Application of rosin ester compound in synthesis process of copper phthalocyanine
By adding rosin ester compounds to the synthesis of copper phthalocyanine, the compatibility of materials was optimized, the problem of incomplete reaction in the copper phthalocyanine synthesis system was solved, the product yield and purity were improved, the raw material loss and the generation of waste were reduced, and a highly efficient and environmentally friendly synthesis was achieved.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-02-02
- Publication Date
- 2026-04-21
AI Technical Summary
Poor compatibility of multiple materials in the copper phthalocyanine synthesis system leads to incomplete reaction, affecting product yield efficiency, quality, and raw material utilization efficiency.
Rosin esters were added to the copper phthalocyanine synthesis process along with phthalic anhydride, urea, and solvent alkylbenzene into the reaction system. The material compatibility was optimized by multi-stage heating and holding reaction, and the solvent was recovered in the subsequent processing to reduce impurity interference.
It improved product yield and purity, reduced raw material loss and waste generation, and enhanced production efficiency and environmental friendliness.
Smart Images
Figure CN121895324A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of copper phthalocyanine synthesis technology, and in particular to the application of rosin ester compounds in the synthesis of copper phthalocyanine. Background Technology
[0002] Copper phthalocyanine synthesis is the core organic synthesis process for the large-scale preparation of copper phthalocyanine. It uses phthalic anhydride, phthalonitrile, etc. as raw materials for phthalocyanine ring construction, copper salts such as cuprous chloride as copper sources, and ammonia sources such as urea and various auxiliaries. Phthalocyanine macrocycles are formed through condensation and cyclization reactions and chelated with copper ions. There are two main methods: solid-phase baking and liquid-phase solvent method. The crude product obtained from the reaction is purified by post-treatment such as acid washing and grinding, and finally the finished copper phthalocyanine is obtained. It is an important production process in dye and pigment chemical industry.
[0003] Rosin esters are ester derivatives obtained by esterification of natural rosin with alcohols. They belong to the category of natural resin chemical auxiliaries. Their molecules combine the terpene skeleton and ester bond structure of rosin, exhibiting good dispersibility and compatibility. In the synthesis of copper phthalocyanine, these compounds can optimize the compatibility of various reactants, reduce the probability of solid raw material agglomeration, improve the dispersibility of the reaction system, promote the full progress of condensation and cyclization reactions, reduce solvent loss, help improve the yield and purity of copper phthalocyanine products, and stabilize the reaction effect of the synthesis process.
[0004] The copper phthalocyanine synthesis system contains a variety of materials such as phthalic anhydride, urea, and solvent alkylbenzene. These materials have poor compatibility, which can easily lead to incomplete reaction and thus affect the product yield, quality, and raw material utilization efficiency.
[0005] Therefore, it is necessary to provide solutions to the above-mentioned technical problems by applying rosin ester compounds in the synthesis of copper phthalocyanine. Summary of the Invention
[0006] This invention provides the application of rosin ester compounds in the synthesis of copper phthalocyanine, solving the problem that poor compatibility of multiple materials in the copper phthalocyanine synthesis system makes it difficult for the reaction to proceed fully, affecting product yield efficiency, quality, and raw material utilization efficiency.
