Continuous reaction process and device for isophthaloyl chloride and paraphthaloyl chloride
By using a process of combining kettle and tower reactions in the preparation of aromatic acid chloride, the problems of low reaction efficiency and unstable product quality in the prior art are solved, efficient and stable reactions and high-purity products are achieved, and production costs and equipment operation and maintenance difficulties are reduced.
Patent Information
- Application Number
- CN202411982488.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-31
- Publication Date
- 2025-04-08
AI Technical Summary
In the prior art, the preparation method of aromatic acid chloride has problems such as low reaction efficiency, unstable product quality, low degree of equipment automation, and high labor intensity. Especially during large-scale production, the reaction is incomplete and impurities are difficult to separate, resulting in low production efficiency and high cost.
The process of combining kettle reaction and tower reaction is adopted, and the first-stage reactor and the second-stage reactor are premixed. Then the reaction liquid enters the reaction tower for high-temperature rapid reaction, and gas-phase sulfoxide chloride is used to regasification and participate in the reaction. Finally, the gas-phase sulfoxide chloride circulating reaction is condensed and replenished to ensure the complete reaction.
It achieves efficient and stable reactions, shortens the total reaction time, and stably produces high-purity inter-terephthalyl chloride, reduces the difficulty of equipment operation and maintenance and manpower investment, and improves production efficiency and product quality.
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Figure CN119775128A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a continuous reaction process and a device for isophthaloyl chloride / terephthaloyl chloride. Background Art
[0002] In the chemical industry, aromatic acyl chloride products, especially isophthaloyl chloride and terephthaloyl chloride, as a kind of important fine chemical intermediates, are widely used in the synthesis of high-performance polymer resins. These products play a core role as polymerization monomers in the production process of high value-added materials such as aramid fibers, aromatic polyesters, and polyaryletherketones. These polymer materials have shown broad application prospects in the fields of aerospace, automobile manufacturing, electronic information, and national defense science and technology due to their excellent physical and chemical properties.
[0003] However, aromatic acyl chloride products, which are monomers in polymerization reactions, have extremely high requirements for purity. Any trace of impurities may significantly affect the performance of the final polymer, and thus affect the quality and application value of the product. Therefore, developing an efficient and stable process for preparing aromatic acyl chlorides to ensure the high purity of the product has become the key to research in this field.
[0004] Traditional methods for preparing aromatic acyl chlorides include the thionyl chloride method, phosphorus trichloride method, phosphorus pentachloride method, and phosgene method. In my country, the thionyl chloride method and phosgene method are the mainstream production methods, and intermittent synthesis technology is mostly used. Although the intermittent method has high economic efficiency in small-scale production, its disadvantages gradually emerge with the expansion of production scale: unstable product quality, low degree of equipment automation, high labor intensity and other problems are becoming increasingly prominent.
[0005] To solve these problems, existing patents (such as CN2014105170371, CN211814213U) propose to use a continuous kettle reactor for continuous synthesis of acyl chlorides. However, this continuous synthesis method still faces the challenges of low reaction efficiency and unstable product quality. Traditional kettle reactions belong to full mixed flow reactions. As the reaction proceeds, the product concentration gradually increases and the reactant concentration gradually decreases, resulting in incomplete reaction in the later stages of the reaction. This will not only produce impurity monoacyl chlorides with a boiling point close to that of the target product, making it difficult to separate and purify the product by distillation, but also reduce the overall conversion rate and production efficiency of the reaction system.
[0006] In addition, traditional intermittent batch reactions usually require extended reaction time to ensure complete reactions, which not only reduces production efficiency but also increases energy consumption and production costs. Although traditional continuous batch reactions can theoretically improve production efficiency, in order to achieve complete reactions, it is often necessary to increase the number of series reactors, which not only makes the reaction system process more complicated, but also makes it difficult to ensure the consistency of conversion rates and product quality stability of each batch of products.
[0007] Therefore, the methods for preparing aromatic acyl chlorides in the prior art still have many deficiencies in terms of product quality, production efficiency, and process stability. Summary of the invention
[0008] The technical problem to be solved by the present invention is to overcome the above-mentioned defects of the prior art and provide a continuous reaction process for isophthaloyl chloride. The process adopts a combination of kettle reaction and tower reaction, and the reaction is efficient and stable, the reaction time is short, and high-purity isophthaloyl chloride can be stably produced. The present invention also provides an isophthaloyl chloride continuous reaction device, which reduces the difficulty of equipment operation and maintenance and manpower investment.
[0009] The isophthaloyl chloride continuous reaction process of the present invention comprises the following steps:
[0010] In the first step, isophthalic acid / terephthalic acid, catalyst, and thionyl chloride are quantitatively and continuously fed into a primary reactor, and a pre-mixing reaction is performed in the primary reactor and a secondary reactor;
[0011] In the second step, the reaction liquid from the secondary reactor is continuously and quantitatively fed to the reaction tower. The reaction tower has three sections of fillers. The reaction liquid reacts rapidly with the gaseous thionyl chloride at high temperature in the three sections of fillers. After each section of reaction fillers, the reaction liquid is collected by a liquid collector at the lower end of the fillers and heated by an intermediate heater to vaporize the thionyl chloride dissolved in the reaction liquid again and then re-participate in the reaction of the first section of fillers. Finally, the gaseous thionyl chloride circulating reaction at the top of the tower is condensed at the top of the tower and then reaches the thionyl chloride reaction circulation tank. One part of the gaseous thionyl chloride added into the reactor is replenished to the primary reactor according to the liquid level of the circulation tank, and the other part is metered, heated and vaporized by a vaporizer, and then injected into the bottom of the third section of the reaction tower to participate in the reaction, so as to finally obtain a crude product of isophthaloyl chloride / terephthaloyl chloride.
[0012] In the premixing reaction in the first step, the reaction pressure is controlled to be normal pressure, and the reaction temperatures of the first reactor and the second reactor are controlled to be 70-75°C.
[0013] The control temperature of the intermediate heater in the second step is 120-135°C.
[0014] The controlled temperature of the gas phase thionyl chloride in the second step is 120-135°C.
[0015] During the whole reaction process, the mass ratio of isophthalic acid in the first reactor to thionyl chloride in the first reactor is 1:2-3; during the whole reaction process, the mass ratio of isophthalic acid in the first reactor to thionyl chloride gasification in the reaction tower is 1:1-1.5.
[0016] The isophthaloyl chloride continuous reaction device used comprises a primary reactor, a secondary reactor and a reaction tower. The bottom of the primary reactor is connected to the top of the secondary reactor, the bottom of the secondary reactor is connected to the top of the reaction tower, the gas outlet at the top of the reaction tower is connected to a reaction circulation tank, and the liquid outlet of the reaction circulation tank is divided into two paths, one of which is connected to the top of the primary reactor and the other is connected to the bottom of the reaction tower.
[0017] The reaction tower is divided into a first section of packing, a second section of packing and a third section of packing. The first section of packing is provided with a gas / liquid distributor a, a liquid collector a and a heater a; the second section of packing is provided with a gas / liquid distributor b, a liquid collector b and a heater b; the third section of packing is provided with a gas / liquid distributor c, a liquid collector c and a heater c.
[0018] The gas outlet at the top of the reaction tower is provided with a condenser.
[0019] A gasifier is arranged on the pipeline connected to the bottom of the reaction tower from the other outlet of the reaction circulation tank.
[0020] Specifically, the isophthaloyl chloride continuous reaction process comprises the following steps:
[0021] In the first step, the raw acid (isophthalic acid / terephthalic acid), catalyst, and thionyl chloride are quantitatively and continuously fed to the primary reactor through a quantitative feeding facility, and a pre-mixed reaction is carried out in the primary reactor and the secondary reactor. The reaction pressure is controlled to be normal pressure, and the reaction temperature of the primary reactor and the secondary reactor is controlled to be 70-75° C. Since the two-stage reactor is in the initial stage of the reaction, the concentration of the reactants is high, and the reaction speed is less affected by the back mixing, the reaction can be fast, and the reaction liquid is mixed evenly at the same time.
[0022] In the second step, the reaction liquid from the secondary reactor is continuously and quantitatively fed to the reaction tower. The reaction tower has three sections of packing, each of which has a gas / liquid distributor, a liquid collector and a middle heater. The reaction liquid reacts rapidly with the gaseous thionyl chloride in the three sections of packing at high temperature. After each section of packing, the reaction liquid is collected by the liquid collector at the lower end of the packing and heated by the middle heater to vaporize the dissolved thionyl chloride in the reaction liquid again and then re-participate in the reaction of the upper packing reaction liquid. Finally, the gaseous thionyl chloride of the top tower circulation reaction is condensed by the top tower condenser to the thionyl chloride reaction circulation tank. One part of it is replenished to the first reactor according to the liquid level of the circulation tank. The other part is injected into the bottom of the third section of the packing of the reaction tower after being heated and vaporized by the vaporizer after metering to participate in the reaction, and finally a crude product of isophthaloyl chloride is obtained. The temperature of the middle heater is controlled at 120-135°C, and the temperature of the vaporizer of thionyl chloride is controlled at 120-135°C, and finally a crude reaction product containing a trace amount of thionyl chloride is obtained. During the whole reaction process, the mass ratio of isophthalic acid in the first reactor to thionyl chloride in the first reactor is 1:2-3; during the whole reaction process, the mass ratio of isophthalic acid in the first reactor to thionyl chloride gasification in the reaction tower is 1:1-1.5.
[0023] Compared with the prior art, the present invention has the following beneficial effects:
[0024] (1) Compared with the traditional kettle reaction, the kettle reaction has an obvious reaction rate disadvantage. Although the reaction is fast when the reactant concentration is high in the early stage, as the process progresses, the reaction gradually slows down due to the decrease in reactant concentration and accumulation of products, which greatly slows down the overall efficiency. The present invention innovatively adopts a process combining kettle and tower reactions to give full play to the advantages of both. In the kettle reaction stage, the good mixing characteristics allow the isophthalic acid to be quickly put into the reaction at the initial stage, quickly consume a large amount of raw materials, and efficiently complete most of the early conversion. At the same time, the reactants, products, and catalysts are evenly mixed. When the reaction enters the later stage and the speed slows down, the stable material flow and contact mode of the tower reaction is used to continuously promote the remaining small amount of isophthalic acid to participate in the reaction, thereby ensuring that the reaction is carried out at a high speed and stably throughout the process, greatly reducing the total reaction time.
[0025] (2) The continuous reaction process of isophthaloyl chloride of the present invention has strict requirements on the purity of the finished isophthaloyl chloride, which is difficult to meet with the traditional batch or continuous kettle reaction. The batch kettle reaction simply prolongs the reaction time, which is easy to cause side reactions and reduce the reaction yield; the continuous kettle reaction increases the residence time and requires too many reactors to be connected in series, resulting in a complicated process and an inability to ensure the conversion rate. The combined process of the present invention directly addresses the shortcomings of the traditional process. The kettle reaction performs preliminary chlorination and quickly converts the raw materials; the tower reaction relay, with its unique advantages of high mass transfer efficiency, low back mixing degree and large reaction processing capacity, allows the remaining small amount of unreacted isophthalic acid to continue to be chlorinated and completely converted into the finished product, avoiding the purity problem caused by the similar boiling point of the monoacyl chloride and the finished product and the difficulty in separation by distillation, and stably produces high-purity isophthaloyl chloride.
[0026] (3) The isophthaloyl chloride continuous reaction device of the present invention is usually trapped in a lengthy reaction cycle or a complex multi-reactor series system is built to achieve high conversion rate and high purity. The equipment purchase and maintenance costs are high, the space is large, the operation is cumbersome, and the energy consumption also rises accordingly. The reactor-tower combined reaction process of the present invention breaks the traditional reaction mode, cleverly avoids the complex continuous reactor system construction, reduces the number of reactors; shortens the overall reaction time, and reduces energy consumption; the streamlined process flow reduces the difficulty of equipment operation and maintenance and manpower investment, while ensuring product quality, comprehensively reducing production costs, and providing a highly cost-effective process solution for industrial large-scale production of isophthaloyl chloride. BRIEF DESCRIPTION OF THE DRAWINGS
[0027] Figure 1 It is a schematic diagram of the isophthaloyl chloride continuous reaction device of the present invention.
[0028] In the figure: 1, primary reactor; 2, secondary reactor;
[0029] 3. Reaction tower; 31. First stage packing; 311. Gas / liquid distributor a; 312. Liquid collector a; 313. Heater a;
[0030] 32. Second stage packing; 321. Gas / liquid distributor b; 322. Liquid collector b; 323. Heater b;
[0031] 33. third stage packing; 331. gas / liquid distributor c; 332. liquid collector c; 333. heater c;
[0032] 4. Condenser; 5. Reaction circulation tank; 6. Vaporizer. DETAILED DESCRIPTION
[0033] The present invention will be further described below in conjunction with specific embodiments.
[0034] like Figure 1 As shown, the isophthaloyl chloride continuous reaction device used includes a primary reactor 1, a secondary reactor 2, and a reaction tower 3. The bottom of the primary reactor 1 is connected to the top of the secondary reactor 2, the bottom of the secondary reactor 2 is connected to the top of the reaction tower 3, the top gas outlet of the reaction tower 3 is connected to a reaction circulation tank 5, and the liquid outlet of the reaction circulation tank 5 is divided into two paths, one of which is connected to the top of the primary reactor 1, and the other is connected to the bottom of the reaction tower 3.
[0035] The reaction tower 3 is divided into a first section packing 31, a second section packing 32, and a third section packing 33. The first section packing 31 is provided with a gas / liquid distributor a311, a liquid collector a312, and a heater a313; the second section packing 32 is provided with a gas / liquid distributor b321, a liquid collector b322, and a heater b323; the third section packing 33 is provided with a gas / liquid distributor c331, a liquid collector c332, and a heater c333.
[0036] The gas outlet at the top of the reaction tower 3 is provided with a condenser 4 .
[0037] A vaporizer 6 is provided on the pipeline connected to the bottom of the reaction tower 3 on the other side of the outlet of the reaction circulation tank 5 .
[0038] The following embodiments are all carried out using the above device.
[0039] Example 1
[0040] The described terephthaloyl chloride continuous reaction process comprises the following steps:
[0041] In the first step, terephthalic acid, DMF catalyst and thionyl chloride are quantitatively and continuously fed into the primary reactor 1 through a quantitative feeding facility, and a premixing reaction is carried out in the primary reactor 1 and the secondary reactor 2. The reaction pressure is controlled to be normal pressure, and the reaction temperature of the primary reactor 1 and the secondary reactor 2 is controlled to be 70° C., and the premixing reaction is started in the primary and secondary reactors.
[0042] Step 2: After maintaining a constant liquid level of the reaction liquid in the secondary reactor 2, the reactor begins to stably input the three-stage packing area of the reaction tower 3, and reacts rapidly with the gaseous thionyl chloride at high temperature. After each stage of packing, the liquid collector collects the reaction liquid, and the intermediate heater heats it to 120°C to vaporize the thionyl chloride, so that it re-participates in the reaction of the upper stage packing. The top gas phase of the tower is condensed to the reaction circulation tank 5 through the condenser 4, and is vaporized to 120°C under the premise of maintaining a constant flow rate into the vaporizer 6 and re-injected into the bottom of the third stage packing 33. The remaining thionyl chloride is re-injected into the primary reactor 1 according to the liquid level of the circulation tank. The mass ratio of the materials in the primary reactor is terephthalic acid: thionyl chloride = 1:2; the reaction tower is terephthalic acid: thionyl chloride gasification = 1:1.
[0043] Finally, a crude product containing 0.77% thionyl chloride, 0.008% monoacyl chloride and terephthalic acid (not detected) was obtained. According to experimental determination, this process takes 13.5 hours and the output reaches 370 kg / h. The same raw material processing as in the above example is compared with the intermittent reaction. It takes 25 hours to reach the same reaction liquid standard as in Example 1, and the output is 200 kg / h. The reaction time of the above Example 1 is reduced by 46% compared with the intermittent reaction, and the output far exceeds the intermittent reaction.
[0044] Example 2
[0045] The described terephthaloyl chloride continuous reaction process comprises the following steps:
[0046] Step 1: In the first step, terephthalic acid, DMF catalyst, and thionyl chloride are quantitatively and continuously fed to the primary reactor 1 through a quantitative feeding facility, and a premixing reaction is carried out in the primary reactor 1 and the secondary reactor 2. The reaction pressure is controlled to be normal pressure, and the reaction temperature of the primary reactor 1 and the secondary reactor 2 is controlled to be 75° C., and a premixing reaction is started in the primary and secondary reactors.
[0047] Step 2: After maintaining a constant liquid level of the reaction liquid in the secondary reactor 2, the reactor begins to stably input the three-stage packing area of the reaction tower 3, and reacts rapidly with the gaseous thionyl chloride at high temperature. After each stage of packing, the liquid collector collects the reaction liquid, and the intermediate heater heats it to 130°C to vaporize the thionyl chloride, so that it re-participates in the reaction of the upper stage packing. The top gas phase of the tower is condensed to the reaction circulation tank 5 through the condenser 4, and is vaporized to 130°C under the premise of maintaining a constant flow rate into the vaporizer 6 and then injected back into the bottom of the third stage packing 33. The remaining thionyl chloride is injected back into the primary reactor 1 according to the liquid level of the circulation tank. The mass ratio of the materials in the primary reactor is terephthalic acid: thionyl chloride = 1:3; the reaction tower is terephthalic acid: thionyl chloride gasification = 1:1.5.
[0048] Finally, a crude product containing 0.7% thionyl chloride, 0.006% monoacyl chloride and terephthaloyl chloride (not detected) was obtained. After testing, the reaction time was 12 hours and the output was 420 kg / h. Comparative Example 1 intermittent reactor required 25 hours to reach the same standard and the output was 200 kg / h. The reaction time of this embodiment was reduced by 52%.
[0049] Example 3
[0050] The isophthaloyl chloride continuous reaction process comprises the following steps:
[0051] Step 1: In the first step, isophthalic acid, DMF catalyst, and thionyl chloride are quantitatively and continuously fed to the primary reactor 1 through a quantitative feeding facility, and a premixing reaction is carried out in the primary reactor 1 and the secondary reactor 2. The reaction pressure is controlled to be normal pressure, and the reaction temperature of the primary reactor 1 and the secondary reactor 2 is controlled to be 75° C., and a premixing reaction is started in the primary and secondary reactors.
[0052] Step 2: After maintaining a constant liquid level of the reaction liquid in the secondary reactor 2, the reactor begins to stably input the three-stage packing area of the reaction tower 3, and reacts rapidly with the gaseous thionyl chloride at high temperature. After each stage of packing, the liquid collector collects the reaction liquid, and the intermediate heater heats it to 135°C to vaporize the thionyl chloride, so that it re-participates in the reaction of the upper stage packing. The top gas phase of the tower is condensed to the reaction circulation tank 5 through the condenser 4, and is vaporized to 135°C under the premise of maintaining a constant flow rate into the vaporizer 6 and re-injected into the bottom of the third stage packing 33. The remaining thionyl chloride is re-injected into the primary reactor 1 according to the liquid level of the circulation tank. The mass ratio of the materials in the primary reactor is isophthalic acid: thionyl chloride = 1:2; the reaction tower is isophthalic acid: thionyl chloride gasification = 1:1.5.
[0053] Finally, a crude product containing 0.68% thionyl chloride, 0.005% monoacyl chloride and isophthalic acid (not detected) was obtained. After precise measurement, the reaction time was 12.2 hours and the output was 410 kg / h. The intermittent reactor of Comparative Example 1 required 25 hours to reach this standard and the output was 200 kg / h. The reaction time of this embodiment was reduced by 51.2%.
[0054] Comparative Example 1
[0055] Experimental materials and equipment: terephthalic acid, DMF catalyst, thionyl chloride, using a traditional batch reactor reactor equipped with conventional components such as a stirrer, thermometer, condenser and collection device.
[0056] A reaction process of terephthaloyl chloride comprises the following steps:
[0057] Terephthalic acid, DMF catalyst, and thionyl chloride were added to the batch reactor in a similar proportion to that in Example 1, and the stirring and heating devices were turned on. The reaction temperature was controlled to 70°C and the pressure was maintained at normal pressure. Stirring was continued during the reaction. In order to make the reaction reach the same standard (impurity content, product yield and other key indicators) as the product in Example 1, it took 25 hours. This reaction period far exceeded the 13.5 hours in Example 1.
[0058] After the reaction, the reactor was cooled, the product was collected and the composition and content were analyzed. After testing, the product contained 35% thionyl chloride, 0.12% monoacyl chloride, and 0.10% terephthalic acid, and the impurity content was significantly higher than that of the product in Example 1. Although the long-term reaction promoted the conversion of some raw materials, the reaction rate dropped sharply due to the low concentration of reactants and product accumulation in the later stage of the reaction, side reactions occurred frequently, impurities increased, and the product quality and purity were far inferior to those of the product in Example 1, which clearly highlighted the outstanding advantages of the continuous reaction process of the present invention in greatly shortening the reaction time and improving product quality.
[0059] Comparative Example 2
[0060] Experimental materials and equipment: terephthalic acid, DMF catalyst, thionyl chloride, using three continuous kettle reaction devices connected in series, each kettle has equal volume, and the kettles are connected by pipes to ensure continuous and stable flow of materials. They are equipped with independent agitators, thermometers, feed pumps, discharge pumps and other precision control components to strictly control material flow and reaction conditions.
[0061] A reaction process of terephthaloyl chloride comprises the following steps:
[0062] The raw material mixture was accurately configured to maintain a mass ratio of terephthalic acid to thionyl chloride of 1:2.5 (near the mass ratio range of the inventive process), and was continuously and stably fed into the first kettle at a specific flow rate through a feed pump, and the reaction temperature of each kettle was controlled to be 70°C and normal pressure, and the total residence time of the materials in the reaction system was finely adjusted to 18h (based on the optimization experience of traditional continuous kettle reactions, this time is longer than that in Example 1).
[0063] During the reaction process, the material is pushed from the first kettle to the second and third kettles in an orderly manner by means of a discharge pump for continuous reaction, and the product is finally collected from the last kettle for testing. The analysis results show that the product contains 37% thionyl chloride, 0.24% monoacyl chloride, and 0.13% terephthalic acid, and the purity is inferior to the product of Example 1 of the present invention. Although continuous feeding improves efficiency, in order to achieve a higher conversion rate, multiple kettles need to be connected in series and the residence time is extended, resulting in a complex process, a large area of equipment, and high energy consumption. In addition, the reaction progress of each kettle is difficult to synchronize accurately, resulting in poor product quality stability and consistency, which effectively demonstrates the outstanding advantages and advancement of the kettle-tower combination process of the present invention in simplifying the process, stabilizing product quality, and reducing energy consumption.
Claims
1. A continuous reaction process of isophthaloyl chloride / terephthaloyl chloride, characterized in that: The following steps are involved: In the first step, isophthalic acid / terephthalic acid, catalyst, and thionyl chloride are quantitatively and continuously fed into a primary reactor, and a pre-mixing reaction is performed in the primary reactor and a secondary reactor; In the second step, the reaction liquid from the secondary reactor is quantitatively fed into the reaction tower. The reaction tower has three sections of fillers. The reaction liquid reacts quickly with the gaseous thionyl chloride in the three sections of fillers. After each section of reaction fillers, the reaction liquid is collected by a liquid collector at the lower end of the fillers and heated by an intermediate heater to vaporize the thionyl chloride dissolved in the reaction liquid again and then re-participate in the reaction of the first section of fillers. Finally, the gaseous thionyl chloride circulating reaction at the top of the tower is condensed at the top of the tower and then enters the thionyl chloride reaction circulation tank. A part of the thionyl chloride in the circulation tank is returned to the primary reactor, and the other part of the thionyl chloride is vaporized and returned to the bottom of the third section of fillers to participate in the reaction, so as to finally obtain a crude isophthaloyl chloride / terephthaloyl chloride product.
2. The continuous reaction process of isophthaloyl chloride according to claim 1, characterized in that: In the premixing reaction in the first step, the reaction pressure is controlled to be normal pressure, and the reaction temperatures of the first reactor and the second reactor are controlled to be 70-75°C.
3. The continuous reaction process of isophthaloyl chloride according to claim 1, characterized in that: The control temperature of the intermediate heater in the second step is 120-135°C.
4. The continuous reaction process of isophthaloyl chloride / terephthaloyl chloride according to claim 1, characterized in that: The controlled temperature of the gas phase thionyl chloride in the second step is 120-135°C.
5. The continuous reaction process of isophthaloyl chloride / terephthaloyl chloride according to claim 1, characterized in that: During the whole reaction process, the mass ratio of isophthalic acid in the first reactor to thionyl chloride in the first reactor is 1:2-3; during the whole reaction process, the mass ratio of isophthalic acid in the first reactor to thionyl chloride gasification in the reaction tower is 1:1-1.
5.
6. A reaction device used in the continuous reaction process of isophthaloyl chloride / terephthaloyl chloride according to any one of claims 1 to 5, characterized in that: The invention comprises a primary reactor (1), a secondary reactor (2), and a reaction tower (3), wherein the bottom of the primary reactor (1) is connected to the top of the secondary reactor (2), the bottom of the secondary reactor (2) is connected to the top of the reaction tower (3), the gas outlet at the top of the reaction tower (3) is connected to a reaction circulation tank (5), and the liquid outlet of the reaction circulation tank (5) is divided into two paths, one of which is connected to the top of the primary reactor (1) and the other is connected to the bottom of the reaction tower (3).
7. The reaction device used in the continuous reaction process of isophthaloyl chloride according to claim 6 is characterized in that: The reaction tower (3) is divided into a first section of fillers (31), a second section of fillers (32), and a third section of fillers (33). The first section of fillers (31) is provided with a gas / liquid distributor a (311), a liquid collector a (312), and a heater a (313); the second section of fillers (32) is provided with a gas / liquid distributor b (321), a liquid collector b (322), and a heater b (323); the third section of fillers (33) is provided with a gas / liquid distributor c (331), a liquid collector c (332), and a heater c (333).
8. The reaction device used in the continuous reaction process of isophthaloyl chloride according to claim 6 is characterized in that: The gas outlet at the top of the reaction tower (3) is provided with a condenser (4).
9. The reaction device used in the continuous reaction process of isophthaloyl chloride according to claim 6, characterized in that: A vaporizer (6) is provided on the pipeline connected to the bottom of the reaction tower (3) from the other outlet of the reaction circulation tank (5).
Citation Information
Patent Citations
Continuous production device of isophthaloyl dichloride / paraphthaloyl chloride
CN211814213U