CN220835492U - Production system of paranitrobenzoyl chloride - Google Patents
Production system of paranitrobenzoyl chloride Download PDFInfo
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- CN220835492U CN220835492U CN202322450395.2U CN202322450395U CN220835492U CN 220835492 U CN220835492 U CN 220835492U CN 202322450395 U CN202322450395 U CN 202322450395U CN 220835492 U CN220835492 U CN 220835492U
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- evaporator
- outlet
- condenser
- mixing kettle
- tubular reactor
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- SKDHHIUENRGTHK-UHFFFAOYSA-N 4-nitrobenzoyl chloride Chemical compound [O-][N+](=O)C1=CC=C(C(Cl)=O)C=C1 SKDHHIUENRGTHK-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 title abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 40
- 239000011552 falling film Substances 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 21
- 239000003507 refrigerant Substances 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000005192 partition Methods 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims description 27
- 238000003756 stirring Methods 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 18
- 239000002912 waste gas Substances 0.000 abstract description 6
- 230000007613 environmental effect Effects 0.000 abstract description 2
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 description 14
- OTLNPYWUJOZPPA-UHFFFAOYSA-N 4-nitrobenzoic acid Chemical compound OC(=O)C1=CC=C([N+]([O-])=O)C=C1 OTLNPYWUJOZPPA-UHFFFAOYSA-N 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 239000002826 coolant Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- OVBPIULPVIDEAO-LBPRGKRZSA-N folic acid Chemical compound C=1N=C2NC(N)=NC(=O)C2=NC=1CNC1=CC=C(C(=O)N[C@@H](CCC(O)=O)C(O)=O)C=C1 OVBPIULPVIDEAO-LBPRGKRZSA-N 0.000 description 2
- UHZYTMXLRWXGPK-UHFFFAOYSA-N phosphorus pentachloride Chemical compound ClP(Cl)(Cl)(Cl)Cl UHZYTMXLRWXGPK-UHFFFAOYSA-N 0.000 description 2
- XAFOTXWPFVZQAZ-UHFFFAOYSA-N 2-(4-aminophenyl)-3h-benzimidazol-5-amine Chemical compound C1=CC(N)=CC=C1C1=NC2=CC=C(N)C=C2N1 XAFOTXWPFVZQAZ-UHFFFAOYSA-N 0.000 description 1
- QIKYZXDTTPVVAC-UHFFFAOYSA-N 4-Aminobenzamide Chemical compound NC(=O)C1=CC=C(N)C=C1 QIKYZXDTTPVVAC-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- OVBPIULPVIDEAO-UHFFFAOYSA-N N-Pteroyl-L-glutaminsaeure Natural products C=1N=C2NC(N)=NC(=O)C2=NC=1CNC1=CC=C(C(=O)NC(CCC(O)=O)C(O)=O)C=C1 OVBPIULPVIDEAO-UHFFFAOYSA-N 0.000 description 1
- HCBIBCJNVBAKAB-UHFFFAOYSA-N Procaine hydrochloride Chemical compound Cl.CCN(CC)CCOC(=O)C1=CC=C(N)C=C1 HCBIBCJNVBAKAB-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229960000304 folic acid Drugs 0.000 description 1
- 235000019152 folic acid Nutrition 0.000 description 1
- 239000011724 folic acid Substances 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000007867 post-reaction treatment Methods 0.000 description 1
- 229960001309 procaine hydrochloride Drugs 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 231100000167 toxic agent Toxicity 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
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- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The utility model discloses a production system of paranitrobenzoyl chloride, which comprises a mixing kettle, a tubular reactor, a falling film evaporator, a slicer, a condenser, a material conveying pump and a driving motor, wherein the mixing kettle is connected with the tubular reactor; the tubular reactor comprises a box body and a tube body arranged in the box body; the box body of the tubular reactor is divided into a first temperature zone and a second temperature zone by a partition plate; a heating medium inlet and a heating medium outlet are formed in the part, located in the first temperature zone, of the box body; and a part of the box body, which is positioned in the second temperature zone, is provided with a refrigerant inlet and a refrigerant outlet. The production system adopts a continuous closed production mode of the tubular reactor, the falling film evaporator and the slicing machine, so that the waste gas emission of the production system is less, the pollution is reduced, the environmental protection pressure is greatly lightened, the possibility of the waste gas unorganized emission is reduced, the production site environment is ensured, the safety is higher, and the tubular reactor adopts two temperature areas, thereby ensuring the stability of the reaction and improving the efficiency of the reaction.
Description
Technical Field
The utility model relates to a production system of paranitrobenzoyl chloride.
