A copper phthalocyanine solid-phase synthesis system and method

Abstract

The application belongs to the technical field of organic pigments, and particularly relates to a copper phthalocyanine solid-phase synthesis system and method. The system comprises a raw material mixer, a horizontal reactor for stirring and heating raw materials, a sedimentation collecting device and a tail gas absorption device connected in sequence. The sedimentation collecting device comprises a sedimentation chamber and a bag-type dust collector connected in sequence. The sedimentation chamber and the bag-type dust collector are connected with a solid collector. The solid collector is connected with the raw material mixer. The customized horizontal reactor is used to replace the vertical reactor, so that the efficiency problem of 'three transmission and one reaction' in the reaction process is effectively solved, the conversion rate of raw materials and the product yield are improved, and the production cost is reduced.

Description

Technical Field

[0001] The invention belongs to the technical field of organic pigments, and in particular relates to a copper phthalocyanine solid phase synthesis system and method. Background Art

[0002] Copper phthalocyanine is currently produced both at home and abroad, and its production methods include solid phase method and solvent method. The raw materials used in the solid phase method for producing copper phthalocyanine are phthalic anhydride, urea, cuprous chloride, and ammonium molybdate. The advantages of the solid phase method for producing copper phthalocyanine over the solvent method are that it reduces the solvent recovery process, reduces the three wastes, does not contain polychlorinated biphenyls (PCBs), does not involve solvents in the production process, and its inherent safety is greatly improved. The current common solid phase method is specifically 0.5-1.0m 3 The reaction is carried out in a vertical reactor. Before the reaction, the base material is added to increase the temperature, and then the mixed raw materials are added to react. The addition speed is controlled by the reaction temperature and stirring current. The oil valve needs to be gradually closed during the reaction. After the addition is completed, the heat preservation and stirring are continued for 1-2 hours before discharging the material. The subsequent batches are repeated in this way.

[0003] However, this approach has the following problems:

[0004] 1. Since the reaction device is a vertical structure, all materials in the production process act on the vertical structure stirring paddle. In the middle and late stages of feeding, as the amount of materials increases and the viscosity of the system increases, the torque of the stirring paddle of the reactor increases, and the current increases, making the feeding process unstable and the temperature difficult to control, affecting the reaction efficiency, and easily causing damage to the equipment and increased energy consumption;

[0005] 2. Due to the vertical structure and large stirring load, the rated volume of the reactor cannot be increased and is basically maintained at 1m 3 The level of production leads to low production capacity of a single device. A certain production capacity can only be achieved by increasing the number of devices, which leads to an increase in fixed asset investment, a low input-output ratio, and a lack of economic efficiency.

[0006] 3. Due to the particularity of the solid-phase reaction process and the structural characteristics of the vertical reactor used, the failure rate of the reaction device is high, the system stability is poor, it is difficult to achieve automation and digitalization of the production process, and a large amount of manpower is consumed;

[0007] 4. Due to the stirring efficiency issues of the vertical reactor structure and the supporting stirring paddle, coupled with the difference in specific gravity between the masterbatch and fresh raw materials, the contact area between the masterbatch and the mixed materials is small during the reaction, affecting the mass transfer and heat transfer efficiency, ultimately leading to low raw material conversion rate and product yield (the ratio of actual output to theoretical output), high production costs, and lack of market competitiveness of the products;

[0008] 5. Due to the defects of the vertical reaction system, the system cannot be sealed, and the supporting exhaust gas absorption system cannot achieve efficient absorption, resulting in a poor on-site environment and failure to meet occupational health requirements. Summary of the Invention

[0009] To overcome the above-mentioned shortcomings of the prior art, the present invention provides a system and method for the solid-phase synthesis of copper phthalocyanine. The present invention utilizes a horizontal reactor instead of a vertical reactor, effectively resolving the efficiency issues of the "three-pass, one-reverse" reaction process, thereby improving the conversion rate of raw materials and product yield, and reducing production costs.

[0010] To achieve one of the above purposes, the present invention adopts the following technical solutions:

[0011] A copper phthalocyanine solid-phase synthesis system comprises a raw material mixer, a horizontal reactor for stirring and heating the raw materials, a sedimentation and collection device, and a tail gas absorption device, which are connected in sequence. The sedimentation and collection device comprises a sedimentation chamber and a bag dust collector, which are connected in sequence. The sedimentation chamber and the bag dust collector are both connected to a solid collector, and the solid collector is connected to the raw material mixer.

[0012] Preferably, the volume of the horizontal reactor is 3-10m 3 .

