CN210620664U - Continuous production equipment for 5-nitro salicylic acid - Google Patents
Continuous production equipment for 5-nitro salicylic acid Download PDFInfo
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- CN210620664U CN210620664U CN201921397948.XU CN201921397948U CN210620664U CN 210620664 U CN210620664 U CN 210620664U CN 201921397948 U CN201921397948 U CN 201921397948U CN 210620664 U CN210620664 U CN 210620664U
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Abstract
The utility model discloses a 5-nitrosalicylic acid's serialization production facility, this equipment include tertiary the cauldron of nitrifying, first the cauldron of nitrifying is equipped with salicylic acid solution dropwise add mouth, and first the cauldron of nitrifying, second nitration cauldron and third are nitrified the cauldron and all are equipped with mixed acid dropwise add mouth, agitating unit, press from both sides cover and cooling inner coil, and inner coil top, tertiary the inner wall average level of nitrifying the cauldron are equipped with the annular baffle, and the lateral wall that first the cauldron of nitrifying is located the annular baffle top is equipped with first overflow mouth, first overflow mouth pass through the pipeline with the feed inlet intercommunication of second nitration cauldron, the lateral wall that the cauldron is located the annular baffle top is nitrified to the second is equipped with the second overflow mouth, the second overflow mouth pass through the pipeline with the feed inlet intercommunication of the cauldron is nitrified to the third, and the lateral wall that the cauldron is located the annular baffle top all has the. The utility model discloses a two dropwise add feeding methods, tertiary reation kettle ally oneself with jointly, realize incessant serialization and nitrify preparation 5-nitro salicylic acid, improve 5-nitro salicylic acid's yield simultaneously.
Description
Technical Field
The utility model belongs to the technical field of chemical industry equipment, a production facility of 5-nitro salicylic acid is related to, concretely relates to 5-nitro salicylic acid's serialization production facility.
Background
The 5-nitro salicylic acid is a main intermediate for synthesizing the masalazine for treating the chronic colitis, is also an important intermediate for synthesizing fine chemicals such as dyes, pigments and the like, and the iron salt of the 5-nitro salicylic acid can be used for measuring the scale and corrosion resistant dispersant 2-phosphonic butane-1, 2, 4-tricarboxylic acid, and has certain market development prospect at home and abroad.
In the existing preparation method, a batch kettle type process is usually adopted, salicylic acid is used as a raw material, and under the action of a catalyst (sulfuric acid), nitric acid is dripped into solvents such as acetic acid, acetic anhydride, ethanol and acetone to prepare the 5-nitro salicylic acid by nitration.
In the nitration reaction process, the nitric acid is continuously dripped to generate the 5-nitro salicylic acid and water, and the concentration of catalyst sulfuric acid in the system is continuously reduced, so that the nitration reaction conversion rate is low; if too much sulfuric acid is added at a time, a nitro-polysubstituted compound is formed, affecting the yield.
SUMMERY OF THE UTILITY MODEL
Aiming at the defects of the prior art, the utility model aims to provide a continuous production device of 5-nitro salicylic acid, which adopts the double-dropping feeding mode and the combination of three-stage reaction kettles, realizes the uninterrupted continuous nitration preparation of 5-nitro salicylic acid and simultaneously improves the yield of 5-nitro salicylic acid.
The utility model discloses a realize through following technical scheme:
a continuous production device of 5-nitro salicylic acid, which comprises a first nitration kettle, a second nitration kettle and a third nitration kettle, the first nitration kettle is provided with a salicylic acid solution dripping port, the first nitration kettle, the second nitration kettle and the third nitration kettle are respectively provided with a mixed acid dripping port, a stirring device, a jacket and a cooling inner coil pipe, annular baffles are horizontally arranged on the inner walls of the first nitrification kettle, the second nitrification kettle and the third nitrification kettle above the inner coil pipe, the side wall of the first nitration kettle above the annular baffle is provided with a first overflow port which is communicated with the feed inlet of the second nitration kettle through a pipeline, the lateral wall that the second nitrifies the cauldron and is located the annular baffle top is equipped with the second overflow mouth, the second overflow mouth pass through the pipeline with the feed inlet intercommunication of the third nitrifies the cauldron, the lateral wall that the third nitrifies the cauldron and is located the annular baffle top is equipped with the third overflow mouth.
Furthermore, the stirring devices of the first nitration kettle, the second nitration kettle and the third nitration kettle are double helix blade stirring devices.
Further, the mixed acid dropwise add mouth of first nitration cauldron, second nitration cauldron and third nitration cauldron all is equipped with mixed acid drainage tube, the end that mixes acid drainage tube is located directly over first nitration cauldron, second nitration cauldron and third nitration cauldron agitating unit's stirring leaf.
The utility model discloses a further improvement scheme does:
and stirring shaft limiting devices are arranged at the bottoms of the first nitration kettle, the second nitration kettle and the third nitration kettle.
Further, the (mixing) shaft stop device includes the tetrafluoro axle sleeve, is used for fixing the support of tetrafluoro axle sleeve, the support is fixed in the chassis, the chassis is fixed in through bolt detachable at the bottom of the cauldron of first nitration cauldron, second nitration cauldron and third nitration cauldron, the chassis is equipped with the blowing valve, the tetrafluoro axle sleeve is located agitating unit's end, the tetrafluoro axle sleeve internal diameter with agitating unit's (mixing) shaft external diameter matches.
The utility model discloses a further improvement scheme does:
and a first sedimentation separator is arranged on a pipeline between the first overflow port and the feed inlet of the second nitration kettle, and a second sedimentation separator is arranged on a pipeline between the second overflow port and the feed inlet of the third nitration kettle.
Furthermore, the first settling separator and the second settling separator are both provided with sight glasses.
Further, the horizontal positions of the first overflow port, the first settling separator, the feed inlet of the second nitration kettle, the second overflow port, the second settling separator, the feed inlet of the third nitration kettle and the third overflow port are sequentially reduced.
The utility model has the advantages that:
the utility model discloses a tertiary cauldron of nitrifying, the continuous feeding of first cauldron of nitrifying, adopt two dropwise mode, the nitric acid that the dropwise add was prepared in proportion and sulphuric acid's mixed acid simultaneously, salicylic acid and solvent mixed salicylic acid solution, the incessant overflow of reaction material to second nitration cauldron, the third cauldron of nitrifying, simultaneously to the second nitration cauldron, the dropwise mixed acid of third nitration cauldron, further promote the salicylic acid among the reaction mass to nitrify, avoided in the intermittent type cauldron formula technology because the continuous conversion rate that reduces salicylic acid that generates of reaction normal water, and simultaneously, the dropwise mixed acid is the mixture of the nitric acid of preparing according to the proportion according to the technological requirement and sulphuric acid, the conversion rate of salicylic acid has been guaranteed and the impurity that can not generate many nitro substitution, the yield of 5-nitro salicylic acid is improved.
The utility model discloses in, adopt double helix leaf agitating unit for the circulation mode of material in nitrifying the cauldron is from top to bottom, from inside to outside circulation, and the stirring is more abundant, and the material of unreacted at first moves down, reacts simultaneously at the in-process that rises, guarantees to reach the anticipated reaction process of process design when reaching the overflow mouth.
The utility model discloses in, use and mix sour drainage tube, make and mix sour direct material circulation center that gets into the cauldron of nitrifying, downstream immediately after getting into participates in the reaction, avoids mixing sour and does not just flow to next-level through the overflow mouth through the reaction and nitrifies the cauldron, improves material utilization.
The utility model discloses in, use (mixing) shaft stop device, prevent effectively that the (mixing) shaft from rocking, guaranteed that the material obtains intensive mixing, avoid because of the stirring that rocks and bring uneven, make the material fully circulate, in time release the produced heat of nitration, avoid removing too late serious consequences such as leading to reaction failure or explosion and take place often because of the heat.
The utility model discloses in, use the settler, isolate in the reaction material diluted and can not reach the acid solution of reaction requirement, guarantee that the ratio of material and mixed acid accords with the requirement of process design in the next nitration cauldron.
Drawings
FIG. 1 is a schematic view of the present invention;
FIG. 2 is a top view of the ring baffle of the present invention;
FIG. 3 is a schematic view of the structure of the stirring shaft limiting device of the present invention;
the device comprises a first nitration kettle 1, a second nitration kettle 2, a third nitration kettle 3, a salicylic acid solution dripping port 4, a mixed acid dripping port 5, a stirring device 6, a jacket 7, a cooling inner coil pipe 8, an annular baffle 9, a first overflow port 10, a feed inlet 11-A, a second overflow port 12, a feed inlet 13-B, a third overflow port 14-A, a mixed acid drainage pipe 15, a stirring shaft limiting device 16, a polytetrafluoroethylene shaft sleeve 161, a support 162, a chassis 163, a discharge valve 164, a first sedimentation separator 17, a second sedimentation separator 18 and a sight glass 19.
Detailed Description
The present invention will be further explained by the following embodiments with reference to the accompanying drawings.
A continuous production device of 5-nitro salicylic acid comprises a first nitration kettle 1, a second nitration kettle 2 and a third nitration kettle 3, wherein the first nitration kettle 1 is provided with a salicylic acid solution dripping port 4, the first nitration kettle 1, the second nitration kettle 2 and the third nitration kettle 3 are respectively provided with a mixed acid dripping port 5, a stirring device 6, a jacket 7 and a cooling inner coil 8, the inner walls of the first nitration kettle 1, the second nitration kettle 2 and the third nitration kettle 3 above the inner coil 8 are respectively and horizontally provided with an annular baffle plate 9, the side wall of the first nitration kettle 1 above the annular baffle plate 9 is provided with a first overflow port 10, the first overflow port 10 is communicated with an A feed port 11 of the second nitration kettle through a pipeline, the side wall of the second nitration kettle 2 above the annular baffle plate 9 is provided with a second overflow port 12, the second overflow port 12 is communicated with a B feed port 13 of the third nitration kettle through a pipeline, the side wall of the third nitrification reactor 3 above the annular baffle 9 is provided with a third overflow port 14.
In this embodiment, a first sedimentation separator 17 is disposed on the pipeline between the first overflow port 10 and the feed port a 11 of the second nitrification reactor, a second sedimentation separator 18 is disposed on the pipeline between the second overflow port 12 and the feed port B13 of the third nitrification reactor, and the first sedimentation separator 17 and the second sedimentation separator 18 are both provided with viewing mirrors 19.
In this embodiment, the horizontal positions of the first overflow port 10, the first settling separator 17, the feed port a 11 of the second nitrification reactor, the second overflow port 12, the second settling separator 18, the feed port B13 of the third nitrification reactor, and the third overflow port 14 are sequentially lowered.
In this embodiment, the stirring devices 6 of the first nitrification reactor 1, the second nitrification reactor 2 and the third nitrification reactor 3 are all double-spiral-blade stirring devices.
The mixed acid dripping ports 5 of the first nitration kettle 1, the second nitration kettle 2 and the third nitration kettle 3 are respectively provided with a mixed acid drainage tube 15, and the tail end of the mixed acid drainage tube 15 is positioned right above the stirring blades of the stirring devices 6 of the first nitration kettle 1, the second nitration kettle 2 and the third nitration kettle 3.
In this embodiment, the bottom of the first nitrification reactor 1, the second nitrification reactor 2, and the third nitrification reactor 3 are provided with a stirring shaft limiting device 16. The stirring shaft limiting device 16 comprises a tetrafluoro shaft sleeve 161 and a support 162 for fixing the tetrafluoro shaft sleeve 161, the support 162 is fixed on a base plate 163, the base plate 163 is detachably fixed at the bottoms of the first nitration kettle 1, the second nitration kettle 2 and the third nitration kettle 3 through bolts, the base plate 163 is provided with a discharge valve 164, the tetrafluoro shaft sleeve 161 is sleeved at the tail end of the stirring device 6, and the inner diameter of the tetrafluoro shaft sleeve 161 is matched with the outer diameter of a stirring shaft of the stirring device 6.
The working principle of utilizing the equipment of the utility model to continuously nitrify and prepare 5-nitro salicylic acid is as follows: according to the process requirements, preparing a mixed acid solution of nitric acid and sulfuric acid according to a proportion, preparing a salicylic acid solution of salicylic acid and a solvent, storing the salicylic acid solution in a tank area, starting a stirring device 6 of a first nitration kettle 1, respectively dripping the salicylic acid solution and the mixed acid solution through a salicylic acid solution dripping port 4 and a mixed acid dripping port 5, leading the temperature in the nitration kettle to reach the nitration requirement through a jacket 7, taking away heat generated by a severe nitration reaction through a cooling inner coil 8 to achieve the aim of controlling the temperature, when materials in the first nitration kettle 1 reach the height of a first overflow port 10, flowing out from the first overflow port 10, entering a first settling separator 17, standing and layering the materials in the first settling separator, observing the layering condition through a sight glass 19, leading upper layer (organic layer) to enter a second nitration kettle 2 through a pipeline, leading lower layer (acid layer) to be discharged at regular time, entering a storage area for treatment, and after the materials enter the second nitration kettle 1, open the stirring, through the 5 dropwise add mixed acid of mixed acid dropwise add mouth of second nitration cauldron 2, other operations are with first nitration cauldron 1, when the material passes through second overflow mouth 12, get into second sedimentation separator 18, after the layering, get into third nitration cauldron 3 again, the operation of third nitration cauldron 3 is with second nitration cauldron 2, when the material in the third nitration cauldron 3 flows out from third overflow mouth 14, go into assay and detect, wherein salicylic acid content falls to the end of technology reaction requirement, and 5-nitro salicylic acid's content exceeds the end of technology reaction requirement, through the utility model discloses the use of equipment makes the yield of 5-nitro salicylic acid reach 97%.