[0007] To solve the above-mentioned technical problems, the application of rosin ester compounds in the synthesis of copper phthalocyanine provided by this invention includes the following steps: S1: Material preparation: In a 3000 ml three-necked synthesis tank equipped with a stirrer, thermometer, and condenser, add 100% rosin ester compound, 310 g of 100% phthalic anhydride, 231 g of urea, and 1500 ml of solvent alkylbenzene to complete the initial material feeding. S2: Initial heating and heat preservation, while maintaining stirring, to uniformly heat the system to 170℃ over 4 hours, and then maintain the temperature for 2 hours after reaching the temperature. S3: Add urea for a second heating and heat preservation. Add 231 grams of urea to the system, then heat the system evenly to 190°C, and keep it at a constant temperature for 2 hours after reaching the temperature. S4: Add catalyst material and heat up and hold for three times. Add 61 g of 100% cuprous chloride and 4 g of 100% ammonium molybdate to the system and keep stirring. Heat the system to 210°C uniformly over 5 hours. After reaching the temperature, keep the system at the temperature and stir for 6 hours. S5: Cool the system and add alkali. Cool the reacted system to 100°C and add 50g of 30% sodium hydroxide solution to complete the initial post-treatment preparation. S6: Steam distillation to recover the solvent. Steam is passed into the system to distill and recover the solvent alkylbenzene. Distillation is continued for about 5 hours until no more solvent is distilled off, at which point the distillation operation is ended. S7: The product post-processing yields the final product. The distilled system is sequentially filtered, washed with water, and dried to finally obtain the copper phthalocyanine product. 295 grams of copper phthalocyanine with a purity of 90% and a yield of 88% can be obtained. The addition of rosin ester compounds needs to be strictly controlled, preferably at 0.1-10% of the total phthalic anhydride. Specific types such as rosin methyl ester, ethyl ester, and n-propyl ester can be selected according to actual synthesis needs, and the dosage can be flexibly adjusted. This compound needs to be added simultaneously with phthalic anhydride, urea, and solvent alkylbenzene in the initial feeding stage to quickly integrate into the system, avoiding material stratification or incomplete local reactions. This allows for more uniform reactions during subsequent multi-stage heating and holding processes. Its unique chemical structure can optimize the dispersion of the reaction system, reduce the local aggregation of catalysts cuprous chloride and ammonium molybdate, and improve catalytic efficiency. At the same time, it reduces impurities in subsequent alkali treatment, solvent recovery, and product purification stages. Ultimately, while improving product yield and purity, it further reduces raw material loss and waste generation, meeting the high-efficiency and environmentally friendly synthesis requirements of copper phthalocyanine.
[0008] Preferably, the synthesis tank used in S1-S7 is characterized by including a mounting base; A synthesis tank is mounted on top of a mounting base via a bracket. A condensation assembly is mounted on the top of the synthesis tank and the top of the mounting base. A primary gas inlet assembly, a secondary gas inlet assembly, and a tertiary gas inlet assembly are respectively installed at the three inlets of the condensation assembly. Multiple drain pipes are installed on the front of the condensation assembly. The other ends of the primary gas inlet assembly, the secondary gas inlet assembly, and the tertiary gas inlet assembly are connected to the primary synthesis tank, the secondary synthesis tank, and the tertiary synthesis tank in the synthesis tank, respectively, so that the generated gas can enter the multi-stage condensation assembly.
[0009] Preferably, a drive structure is installed on the top of the synthesis tank, and a stirring assembly is installed at the output end of the drive structure.
[0010] Preferably, the stirring assembly includes a rotating shaft, multiple stirring racks, and multiple fixing racks, wherein the multiple fixing racks are used to mount the multiple stirring racks on the outer surface of the rotating shaft; Each fixed rack has a set of mixing racks, which can be used for simultaneous mixing inside multi-stage synthesis tanks.
[0011] Preferably, a feed pipe is installed at the top of the synthesis tank, and a discharge assembly is installed at the bottom of the synthesis tank. The discharge assembly includes a valve and a discharge pipe, and the valve is used to install the discharge pipe at the bottom of the synthesis tank. There are multiple feed pipes, allowing different materials to enter separately.
[0012] Preferably, the mounting base includes a base plate, a mounting structure, and an adjustment structure, wherein the mounting structure is used to mount the adjustment structure on the bottom of the base plate; The threaded connection of the mounting and adjusting structure allows for adjustment of the stability of the base plate as needed.
[0013] Preferably, a control box with a door is installed on the top of the mounting base, and an operation panel is installed on one side of the control box.
[0014] Preferably, the synthesis tank includes a primary synthesis tank, a secondary synthesis tank, and a tertiary synthesis tank, and the connecting ring is used to install the primary synthesis tank, the connecting ring, the secondary synthesis tank, and the tertiary synthesis tank together; The synthesis tank has heating equipment that can independently heat multiple synthesis tanks, and the synthesis tank is equipped with multiple sensors that can independently monitor the temperature.