Background
The p-nitrobenzoyl chloride is an important intermediate for synthesizing important special chemicals and bulk drugs such as p-aminobenzamide, 4' -diaminobenzanilide, 2- (4-aminophenyl) -5-aminobenzimidazole, folic acid, procaine hydrochloride and the like, and is also widely used for the production of pigments and color developers. In particular, in recent years, as market demand for special chemicals continues to increase, p-nitrobenzoyl chloride is an important raw material for producing special chemicals, and market demand is rapidly rising, and meanwhile, higher and higher requirements are also put on the quality of the products.
At present, the existing production process of paranitrobenzoyl chloride mainly comprises the following steps: ① Is prepared by the reaction of p-nitrobenzoic acid and phosgene; ② Is prepared by the reaction of p-nitrobenzoic acid and phosphorus oxychloride or phosphorus pentachloride; ③ Is prepared by reacting p-nitrobenzoic acid with thionyl chloride in the presence of a catalyst. Wherein: (1) The phosgene method has low safety and can cause harm to human bodies; (2) Phosphorus oxychloride is a highly toxic substance, and is safe to human bodies and easy to cause harm to the environment; (3) The phosphorus pentachloride is solid, and a solvent is required to be added to accelerate the reaction, so that the reaction selectivity is low, and the post-reaction treatment is complicated.
At present, the most important method for producing p-nitrobenzoyl chloride is the sulfoxide chloride method, namely, the p-nitrobenzoic acid is reacted with excessive sulfoxide chloride to prepare the p-nitrobenzoyl chloride. In the prior art, a kettle type reactor is adopted for reaction, so that the reaction operation difficulty is high, the instantaneous release of waste gas is high, and the absorption and treatment load is high. In addition, the prior art mostly removes the front cut through general rectification and purification, and can remove the residual thionyl chloride in the reaction to a certain extent, but the separation efficiency is limited, and a small amount of thionyl chloride is still brought into the product, thereby bringing trouble to the drying and quality control of the product.
Disclosure of utility model
The utility model aims to solve the problems and provide a production system of paranitrobenzoyl chloride, which is friendly to the environment, high in safety, high in reaction efficiency and stability and high in product quality.
The technical scheme for realizing the aim of the utility model is as follows: a system for producing paranitrobenzoyl chloride, comprising: a mixing kettle; the mixing kettle is provided with a mixing kettle feed inlet, a mixing kettle discharge outlet and a mixing kettle liquid inlet; a stirring device is arranged in the mixing kettle; a tubular reactor; the tubular reactor comprises a box body and a tube body arranged in the box body; the box body is provided with a reactor feed inlet and a reactor discharge outlet; the reactor feed inlet of the tubular reactor is connected with the material mixing kettle discharge outlet of the material mixing kettle; a falling film evaporator; the falling film evaporator comprises an evaporator body and a gas-liquid separator communicated with the lower part of the evaporator body; the evaporator body is provided with an evaporator feed inlet, an evaporator refrigerant outlet and a residue outlet; the gas-liquid separator is provided with an evaporator liquid outlet and an evaporator air outlet; the evaporator feed inlet of the falling film evaporator is connected with the reactor discharge outlet of the tubular reactor; a slicer; the slicer is provided with a slicer feed inlet and a slicer discharge outlet; the slicer feed inlet of the slicer is connected with the evaporator liquid outlet of the falling film evaporator; a condenser; the condenser is provided with a condenser air inlet, a condenser air outlet, a condenser liquid outlet, a condenser refrigerant inlet and a condenser refrigerant outlet; the condenser air inlet of the condenser is connected with the evaporator air outlet of the falling film evaporator; and a condenser liquid outlet of the condenser is connected with a liquid inlet of the mixing kettle.
And a material conveying pump is further arranged between the reactor feed inlet of the tubular reactor and the material mixing kettle discharge outlet of the material mixing kettle.
The inner surface of the tube body of the tube reactor is made of glass lining.
The slicer is driven by a drive motor.
The box body of the tubular reactor is divided into a first temperature zone and a second temperature zone by a partition plate; a heating medium inlet and a heating medium outlet are formed in the part, located in the first temperature zone, of the box body; and a part of the box body, which is positioned in the second temperature zone, is provided with a refrigerant inlet and a refrigerant outlet.
The utility model has the positive effects that:
(1) The production system adopts a tubular reactor, a falling film evaporator and a slicing machine to carry out a continuous closed production mode, so that the waste gas emission of the production system is less, the pollution is reduced, the environmental protection pressure is greatly lightened, the possibility of unorganized emission of waste gas is reduced, the production site environment is ensured, and the safety is higher.