[0013] Preferably, the tail gas absorption device includes a primary water absorption tower, a secondary water absorption tower and a tertiary water absorption tower connected in sequence, the liquid outlet of the primary water absorption tower is connected to the liquid inlet of the primary absorption liquid collecting tank; the liquid outlet of the secondary water absorption tower is connected to the liquid inlet of the secondary absorption liquid collecting tank; the liquid outlet of the tertiary water absorption tower is connected to the liquid inlet of the tertiary absorption liquid collecting tank; the liquid outlet of the tertiary absorption liquid collecting tank is connected to the secondary water absorption tower, the liquid outlet of the secondary absorption liquid collecting tank is connected to the primary water absorption tower, the liquid outlet of the primary absorption liquid collecting tank is connected to the ammonia recovery system; the liquid inlet of the tertiary absorption liquid collecting tank is connected to the fresh absorption liquid tank.

[0014] Preferably, the inlet of the settling chamber is connected to the outlet of the horizontal reactor, and the bag dust collector is connected to the tail gas absorption device through a fan.

[0015] Preferably, a plurality of metal balls are arranged in the horizontal reactor.

[0016] Preferably, a quantitative feeding device is provided in the horizontal reactor to ensure that the added materials can react in time within a prescribed time after a single addition through quantitative feeding.

[0017] To achieve the second of the above objectives, the present invention provides a solid-phase synthesis method for copper phthalocyanine, comprising the following steps:

[0018] S1, the raw materials are mixed in a raw material mixer, then are put into a horizontal reactor for stirring and heating for 1h, and then are discharged;

[0019] S2, the tail gas and by-products generated in the horizontal reactor enter a settling chamber, the solid by-products are collected, the remaining part enters a bag filter for collection, and the tail gas enters a first water absorption tower, a second water absorption tower and a third water absorption tower for absorption;

[0020] S3, fresh absorption liquid enters the third water absorption tower for spray absorption to obtain third absorption liquid, the third absorption liquid is pumped into the second water absorption tower for secondary spray absorption to obtain second absorption liquid, the second absorption liquid is pumped into the first water absorption tower for primary absorption to obtain first absorption liquid, and the first absorption liquid is directly transported to an ammonia recovery system for ammonia water recovery.

[0021] Preferably, before the raw materials are put into the horizontal reactor, the stirring function of the horizontal reactor is started, and the horizontal reactor is heated to 180-240 DEG C.

[0022] Preferably, in step S1, the mixed materials are added through a feeding device, and the feeding temperature is controlled at 180-240 DEG C.

[0023] Preferably, in step S1, the total feeding time is controlled at 6-10h, and after the feeding is completed, the materials are stirred for 1h for heating, and then are discharged.

[0024] The present application has the following advantages:

[0025] (1) The present application uses a customized horizontal reactor to replace a vertical reactor, effectively solves the efficiency problem of "three transmission and one reaction" in the reaction process, thereby improving the conversion rate of raw materials and the product yield, reducing the production cost, and ultimately improving the market competitiveness of the product.

[0026] (2) The material in the horizontal reactor acts on the horizontal shaft of the horizontal reactor, and the stirring shaft and stirring paddle are uniformly stressed, so that the current is stable during the whole production process, the reaction temperature can be controlled stably, and the reaction process is stable.

[0027] (3) Since the system reaction process of the present application runs stably, the failure rate of the reaction device is low, the system stability is high, automation and digitization can be realized, and the labor consumption is low.

[0028] (4) The horizontal reactor is heated by passing heat-conducting oil into the jacket and hollow stirring paddle, the heating area in the horizontal reactor is large, the heating efficiency and stirring efficiency are high, and the reaction efficiency of the raw materials is effectively improved; due to the structural characteristics of the horizontal reactor, the stirring system is uniformly stressed and the torque is small during the reaction process, so the size of the reactor is less restricted by the stirring system, and therefore the volume of the horizontal reactor is 3-10m 3The horizontal reactor can reach 3-20 times of the vertical reactor, greatly increasing the production capacity of a single device, and under the condition of realizing the same production capacity, the horizontal reactor needs less fixed asset investment, has higher input-output ratio and better economy.

[0029] (5) In the process of producing phthalocyanine copper by the solid phase method, the materials are easy to be caked and stick to the wall, in order to further improve the reaction effect, corresponding metal balls are added in the kettle, which can not only ensure that the balls do not participate in the reaction, but also increase the crushing effect, so that the reaction is more sufficient.

[0030] (6) The horizontal reactor can effectively solve the problem of system sealing. The horizontal reactor has the characteristics of high-efficiency "three transmissions and one reaction" (momentum transmission, heat transmission, mass transmission and chemical reaction process), complete reaction and improved reaction efficiency; in the production process, master batch is not needed, one-time feeding, gradual heating and finally holding reaction until the reaction is completed can be used to organize production, which can effectively improve the batch yield. At the same time, the system can be sealed, that is, the feeding port is sealed after feeding is completed, so that the reaction process can be carried out in a relatively sealed system, the on-site environment can be effectively controlled, and the occupational health requirements are met.