[0015] Preferably, the condensation assembly includes a condenser, a liquid inlet pipe, and a liquid outlet pipe, wherein the liquid inlet pipe and the liquid outlet pipe are installed at the inlet and outlet of the condenser.
[0016] Preferably, the primary gas inlet assembly includes an inlet pipe, a valve, and a connecting pipe. The connecting pipe is installed at the gas inlet of the condensation assembly, and the valve is used to connect the inlet pipe to the other end of the connecting pipe.
[0017] Compared with related technologies, the application of rosin ester compounds provided by this invention in the synthesis of copper phthalocyanine has the following beneficial effects: This invention provides the application of rosin ester compounds in the synthesis of copper phthalocyanine. In the initial stage of synthesis, the compound is added to the reaction system along with phthalic anhydride, urea, and solvent alkylbenzene. This effectively improves the compatibility between the materials, creating a better reaction environment for subsequent steps such as heating to 170°C for 4 hours, heating to 190°C after adding urea, and heating to 210°C after adding a catalyst. This promotes a more complete reaction, increasing the product yield by 3-5% compared to the case without the addition, up to a maximum of 93%. Simultaneously, the product content is optimized from 90% to 91.5%-92%, resulting in more stable purity and quality. Furthermore, the improved reaction sufficiency reduces raw material waste, lowers the raw material consumption per unit of product, and reduces byproducts. In subsequent post-processing steps such as solvent recovery via steam distillation, filtration, washing, and drying, the emissions of waste gas, wastewater, and solid waste are correspondingly reduced, balancing production efficiency, product quality, and environmental requirements. Attached Figure Description
[0018] Figure 1 A schematic diagram of the structure of a first embodiment of the application of rosin ester compounds provided by the present invention in the synthesis of copper phthalocyanine; Figure 2 A schematic diagram of the general formula of rosin ester compounds is provided for this invention; Figure 3 A schematic diagram of the structure of the eighth embodiment of the application of the rosin ester compounds provided by the present invention in the synthesis of copper phthalocyanine; Figure 4 A schematic diagram of the base plate is provided for this invention; Figure 5 Provided for the present invention Figure 3 An enlarged view of point A shown; Figure 6 Provided for the present invention Figure 4 An enlarged view of point B shown; Figure 7 Provided for the present invention Figure 4 A magnified view of point C shown.
[0019] The diagram is labeled as follows: 1. Mounting base frame, 101. Base plate, 102. Mounting structure, 103. Adjustment structure, 2. Support, 3. Discharge assembly, 301. Valve, 302. Discharge pipe, 4. Synthesis tank, 401. Primary synthesis tank, 402. Connecting ring, 403. Secondary synthesis tank, 404. Tertiary synthesis tank, 5. Feed pipe, 6. Drive structure, 7. Primary gas inlet assembly, 701. Inlet pipe, 702. Valve, 703. Connecting pipe, 8. Secondary gas inlet assembly, 9. Condensation assembly, 901. Condenser, 902. Liquid inlet pipe, 903. Liquid discharge pipe, 10. Drain pipe, 11. Tertiary gas inlet assembly, 12. Control box, 13. Stirring assembly, 131. Rotating shaft, 132. Stirring frame, 133. Fixing frame, 14. Box door, 15. Operation panel. Detailed Implementation
[0020] The present invention will be further described below with reference to the accompanying drawings and embodiments.
[0021] First Embodiment Please refer to the following: Figure 1 , Figure 2 ,in, Figure 1 A schematic diagram of the structure of a first embodiment of the application of rosin ester compounds provided by the present invention in the synthesis of copper phthalocyanine; Figure 2 A schematic diagram of the general formula of rosin ester compounds is provided for this invention. The specific method for the application of rosin ester compounds in the synthesis of copper phthalocyanine is as follows: In a 3000 mL three-necked flask equipped with a stirrer, thermometer, and condenser, add 310 g of 100% phthalic anhydride, 231 g of urea, and 1500 mL of alkylbenzene solvent. While stirring, uniformly raise the temperature to 170 °C over 4 hours and maintain this temperature for 2 hours. Add 231 g of urea, uniformly raise the temperature to 190 °C over 1 hour and maintain this temperature for 2 hours. Add 61 g of 100% cuprous chloride and 4 g of 100% ammonium molybdate, uniformly raise the temperature to 210 °C over 5 hours, maintain this temperature, and stir for 6 hours. Cool to 100 °C, add 50 g of 30% sodium hydroxide solution, and steam distill to recover the alkylbenzene solvent. After approximately 5 hours, no more solvent flows out. Once distillation is complete, filter, wash with water, and dry to obtain copper phthalocyanine.
