司 | Silicon dioxide filtering and separating device for producing anhydrous hydrogen fluoride |
| CN114805082A (en) * | 2022-04-22 | 2022-07-29 | 浙江华亿工程设计股份有限公司 | Method for preparing nitroaniline by continuous convective ammoniation of nitrochlorobenzene |
-
2023
- 2023-08-29 CN CN202311091352.8A patent/CN117126057B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2235376C1 (en) * | 2002-12-09 | 2004-08-27 | Государственное унитарное предприятие города Москвы - объединенный эколого-технологический и научно-исследовательский центр по обезвреживанию РАО и охране окружающей среды (ГУП МосНПО "Радон") | Thermochemical treatment plant for powdered and crushed combustible radioactive wastes |
| CN101343231A (en) * | 2008-08-21 | 2009-01-14 | 苏州市罗森助剂有限公司 | Production method of p-nitroaniline |
| CN102001952A (en) * | 2009-09-02 | 2011-04-06 | 南化集团研究院 | Preparation method of high-purity paranitroaniline |
| CN103420850A (en) * | 2013-07-19 | 2013-12-04 | 浙江闰土股份有限公司 | Continuous production method of paranitroaniline |
| CN106957231A (en) * | 2016-01-11 | 2017-07-18 | 江苏圣奥化学科技有限公司 | The preparation method of N, N '-bis- (alkyl)-p-phenylenediamine |
| CN107382747A (en) * | 2017-08-01 | 2017-11-24 | 安徽东至广信农化有限公司 | A kind of continuous ammonating process of phenyl amines organic intermediate |
| CN109516921A (en) * | 2018-11-12 | 2019-03-26 | 江苏扬农化工集团有限公司 | A method of preparing paranitroanilinum |
| CN210683725U (en) * | 2019-08-28 | 2020-06-05 | 兴国红天下山茶油有限公司 | Concentrated extraction equipment of camellia oil |
| CN215137394U (en) * | 2020-10-27 | 2021-12-14 | 贵州瓮福开磷氟硅新材料有限公司 | Silicon dioxide filtering and separating device for producing anhydrous hydrogen fluoride |
| CN114805082A (en) * | 2022-04-22 | 2022-07-29 | 浙江华亿工程设计股份有限公司 | Method for preparing nitroaniline by continuous convective ammoniation of nitrochlorobenzene |
Also Published As
| Publication number | Publication date |
|---|---|
| CN117126057A (en) | 2023-11-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN117126057B (en) | Synthesis process and synthesis system for continuously synthesizing paranitroaniline | |
| CN114875600B (en) | Environment-friendly soaping-free active dyeing and finishing system and process for dyeing and finishing Roman cloth | |
| CN114789010A (en) | Modular raw materials turns over mixes device | |
| CN209630667U (en) | A kind of agitating device of P507 extraction box | |
| CN117160306B (en) | Mixer that permanent magnet motor directly drives | |
| CN214162572U (en) | Centrifugal grinding machine with changeable angle | |
| CN108689859B (en) | Production process of p-nitroaniline | |
| CN212504010U (en) | Automatic raw material impregnation tank with good sealing performance for graphite ring production | |
| CN1322818C (en) | Multi-rubbing-bucket fully-automatic tea kneading machine | |
| CN115139425A (en) | Rubber mixing and stirring equipment | |
| CN212663279U (en) | Production facility of yarn dyeing wax emulsion | |
| CN208713767U (en) | A kind of fixture processed for fixing motor housing | |
| CN110158250B (en) | Circulating quick printing and dyeing system | |
| CN110075731B (en) | Printing and dyeing raw material processing system | |
| CN202837064U (en) | Vacuum drying mixing device of coal samples | |
| CN208896287U (en) | A kind of color-mixture device | |
| CN115634749B (en) | Reducing mechanism is used in zinc laurate preparation | |
| CN205995303U (en) | A kind of wear-resistant kneading machine | |
| CN215713072U (en) | Sectional type leather tanning device | |
| CN221514376U (en) | Quantitative mixing device for synthetic fiber treating agent | |
| CN214234059U (en) | Conveniently get rid of lauroyl glutamic acid synthesizer of solvent | |
| CN221788911U (en) | Cleaning agent production and processing equipment | |
| CN221868171U (en) | Stirring device for manufacturing chemical products | |
| CN218741558U (en) | Gel raw material stirrer capable of mixing uniformly | |
| CN114851611B (en) | Processing method of bioengineering composite pipe with tea seed shells as raw material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |