Continuous production system of substituent-containing benzenesulfonyl isocyanate
By using a continuous batch reaction mode and a continuous production system that utilizes solvent recovery, the problems of high equipment requirements and poor safety in isocyanate production have been solved, achieving high yield, high purity, and high safety in production.
Patent Information
- Application Number
- CN202520228311.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-13
- Publication Date
- 2025-11-28
- Estimated Expiration
- 2035-02-13
AI Technical Summary
Existing isocyanate production processes suffer from high equipment requirements, poor safety, and the use of highly toxic raw material phosgene.
The continuous batch reactor mode is adopted, and through the combination of the preparation system, esterification reaction system and purification system, the safer dimethyl carbonate is used to replace phosgene for synthesis. Combined with the real-time recycling and purification methods of solvent, continuous production is achieved.
It improved product yield and purity, enhanced safety performance, reduced process wastewater generation, and met the needs of efficient and safe production.
Smart Images
Figure CN223607195U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The utility model relates to a continuous production system of substituted benzene sulfonyl isocyanate, and particularly relates to a continuous production system of substituted benzene sulfonyl isocyanate. BACKGROUND
[0002] Isocyanate is an important substance of synthetic organic matter, and many chemicals can be prepared by synthesis. The p-toluenesulfonyl isocyanate is mainly used in adhesive glue, sealant, organic solvent and water removing agent due to its high activity and low viscosity, and can be used as a herbicide intermediate and a medical intermediate to prepare related hypoglycemic drugs, and is also an important intermediate of new materials. The domestic production process is mostly prepared by intermittent reaction of p-toluenesulfonamide and phosgene in the kettle. The preparation method has high requirements for equipment, and there is toxic raw material phosgene, and the production safety is poor. UTILITY MODEL CONTENT
[0003] In view of the deficiencies of the prior art, the utility model aims at providing a continuous production system of substituted benzene sulfonyl isocyanate, which has higher product yield and purity, better safety performance, and the solvent in the reaction process can be recycled in real time.
[0004] The utility model solves technical problems by adopting the following technical scheme: a continuous production system of substituted benzene sulfonyl isocyanate, the production system includes preparation system, esterification reaction system and refining system, the preparation system includes first preparation kettle and second preparation kettle, the esterification reaction system includes a plurality of reaction kettles, and each reaction kettle is connected in turn, the first preparation kettle and the second preparation kettle are connected with the first reaction kettle in the esterification reaction system respectively, the refining system includes primary solvent recovery system, secondary solvent recovery system and distillation system, and the solvent recovered in each solvent recovery system is collected in a solvent recovery tank, and the last reaction kettle in the esterification reaction system is connected with the refining system.
[0005] Further, the first preparation kettle is used for preparing bistrichloromethyl carbonate chlorobenzene solution, and the first preparation kettle is provided with a reflux system; and the discharge port of the first preparation kettle is connected with the reaction kettle in the esterification reaction system through a pipeline.
[0006] Further, the second preparation kettle is used for preparing substituted benzene sulfonyl amide chlorobenzene solution, and the second preparation kettle is provided with a reflux system; and the discharge port of the second preparation kettle is connected with the reaction kettle in the esterification reaction system through a pipeline.
[0007] Further, the esterification reaction system is three-stage, comprising a first-stage reaction kettle, a second-stage reaction kettle and a third-stage reaction kettle connected in sequence; each stage reaction kettle is provided with a reflux system; during production, the reaction mixture is kept flowing at a certain flow rate between the reaction kettles.
[0008] Further, a buffer kettle is arranged between the esterification reaction system and the refining system; the buffer kettle is connected with the first-stage solvent recovery system of the refining system through a metering pump and a pipeline.
[0009] Further, the first-stage solvent recovery system comprises a first-stage evaporator, a first-stage condenser and a first-stage storage tank, the first-stage evaporator is a normal-pressure evaporator; the second-stage solvent recovery system comprises a second-stage evaporator, a second-stage condenser and a second-stage storage tank, the second-stage evaporator is connected with a vacuum system; the discharge outlets of the first-stage condenser and the second-stage condenser are connected to a solvent recovery tank.
[0010] Further, the discharge outlet of the solvent recovery tank is connected to the preparation system and the esterification reaction system through a metering pump and a pipeline.
[0011] Further, the distillation system comprises a molecular distillation device, a product storage tank and a waste storage tank, the molecular distillation device is connected with a vacuum system.
[0012] The beneficial effects of the present application are as follows: compared with the prior art, the continuous production system for substituted phenylsulfonyl isocyanate provided by the present application has higher product yield and purity and better safety performance; carbon dimethyl ester is used as the reaction raw material in the reaction system to replace the toxic phosgene for synthesis reaction, so that the safety performance is high, high-pressure reaction equipment is not needed to meet the synthesis requirements, the production equipment is simple, the reaction is carried out in almost water-free environment, the hydrolysis reaction of the substituted phenylsulfonyl isocyanate is avoided, the product yield is high, and the product yield is more than 95%; the distillation method is used for refining, the product purity is high, and the product purity is more than 99%; the reaction solvent recovery utilization rate is high, and almost no process wastewater is generated. BRIEF DESCRIPTION OF DRAWINGS
[0013] Fig. 1 The structure diagram of the preparation system in the production system provided by the present application is shown.
[0014] Fig. 2 The structure diagram of the esterification reaction system in the production system provided by the present application is shown.
[0015] Fig. 3 The structure diagram of the refining system in the production system provided by the present application is shown.
[0016] Among them, 101-first preparation vessel; 102-second preparation vessel; 201-first stage reaction vessel; 202-second stage reaction vessel; 203-third stage reaction vessel; 204-buffer vessel; 301-first stage evaporator; 302-first stage condenser; 303-first stage storage tank; 304-second stage evaporator; 305-second stage condenser; 306-second stage storage tank; 307-solvent recovery tank; 308-molecular distillation apparatus; 309-product storage tank; 310-waste storage tank; 311-pressure reduction system. Detailed Implementation
[0017] To facilitate understanding of this utility model, a more comprehensive description will be given below with reference to the accompanying drawings. The drawings illustrate preferred embodiments of this utility model. However, this utility model can be implemented in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided to provide a more thorough and complete understanding of the disclosure of this utility model.
[0018] Example
[0019] like Figs. 1-3 As shown, a continuous production system for substituted benzenesulfonyl isocyanate is disclosed. The production system includes a preparation system, an esterification reaction system, and a purification system. The preparation system includes a first preparation vessel 101 and a second preparation vessel 102. The esterification reaction system includes several reaction vessels connected in sequence. The first preparation vessel 101 and the second preparation vessel 102 are respectively connected to the first reaction vessel in the esterification reaction system. The purification system includes a primary solvent recovery system, a secondary solvent recovery system, and a distillation system. The solvents recovered in each solvent recovery system are collected in a solvent recovery tank 307. The last reaction vessel in the esterification reaction system is connected to the purification system.
[0020] like Fig. 1 As shown, the first preparation vessel 101 is used to prepare a bis(trichloromethyl) carbonate chlorobenzene solution, and the first preparation vessel 101 is equipped with a reflux system; the outlet of the first preparation vessel 101 is connected to the reaction vessel in the esterification reaction system through a pipeline. During the production process, the bis(trichloromethyl) carbonate chlorobenzene solution in the first preparation vessel 101 is refluxed while being quantitatively fed into the primary reaction vessel 201 through a metering pump and pipeline.
[0021] like Fig. 1 As shown, the second preparation vessel 102 is used to prepare a p-toluenesulfonamide chlorobenzene solution, and the second preparation vessel 102 is equipped with a reflux system; the outlet of the second preparation vessel 102 is connected to the reaction vessel in the esterification reaction system through a pipeline. During the production process, the p-toluenesulfonamide chlorobenzene solution in the second preparation vessel 102 is refluxed while being quantitatively fed into the primary reaction vessel 201 through a metering pump and pipeline.
[0022] As shown in Fig. 2 The esterification reaction system is three-stage, including first-stage reaction kettle 201, second-stage reaction kettle 202 and third-stage reaction kettle 203 connected in sequence; each stage reaction kettle is provided with a reflux system; in the production process, the reaction mixture is kept flowing at a certain flow rate between the reaction kettles. The reaction progress can be controlled by adjusting the flow rate, which is controlled and adjusted by the metering pump between the reaction kettles; and different reaction temperatures and other conditions can be set in each stage reaction kettle, and the whole esterification reaction is continuously carried out in the reaction kettles, which improves the production efficiency and the reaction efficiency.
[0023] As shown in Fig. 2 The esterification reaction system is three-stage, including first-stage reaction kettle 201, second-stage reaction kettle 202 and third-stage reaction kettle 203 connected in sequence; each stage reaction kettle is provided with a reflux system; in the production process, the reaction mixture is kept flowing at a certain flow rate between the reaction kettles. The reaction progress can be controlled by adjusting the flow rate, which is controlled and adjusted by the metering pump between the reaction kettles; and different reaction temperatures and other conditions can be set in each stage reaction kettle, and the whole esterification reaction is continuously carried out in the reaction kettles, which improves the production efficiency and the reaction efficiency.
[0024] As shown in Fig. 3 The first-stage solvent recovery system includes first-stage evaporator 301, first-stage condenser 302 and first-stage storage tank 303, and the first-stage evaporator 301 is a normal-pressure evaporator; the second-stage solvent recovery system includes second-stage evaporator 304, second-stage condenser 305 and second-stage storage tank 306, and the second-stage evaporator 304 is connected with the vacuum system 311; the discharge outlets of the first-stage condenser 302 and the second-stage condenser 305 are connected to the solvent recovery tank 307. The discharge outlet of the solvent recovery tank 307 is connected to the preparation system and the esterification reaction system through the metering pump and the pipeline. After the reaction product with solvent enters the first-stage solvent recovery system, most of the solvent chlorobenzene is recovered by normal-pressure distillation; then the reaction product continues to enter the second-stage solvent recovery system, and the solvent chlorobenzene is further recovered by vacuum distillation (vacuum degree: -0.08 to -0.095 Mpa). The recovered chlorobenzene is returned to the first preparation kettle 101, the second preparation kettle 102 and the first-stage reaction kettle 201 for reuse, and almost no process wastewater is generated in the whole production process.
[0025] As shown in Fig. 3 The distillation system includes molecular distiller 308, product storage tank 309 and waste storage tank 310, and the molecular distiller 308 is connected with the vacuum system 311. After the solvent is recovered, the remaining reaction product enters the molecular distiller 308 for high-vacuum distillation (vacuum degree: ≤-0.095 Mpa), and finally the product p-toluenesulfonyl isocyanate is collected in the product storage tank 309.
[0026] The production system provided in the embodiment is continuous from preparation of the raw material liquid, esterification reaction, solvent recovery and product refining, no interruption occurs in the middle, the product yield and purity are higher, and the safety performance is better.
[0027] The above embodiments are only used for describing the present application, and are not intended to limit the present application, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the present application, therefore, all equivalent technical solutions also belong to the scope of the present application, and the patent protection scope of the present application should be defined by the claims.
Claims
1. A continuous production system of substituted phenylsulfonylisocyanate, characterized by: The production system comprises a preparation system, an esterification reaction system and a refining system; the preparation system comprises a first preparation kettle and a second preparation kettle; the esterification reaction system comprises a plurality of reaction kettles, each of which is connected in sequence; the first preparation kettle and the second preparation kettle are connected with the first reaction kettle in the esterification reaction system respectively; the refining system comprises a primary solvent recovery system, a secondary solvent recovery system and a distillation system, and the solvent recovered in each solvent recovery system is collected in a solvent recovery tank; the last reaction kettle in the esterification reaction system is connected with the refining system.
2. A continuous production system of substituted phenylsulfonylisocyanate according to claim 1, characterized in that: The first preparation kettle is used for preparing a solution of bistrichloromethyl carbonate in chlorobenzene, and is provided with a reflux system; the discharge port of the first preparation kettle is connected with the reaction kettle in the esterification reaction system through a pipeline.
3. The continuous production system of substituted phenylsulfonyl isocyanate according to claim 1, wherein: The second preparation kettle is used for preparing a solution of a substituted benzene sulfonamide in chlorobenzene, and is provided with a reflux system; the discharge port of the second preparation kettle is connected with the reaction kettle in the esterification reaction system through a pipeline.
4. The continuous production system of substituted phenylsulfonylisocyanate according to claim 1, wherein: The esterification reaction system is three-stage, comprising a first-stage reaction kettle, a second-stage reaction kettle and a third-stage reaction kettle connected in sequence; each reaction kettle is provided with a reflux system; during production, the reaction mixture is kept flowing at a certain flow rate between the reaction kettles.
5. The continuous production system for substituted benzenesulfonyl isocyanate as described in claim 1, characterized in that: A buffer kettle is arranged between the esterification reaction system and the refining system; the buffer kettle is connected with the primary solvent recovery system in the refining system through a metering pump and a pipeline.
6. The continuous production system of substituted phenylsulfonylisocyanate according to claim 1, wherein: The primary solvent recovery system comprises a primary evaporator, a primary condenser and a primary storage tank, and the primary evaporator is a normal-pressure evaporator; the secondary solvent recovery system comprises a secondary evaporator, a secondary condenser and a secondary storage tank, and the secondary evaporator is connected with a vacuum system; the discharge ports of the primary condenser and the secondary condenser are connected to the solvent recovery tank.
7. The continuous production system of substituted phenylsulfonylisocyanate according to claim 1, wherein: The discharge port of the solvent recovery tank is connected to the preparation system and the esterification reaction system through a metering pump and a pipeline.
8. The continuous production system of substituted phenylsulfonylisocyanate according to claim 1, wherein: The distillation system comprises a molecular distiller, a product storage tank and a waste storage tank, and the molecular distiller is connected with a vacuum system.