[0022] The working principle of the rosin ester compounds provided by this invention in the synthesis of copper phthalocyanine is as follows: In a 3000 mL three-necked flask equipped with a stirrer, thermometer, and condenser, 100% rosin ester compound, 310 g phthalic anhydride, 231 g urea, and 1500 mL alkylbenzene solvent were added. The mixture was stirred and heated uniformly to 170 °C over 4 hours, then held at that temperature for 2 hours. 231 g urea was added, and the mixture was heated uniformly to 190 °C over 1 hour and held at that temperature for 2 hours. 61 g cuprous chloride and 4 g ammonium molybdate were added, and the mixture was heated uniformly to 210 °C over 5 hours. The mixture was stirred and held at that temperature for 6 hours, then cooled to 100 °C. 50 g 30% sodium hydroxide solution was added, and the alkylbenzene solvent was recovered by steam distillation. After about 5 hours, no more solvent flowed out. The distillation was completed, and the mixture was filtered, washed with water, and dried to obtain copper phthalocyanine.
[0023] Compared with related technologies, the application of rosin ester compounds provided by this invention in the synthesis of copper phthalocyanine has the following beneficial effects: In the initial stage of synthesis, this compound is added to the reaction system along with phthalic anhydride, urea, and the solvent alkylbenzene. This effectively improves the compatibility between the materials, creating a better reaction environment for subsequent steps such as heating to 170°C for 4 hours and holding, heating to 190°C after adding urea and holding, and heating to 210°C after adding the catalyst. This promotes a more complete reaction, increasing the product yield by 3-5% compared to the case without the addition, up to a maximum of 93%. At the same time, the product content is optimized from 90% to 91.5%-92%, with more stable purity and quality. In addition, the improved reaction sufficiency reduces raw material waste and lowers the raw material consumption per unit of product. Furthermore, the reduction of by-products leads to a corresponding decrease in the emission of waste gas, wastewater, and solid waste in subsequent post-processing steps such as solvent recovery by steam distillation, filtration, washing, and drying. This approach balances production efficiency, product quality, and environmental protection requirements.
[0024] Second Embodiment The specific method for applying the formamide compounds in the synthesis of copper phthalocyanine based on this application is as follows: In a 3000 mL three-necked flask equipped with a stirrer, thermometer, and condenser, 3 g of rosin methyl ester, 310 g of 100% phthalic anhydride, 231 g of urea, and 1500 mL of alkylbenzene solvent were added. The mixture was stirred and heated uniformly to 170 °C over 4 hours, then held at that temperature for 2 hours. 231 g of urea was added, and the mixture was heated uniformly to 190 °C over 1 hour and held at that temperature for 2 hours. 61 g of 100% cuprous chloride and 4 g of 100% ammonium molybdate were added, and the mixture was heated uniformly to 210 °C over 5 hours, held at that temperature, and stirred for 6 hours. The mixture was then cooled to 100 °C. 50 g of 30% sodium hydroxide solution was added, and the alkylbenzene solvent was recovered by steam distillation. After approximately 5 hours, no solvent was evaporating. The mixture was then filtered, washed with water, and dried to obtain 305 g of copper phthalocyanine with a purity of 92% and a yield of 93%.
[0025] Third Embodiment The specific method for applying the formamide compounds in the synthesis of copper phthalocyanine based on this application is as follows: In a 3000 mL three-necked flask equipped with a stirrer, thermometer, and condenser, 1 g of rosin ethyl ester, 310 g of 100% phthalic anhydride, 231 g of urea, and 1500 mL of solvent alkylbenzene are added. Under stirring, the temperature is uniformly raised to 170 °C over 4 hours and held for 2 hours. Then, 231 g of urea is added, and the temperature is uniformly raised to 190 °C over 1 hour and held for 2 hours. Next, 61 g of 100% cuprous chloride and 4 g of 100% ammonium molybdate are added, and the temperature is uniformly raised to 210 °C over 5 hours. The reaction is stirred and held for 6 hours, then cooled to 100 °C. 50 g of 30% sodium hydroxide solution is added, and the solvent alkylbenzene is recovered by steam distillation. After about 5 hours, no solvent flows out. After distillation, the mixture is filtered, washed with water, and dried to obtain 300 g of copper phthalocyanine with a purity of 92% and a yield of 91.5%.
[0026] Fourth embodiment The specific method for applying the formamide compounds in the synthesis of copper phthalocyanine based on this application is as follows: In a 3000 mL three-necked flask equipped with a stirrer, thermometer, and condenser, 2 g of rosin n-propyl ester, 310 g of 100% phthalic anhydride, 231 g of urea, and 1500 mL of solvent alkylbenzene were added. The mixture was stirred and heated uniformly to 170 °C over 4 hours, and held at that temperature for 2 hours. Then, 231 g of urea was added, and the mixture was heated uniformly to 190 °C over 1 hour and held at that temperature for 2 hours. Next, 61 g of 100% cuprous chloride and 4 g of 100% ammonium molybdate were added, and the mixture was heated uniformly to 210 °C over 5 hours. The mixture was stirred and held at that temperature for 6 hours, and then cooled to 100 °C. 50 g of 30% sodium hydroxide solution was added, and the solvent alkylbenzene was recovered by steam distillation. After about 5 hours, no solvent was evaporating. The mixture was then filtered, washed with water, and dried to obtain 304 g of copper phthalocyanine with a purity of 92% and a yield of 92.7%.
[0027] Fifth embodiment The specific method for applying the formamide compounds in the synthesis of copper phthalocyanine based on this application is as follows: In a 3000 mL three-necked flask equipped with a stirrer, thermometer, and condenser, 5 g of rosin isopropyl ester, 310 g of 100% phthalic anhydride, 231 g of urea, and 1500 mL of solvent alkylbenzene were added. The mixture was stirred and heated uniformly to 170 °C over 4 hours, and held at that temperature for 2 hours. Then, 231 g of urea was added, and the mixture was heated uniformly to 190 °C over 1 hour and held at that temperature for 2 hours. Next, 61 g of 100% cuprous chloride and 4 g of 100% ammonium molybdate were added, and the mixture was heated uniformly to 210 °C over 5 hours. The mixture was stirred and held at that temperature for 6 hours, and then cooled to 100 °C. 50 g of 30% sodium hydroxide solution was added, and the solvent alkylbenzene was recovered by steam distillation. After about 5 hours, no solvent was evaporating. The mixture was then filtered, washed with water, and dried to obtain 305 g of copper phthalocyanine with a purity of 91.5% and a yield of 92.5%.
[0028] Sixth Embodiment The specific method for applying the formamide compounds in the synthesis of copper phthalocyanine based on this application is as follows: In a 3000 mL three-necked flask equipped with a stirrer, thermometer, and condenser, 3 g of rosin n-butyl ester, 310 g of 100% phthalic anhydride, 231 g of urea, and 1500 mL of solvent alkylbenzene were added. The mixture was stirred and heated uniformly to 170 °C over 4 hours, and held at that temperature for 2 hours. Then, 231 g of urea was added, and the mixture was heated uniformly to 190 °C over 1 hour and held at that temperature for 2 hours. Then, 61 g of 100% cuprous chloride and 4 g of 100% ammonium molybdate were added, and the mixture was heated uniformly to 210 °C over 5 hours. The mixture was stirred and held at that temperature for 6 hours, and then cooled to 100 °C. 50 g of 30% sodium hydroxide solution was added, and the solvent alkylbenzene was recovered by steam distillation. After about 5 hours, no solvent flowed out. After distillation, the mixture was filtered, washed with water, and dried to obtain 305 g of copper phthalocyanine with a purity of 92% and a yield of 93%.