(2) The tubular reactor of the production system adopts two temperature areas, the first temperature area ensures that the materials are rapidly started to react at high temperature, and the second temperature area ensures that the materials are reacted at the reaction temperature, so that the stability of the reaction is ensured, and the reaction efficiency is improved.
(3) The production system adopts the falling film evaporator to separate the materials, ensures the rapid and efficient separation of the paranitrobenzoyl chloride and the thionyl chloride, reduces the possibility of impurity generation caused by the deterioration of the materials at high temperature, and improves the quality of products.
Drawings
FIG. 1 is a schematic diagram of the production system of paranitrobenzoyl chloride according to the present utility model.
FIG. 2 is a schematic structural view of the tubular reactor in FIG. 1.
Detailed Description
Example 1
Referring to fig. 1, the production system of paranitrobenzoyl chloride of the present embodiment comprises a mixing kettle 1, a tubular reactor 2, a falling film evaporator 3, a slicer 4, a condenser 5, a material conveying pump 6 and a driving motor 7.
The mixing kettle 1 is provided with a mixing kettle feed inlet 1-1, a mixing kettle discharge outlet 1-2 and a mixing kettle liquid inlet 1-3, and a stirring device 11 is arranged in the mixing kettle 1.
The tubular reactor 2 comprises a box body 21 and a pipe body 22 arranged in the box body 21, wherein a reactor feed inlet 2-1 and a reactor discharge outlet 2-2 are arranged on the box body 21, the inner surface of the pipe body 22 of the tubular reactor 2 is made of glass lining, and the reactor feed inlet 2-1 of the tubular reactor 2 is connected with the mixing kettle discharge outlet 1-2 of the mixing kettle 1 through a material conveying pump 6.
Referring to fig. 2, a tank 21 of the tubular reactor 2 is divided into a first temperature zone 21-1 and a second temperature zone 21-2 by a partition plate 23, a heat medium inlet 2-3 and a heat medium outlet 2-4 are provided at a portion of the tank 21 located in the first temperature zone 21-1, and a refrigerant inlet 2-5 and a refrigerant outlet 2-6 are provided at a portion of the tank 21 located in the second temperature zone 21-2.
The falling film evaporator 3 comprises an evaporator body 31 and a gas-liquid separator 32 communicated with the lower part of the evaporator body 31, wherein an evaporator feed inlet 3-1, an evaporator refrigerant inlet 3-2, an evaporator refrigerant outlet 3-3 and a residue outlet 3-4 are arranged on the evaporator body 31, an evaporator liquid outlet 3-5 and an evaporator air outlet 3-6 are arranged on the gas-liquid separator 32, and the evaporator feed inlet 3-1 of the falling film evaporator 3 is connected with a reactor discharge outlet 2-2 of the tubular reactor 2.
The slicer 4 is provided with a slicer feed inlet 4-1 and a slicer discharge outlet 4-2, and the slicer 4 is driven by a driving motor 7. The slicer feed inlet 4-1 of the slicer 4 is connected with the evaporator outlet 3-5 of the falling film evaporator 3.
The condenser 5 is provided with a condenser air inlet 5-1, a condenser air outlet 5-2, a condenser liquid outlet 5-3, a condenser refrigerant inlet 5-4 and a condenser refrigerant outlet 5-5, the condenser air inlet 5-1 of the condenser 5 is connected with the evaporator air outlet 3-6 of the falling film evaporator 3, and the condenser liquid outlet 5-3 of the condenser 5 is connected with the mixing kettle liquid inlet 1-3 of the mixing kettle 1.
The technological process is as follows:
① And (3) starting a stirring device 11 in the mixing kettle 1, adding p-nitrobenzoic acid, thionyl chloride and a catalyst into the mixing kettle 1 from a feeding port 1-1 of the mixing kettle according to the conventional dosage, and stirring and mixing uniformly.
② The heating medium, the cooling medium and the cooling medium in the tubular reactor 2 and the cooling medium in the falling film evaporator 3 are respectively started, and the tubular reactor 2 and the falling film evaporator 3 are respectively preheated and precooled, wherein the temperature of the first temperature zone 21-1 is required to be higher than the reaction temperature so as to ensure that the materials can quickly start the reaction, and the temperature of the second temperature zone 21-2 is stable.
③ Then the material conveying pump 6 is started, the materials in the material mixing kettle 1 are conveyed into the pipe body 22 of the pipe reactor 2, the materials rapidly start reaction in the first temperature zone 21-1, and then the reaction is insulated in the second temperature zone 21-2.
④ After the reaction is finished, the materials are sent into a falling film evaporator 3 through a reactor discharge port 2-2, so that the efficient separation of the paranitrobenzoyl chloride liquid and the gas is realized, and after the separation is finished, the product paranitrobenzoyl chloride liquid is sent into a slicer 5 through an evaporator discharge port 3-5, and the paranitrobenzoyl is obtained through cooling, drying and slicing.
The gas enters a condenser 5 through an evaporator gas outlet 3-6, the condensed thionyl chloride liquid can be recycled into the mixing kettle 1 through a condenser liquid outlet 5-3, and the uncondensed gas (such as hydrogen chloride, sulfur dioxide and the like) is sent to a waste gas treatment system for recycling treatment through a condenser gas outlet 5-2.
Claims (5)
1. A system for producing paranitrobenzoyl chloride, comprising:
A mixing kettle (1); the mixing kettle (1) is provided with a mixing kettle feed inlet (1-1), a mixing kettle discharge outlet (1-2) and a mixing kettle liquid inlet (1-3); a stirring device (11) is arranged in the mixing kettle (1);
A tubular reactor (2); the tubular reactor (2) comprises a box body (21) and a tube body (22) arranged in the box body (21); the box body (21) is provided with a reactor feed inlet (2-1) and a reactor discharge outlet (2-2); the reactor feed inlet (2-1) of the tubular reactor (2) is connected with the mixing kettle discharge outlet (1-2) of the mixing kettle (1);
A falling film evaporator (3); the falling film evaporator (3) comprises an evaporator body (31) and a gas-liquid separator (32) communicated with the lower part of the evaporator body (31); the evaporator body (31) is provided with an evaporator feed inlet (3-1), an evaporator refrigerant inlet (3-2), an evaporator refrigerant outlet (3-3) and a residue outlet (3-4); the gas-liquid separator (32) is provided with an evaporator liquid outlet (3-5) and an evaporator air outlet (3-6); an evaporator feed inlet (3-1) of the falling film evaporator (3) is connected with a reactor discharge outlet (2-2) of the tubular reactor (2);
A slicer (4); the slicer (4) is provided with a slicer feed inlet (4-1) and a slicer discharge outlet (4-2); a slicer feed inlet (4-1) of the slicer (4) is connected with an evaporator liquid outlet (3-5) of the falling film evaporator (3);
A condenser (5); the condenser (5) is provided with a condenser air inlet (5-1), a condenser air outlet (5-2), a condenser liquid outlet (5-3), a condenser refrigerant inlet (5-4) and a condenser refrigerant outlet (5-5); a condenser air inlet (5-1) of the condenser (5) is connected with an evaporator air outlet (3-6) of the falling film evaporator (3); the condenser liquid outlet (5-3) of the condenser (5) is connected with the liquid inlet (1-3) of the mixing kettle (1).
2. The system for producing paranitrobenzoyl chloride according to claim 1, wherein: a material conveying pump (6) is further arranged between the reactor feed inlet (2-1) of the tubular reactor (2) and the material mixing kettle discharge outlet (1-2) of the material mixing kettle (1).
3. The system for producing paranitrobenzoyl chloride according to claim 1, wherein: the inner surface of the pipe body (22) of the pipe reactor (2) is made of glass lining.
4. The system for producing paranitrobenzoyl chloride according to claim 1, wherein: the slicer (4) is driven by a driving motor (7).
5. The system for producing paranitrobenzoyl chloride according to any one of claims 1 to 4, wherein: the box body (21) of the tubular reactor (2) is divided into a first temperature zone (21-1) and a second temperature zone (21-2) by a partition plate (23); a heating medium inlet (2-3) and a heating medium outlet (2-4) are arranged on the part of the box body (21) located in the first temperature zone (21-1); the part of the box body (21) located in the second temperature zone (21-2) is provided with a refrigerant inlet (2-5) and a refrigerant outlet (2-6).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202322450395.2U CN220835492U (en) | 2023-09-09 | 2023-09-09 | Production system of paranitrobenzoyl chloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202322450395.2U CN220835492U (en) | 2023-09-09 | 2023-09-09 | Production system of paranitrobenzoyl chloride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN220835492U true CN220835492U (en) | 2024-04-26 |
Family
ID=90740705
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202322450395.2U Active CN220835492U (en) | 2023-09-09 | 2023-09-09 | Production system of paranitrobenzoyl chloride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN220835492U (en) |
-
2023
- 2023-09-09 CN CN202322450395.2U patent/CN220835492U/en active Active
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