Claims (8)
1. The continuous production equipment of the 5-nitrosalicylic acid is characterized by comprising a first nitration kettle (1), a second nitration kettle (2) and a third nitration kettle (3), wherein the first nitration kettle (1) is provided with a salicylic acid solution dripping port (4), the first nitration kettle (1), the second nitration kettle (2) and the third nitration kettle (3) are respectively provided with a mixed acid dripping port (5), a stirring device (6), a jacket (7) and a cooling inner coil (8), annular baffles (9) are horizontally arranged on the inner walls of the inner coil (8), the first nitration kettle (1), the second nitration kettle (2) and the third nitration kettle (3), a first overflow port (10) is arranged on the side wall of the first nitration kettle (1) above the annular baffles (9), and the first overflow port (10) is communicated with a feed inlet (11) of the second nitration kettle (2) through a pipeline, the lateral wall that second nitration cauldron (2) are located annular baffle (9) top is equipped with second overflow mouth (12), second overflow mouth (12) through the pipeline with B feed inlet (13) the intercommunication of third nitration cauldron (3), the lateral wall that third nitration cauldron (3) are located annular baffle (9) top is equipped with third overflow mouth (14).
2. The continuous production apparatus of 5-nitrosalicylic acid as claimed in claim 1, wherein: and the stirring devices (6) of the first nitration kettle (1), the second nitration kettle (2) and the third nitration kettle (3) are double-helix blade stirring devices.
3. The continuous production apparatus of 5-nitrosalicylic acid as claimed in claim 1, wherein: the mixed acid dripping ports (5) of the first nitration kettle (1), the second nitration kettle (2) and the third nitration kettle (3) are respectively provided with a mixed acid drainage tube (15), and the tail end of the mixed acid drainage tube (15) is positioned right above the stirring blades of the stirring devices (6) of the first nitration kettle (1), the second nitration kettle (2) and the third nitration kettle (3).
4. The continuous production apparatus of 5-nitrosalicylic acid as claimed in claim 1, wherein: the kettle bottoms of the first nitration kettle (1), the second nitration kettle (2) and the third nitration kettle (3) are respectively provided with a stirring shaft limiting device (16).
5. The continuous production apparatus of 5-nitrosalicylic acid as set forth in claim 4, wherein: (mixing) shaft stop device (16) include tetrafluoro axle sleeve (161), support (162) that are used for fixed tetrafluoro axle sleeve (161), support (162) are fixed in chassis (163), chassis (163) are fixed in through bolt detachable at the bottom of the cauldron of first nitration cauldron (1), second nitration cauldron (2) and third nitration cauldron (3), chassis (163) are equipped with blowing valve (164), tetrafluoro axle sleeve (161) cover is located the end of agitating unit (6), tetrafluoro axle sleeve (161) internal diameter with the (mixing) shaft external diameter of agitating unit (6) matches.
6. The continuous production apparatus of 5-nitrosalicylic acid as claimed in claim 1, wherein: and a first sedimentation separator (17) is arranged on a pipeline between the first overflow port (10) and the A feed port (11) of the second nitration kettle (2), and a second sedimentation separator (18) is arranged on a pipeline between the second overflow port (12) and the B feed port (13) of the third nitration kettle (3).
7. The continuous production apparatus of 5-nitrosalicylic acid as set forth in claim 6, wherein: the first settling separator (17) and the second settling separator (18) are both provided with sight glasses (19).
8. The continuous production apparatus of 5-nitrosalicylic acid as set forth in claim 6, wherein: the horizontal positions of the first overflow port (10), the first sedimentation separator (17), the A feed inlet (11) of the second nitration kettle (2), the second overflow port (12), the second sedimentation separator (18), the B feed inlet (13) of the third nitration kettle (3) and the third overflow port (14) are sequentially reduced.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921397948.XU CN210620664U (en) | 2019-08-27 | 2019-08-27 | Continuous production equipment for 5-nitro salicylic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921397948.XU CN210620664U (en) | 2019-08-27 | 2019-08-27 | Continuous production equipment for 5-nitro salicylic acid |
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| Publication Number | Publication Date |
|---|---|
| CN210620664U true CN210620664U (en) | 2020-05-26 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201921397948.XU Active CN210620664U (en) | 2019-08-27 | 2019-08-27 | Continuous production equipment for 5-nitro salicylic acid |
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| CN (1) | CN210620664U (en) |
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- 2019-08-27 CN CN201921397948.XU patent/CN210620664U/en active Active
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