[0029] Seventh Embodiment The specific method for applying the formamide compounds in the synthesis of copper phthalocyanine based on this application is as follows: In a 3000 mL three-necked flask equipped with a stirrer, thermometer, and condenser, 3 g of rosin isobutyl ester, 310 g of 100% phthalic anhydride, 231 g of urea, and 1500 mL of solvent alkylbenzene were added. The mixture was stirred and heated uniformly to 170 °C over 4 hours, and held at that temperature for 2 hours. Then, 231 g of urea was added, and the mixture was heated uniformly to 190 °C over 1 hour and held at that temperature for 2 hours. Next, 61 g of 100% cuprous chloride and 4 g of 100% ammonium molybdate were added, and the mixture was heated uniformly to 210 °C over 5 hours. The mixture was stirred and held at that temperature for 6 hours, and then cooled to 100 °C. 50 g of 30% sodium hydroxide solution was added, and the solvent alkylbenzene was recovered by steam distillation. After about 5 hours, no solvent was evaporating. The mixture was then filtered, washed with water, and dried to obtain 305 g of copper phthalocyanine with a purity of 92% and a yield of 93%.
[0030] Eighth embodiment Please refer to the following: Figures 3-4 - Figures 5-6 - Figure 7 , Figure 3 A schematic diagram of the structure of the eighth embodiment of the application of the rosin ester compounds provided by the present invention in the synthesis of copper phthalocyanine; Figure 4 A schematic diagram of the base plate is provided for this invention; Figure 5 Provided for the present invention Figure 3 An enlarged view of point A shown; Figure 6 Provided for the present invention Figure 4 An enlarged view of point B shown; Figure 7 Provided for the present invention Figure 4The enlarged view at point C shows the application of rosin ester compounds in the synthesis of copper phthalocyanine based on the eighth embodiment of this application. The eighth embodiment of this application proposes the application of other rosin ester compounds in the synthesis of copper phthalocyanine. The eighth embodiment is merely a preferred embodiment of the first embodiment, and its implementation will not affect the individual implementation of the first embodiment.
[0031] Specifically, the application of rosin ester compounds in the synthesis process of copper phthalocyanine provided in the eighth embodiment of this application is different in that the synthesis tank used in S1-S7 is characterized by including a mounting base 1; Synthesis tank 4 is mounted on top of mounting base 1 via bracket 2. A condensation assembly 9 is mounted on top of the synthesis tank 4 and the top of mounting base 1. A primary gas inlet assembly 7, a secondary gas inlet assembly 8 and a tertiary gas inlet assembly 11 are respectively installed at the three inlets of the condensation assembly 9. Multiple drain pipes 10 are installed on the front of the condensation assembly 9. The other ends of the primary gas inlet assembly 7, the secondary gas inlet assembly 8, and the tertiary gas inlet assembly 11 are respectively connected to the primary synthesis tank 401, the secondary synthesis tank 403, and the tertiary synthesis tank 4 in the synthesis tank 4, so that the generated gas can enter the multi-stage condensation assembly 9. Multiple drain pipes 10 are respectively connected to the other ends of the primary gas inlet assembly 7, the secondary gas inlet assembly 8, and the tertiary gas inlet assembly 11, so that the condensed liquid can be discharged separately.
[0032] Please refer to Figure 3 and Figure 4 The top of the synthesis tank 4 is equipped with a drive structure 6, and the output end of the drive structure 6 is equipped with a stirring assembly 13. The stirring assembly 13 is located inside the synthesis tank 4, and the drive structure 6 includes a housing and a motor.
[0033] Please refer to Figure 4 and Figure 6 The stirring assembly 13 includes a rotating shaft 131, a plurality of stirring racks 132 and a plurality of fixing racks 133, wherein the plurality of fixing racks 133 are used to mount the plurality of stirring racks 132 on the outer surface of the rotating shaft 131; Each fixed frame 133 has a set of stirring racks 132, which can be used for simultaneous mixing inside a multi-stage synthesis tank.
[0034] Please refer to Figure 4 and Figure 5 The top of the synthesis tank 4 is equipped with a feed pipe 5, and the bottom of the synthesis tank 4 is equipped with a discharge assembly 3. The discharge assembly 3 includes a valve 301 and a discharge pipe 302. The valve 301 is used to install the discharge pipe 302 at the bottom of the synthesis tank 4. The feed pipe 5 has multiple feed pipes, allowing different materials to enter separately.
[0035] Please refer to Figure 3 and Figure 4 The mounting base 1 includes a base plate 101, a mounting structure 102, and an adjustment structure 103. The mounting structure 102 is used to mount the adjustment structure 103 on the bottom of the base plate 101. The threaded connection between the mounting structure 102 and the adjusting structure 103 allows for adjustment of the stability of the base plate 101 as needed.
[0036] Please refer to Figure 3 , Figure 4 and Figure 5 A control box 12 with a door 14 is installed on the top of the mounting base 1, and an operation panel 15 is installed on one side of the control box 12. The control panel 15 displays the equipment's operating parameters. The door 14 is equipped with a lock. The control box 12 contains a power switch and a controller for the operation of auxiliary equipment.
[0037] Please refer to Figure 3 and Figure 4 The synthesis tank 4 includes a primary synthesis tank 401, a secondary synthesis tank 403, and a tertiary synthesis tank 404. The connecting ring 402 is used to install the primary synthesis tank 401, the connecting ring 402, the secondary synthesis tank 403, and the tertiary synthesis tank 404 together. Synthesis tank 4 has heating equipment that can independently heat multiple synthesis tanks, and synthesis tank 4 is equipped with multiple sensors that can independently monitor the temperature.
[0038] Please refer to Figure 3 and Figure 4 The condensation assembly 9 includes a condenser 901, a liquid inlet pipe 902, and a liquid outlet pipe 903, wherein the liquid inlet pipe 902 and the liquid outlet pipe 903 are installed at the inlet and outlet of the condenser 901. The condenser 901 has a multi-stage assembly structure, which can achieve condensation at different temperatures for the primary gas inlet component 7, the secondary gas inlet component 8, and the tertiary gas inlet component 11, thereby enabling the gas generated during synthesis to be recovered, condensed, and separated in a timely manner for convenient subsequent use.
[0039] Please refer to Figure 4 and Figure 7 The primary gas inlet assembly 7 includes an inlet pipe 701, a valve 702, and a connecting pipe 703. The connecting pipe 703 is installed at the gas inlet of the condensation assembly 9, and the valve 702 is used to connect the inlet pipe 701 to the other end of the connecting pipe 703. The other end of the inlet pipe 701 is connected to the gas outlet of the synthesis tank 4.
[0040] Compared with related technologies, the application of rosin ester compounds provided by this invention in the synthesis of copper phthalocyanine has the following beneficial effects: To improve the liquid recovery rate of rosin ester compounds during the synthesis of copper phthalocyanine, a multi-layer condenser assembly 9 is used. Then, through a primary gas inlet assembly 7, a secondary gas inlet assembly 8, and a tertiary gas inlet assembly 11, gases generated at different temperatures in the synthesis tank 4 are discharged separately. In conjunction with the condenser assembly 9, condensation is carried out at different temperatures at the inlet and outlet ends, and then discharged separately through the drain pipe 10. This allows materials with different vaporization temperatures to be liquefied at different condensation temperatures, thereby achieving raw material separation during the condensation process and facilitating subsequent use.
[0041] The above description is merely an embodiment of the present invention and does not limit the patent scope of the present invention. Any equivalent structural or procedural transformations made based on the content of the present invention's specification and drawings, or direct or indirect applications in other related technical fields, are similarly included within the patent protection scope of the present invention.
Claims
1. The application of rosin ester compounds in the synthesis of copper phthalocyanine, characterized in that, Includes the following steps: S1: Material preparation: In a 3000 ml three-necked synthesis tank equipped with a stirrer, thermometer, and condenser, add 100% rosin ester compound, 310 g of 100% phthalic anhydride, 231 g of urea, and 1500 ml of solvent alkylbenzene to complete the initial material feeding. S2: Initial heating and heat preservation, while maintaining stirring, to uniformly heat the system to 170℃ over 4 hours, and then maintain the temperature for 2 hours after reaching the temperature. S3: Add urea for a second heating and heat preservation. Add 231 grams of urea to the system, then heat the system evenly to 190°C, and keep it at a constant temperature for 2 hours after reaching the temperature. S4: Add catalyst material and heat up and hold for three times. Add 61 g of 100% cuprous chloride and 4 g of 100% ammonium molybdate to the system and keep stirring. Heat the system to 210°C uniformly over 5 hours. After reaching the temperature, keep the system at the temperature and stir for 6 hours. S5: Cool the system and add alkali. Cool the reacted system to 100°C and add 50g of 30% sodium hydroxide solution to complete the initial post-treatment preparation. S6: Steam distillation to recover the solvent. Steam is passed into the system to distill and recover the solvent alkylbenzene. Distillation is continued for about 5 hours until no more solvent is distilled off, at which point the distillation operation is ended. S7: The product is post-processed to obtain the final product. The distilled system is then filtered, washed with water, and dried in sequence to finally obtain the copper phthalocyanine product.
2. The application of the rosin ester compounds according to claim 1 in the synthesis process of copper phthalocyanine, wherein the synthesis vessel required in steps S1-S7 is characterized in that, Including the installation base frame; A synthesis tank is mounted on top of a mounting base via a bracket. A condensation assembly is mounted on the top of the synthesis tank and the top of the mounting base. The condensation assembly has three inlets, each equipped with a primary gas inlet assembly, a secondary gas inlet assembly, and a tertiary gas inlet assembly. Multiple drain pipes are mounted on the front of the condensation assembly.
3. The application of the rosin ester compounds according to claim 2 in the synthesis of copper phthalocyanine, characterized in that, The top of the synthesis tank is equipped with a drive structure, and the output end of the drive structure is equipped with a stirring assembly.
4. The application of the rosin ester compounds according to claim 3 in the synthesis of copper phthalocyanine, characterized in that, The stirring assembly includes a rotating shaft, multiple stirring racks, and multiple fixing racks, with the multiple fixing racks used to mount the multiple stirring racks on the outer surface of the rotating shaft.
5. The application of the rosin ester compounds according to claim 2 in the synthesis of copper phthalocyanine, characterized in that, The top of the synthesis tank is equipped with a feed pipe, and the bottom of the synthesis tank is equipped with a discharge assembly. The discharge assembly includes a valve and a discharge pipe, and the valve is used to install the discharge pipe at the bottom of the synthesis tank.
6. The application of the rosin ester compounds according to claim 2 in the synthesis of copper phthalocyanine, characterized in that, The mounting base includes a base plate, a mounting structure, and an adjustment structure. The mounting structure is used to mount the adjustment structure on the bottom of the base plate.
7. The application of the rosin ester compounds according to claim 2 in the synthesis of copper phthalocyanine, characterized in that, A control box with a door is mounted on the top of the mounting base, and an operation panel is mounted on one side of the control box.
8. The application of the rosin ester compounds according to claim 2 in the synthesis of copper phthalocyanine, characterized in that, The synthesis tank includes a primary synthesis tank, a secondary synthesis tank, and a tertiary synthesis tank, and the connecting ring is used to install the primary synthesis tank, the connecting ring, the secondary synthesis tank, and the tertiary synthesis tank together.
9. The application of the rosin ester compounds according to claim 2 in the synthesis of copper phthalocyanine, characterized in that, The condensation assembly includes a condenser, a liquid inlet pipe, and a liquid outlet pipe, which are installed at the inlet and outlet of the condenser.
10. The application of the rosin ester compounds according to claim 2 in the synthesis of copper phthalocyanine, characterized in that, The primary gas inlet assembly includes an inlet pipe, a valve, and a connecting pipe. The connecting pipe is installed at the gas inlet of the condensation assembly, and the valve is used to connect the inlet pipe to the other end of the connecting pipe.