[0031] (7) The tail gas of the solid phase method for synthesizing copper phthalocyanine mainly contains ammonia, carbon dioxide and organic sublimates. Since the horizontal reaction system can achieve good sealing, the organic sublimates in the reaction tail gas can be fully collected to achieve the purpose of purifying the tail gas, so that the tail gas is mainly ammonia and carbon dioxide, and the ammonia resource can be effectively recovered through multi-stage acid absorption and water absorption. In addition, the organic sublimates collected by the sedimentation collection device are returned to the reaction system to participate in the reaction, realizing the full utilization of resources and effectively reducing the raw material consumption and production cost.

[0032] (8) The volume of a single horizontal reactor is 3-20 times of that of a vertical reactor, the single-kettle yield can reach 3-20 times, the batch yield is high, the production efficiency is multiplied, the energy consumption is reduced, the automation is improved, the labor intensity is greatly reduced, and the labor personnel are reduced.

[0033] (9) The present application uses the sedimentation chamber and the bag dust collector to collect the organic matter in the reaction waste gas, and recycles the recovered organic matter, effectively reduces the difficulty of wastewater treatment and avoids resource waste, and meets the requirements of green manufacturing. BRIEF DESCRIPTION OF DRAWINGS

[0034] Figure 1 The process flowchart of the present application. DETAILED DESCRIPTION

[0035] In order to make the purpose, technical scheme and advantages of the present application more clear, the present application is further described in detail below in combination with the drawings and examples. All other examples obtained by those skilled in the art without creative labor based on the examples in the present application belong to the protection scope of the present application.

[0036] As shown in Figure 1 A copper phthalocyanine solid-phase synthesis system, which comprises a reactor for stirring and heating raw materials, and the reactor is a special copper phthalocyanine horizontal reactor with a volume of 3-10 m 3 The remaining space of the reactor is increased relative to the existing vertical reactor, and the contact time of the materials is increased. The inlet of the horizontal reactor is connected with a raw material mixer for preliminary mixing of the raw materials before feeding. After the raw materials are heated in the horizontal reactor, part of the raw materials will melt, and then a state of coexistence of solid and liquid will appear. Therefore, the horizontal reactor not only has the function of heating reaction, but also has the function of continuing to mix the raw materials, which ensures that the raw materials continue to be fully mixed, realizes good mass and heat transfer effect, and ensures the effect of the synthesis reaction.

[0037] Specifically, the system further comprises a sedimentation and collection device, which is composed of a connected sedimentation chamber and a bag dust collector. The inlet of the sedimentation chamber is connected with the outlet of the horizontal reactor. The sedimentation chamber can collect solid by-products, and the remaining part enters the bag dust collector. The sedimentation chamber and the bag dust collector are both connected with a solid collector, and the solid collector is connected with the raw material mixer. The reaction tail gas of the horizontal reactor contains unreacted raw material sublimates. When passing through the sedimentation chamber, the larger solid in the waste gas is first settled in the sedimentation chamber and separated from the waste gas. The fine particulate solid in the waste gas enters the bag dust collector together with the waste gas and is separated from the waste gas after being intercepted by the bag. Then the solid collected in the sedimentation chamber and the solid captured by the bag are concentrated in the solid collector. The function of the solid collector is to collect the solid in the sedimentation chamber and the bag dust collector for reuse.

[0038] Further, the system further comprises a tail gas absorption device, which comprises a first-stage water absorption tower, a second-stage water absorption tower and a third-stage water absorption tower connected in sequence. The liquid outlet of the first-stage water absorption tower is connected with the liquid inlet of a first-stage absorption liquid collection tank. The liquid outlet of the second-stage water absorption tower is connected with the liquid inlet of a second-stage absorption liquid collection tank. The liquid outlet of the third-stage water absorption tower is connected with the liquid inlet of a third-stage absorption liquid collection tank. The liquid outlet of the third-stage absorption liquid collection tank is connected with the second-stage water absorption tower. The liquid outlet of the second-stage absorption liquid collection tank is connected with the first-stage water absorption tower. The liquid outlet of the first-stage absorption liquid collection tank is connected with an ammonia recovery system.

[0039] The feeding process is optimized. In order to increase the stirring effect during the feeding process, corresponding metal balls are added to strengthen the stirring effect.

[0040] A copper phthalocyanine solid phase synthesis method, comprising the following steps:

[0041] S1, the raw materials are put into the raw material mixer for preliminary mixing;

[0042] S2, open the horizontal reactor heat transfer oil inlet and outlet valve, then open the horizontal reactor stirring function, ensure that the material enters the horizontal reactor immediately stirring mixed, the horizontal reactor is heated to 180-240℃, then the mixed material in the raw material mixer is added through the quantitative feeding device, the feeding temperature is controlled at 180-240℃, the total feeding time is controlled at 6-10h, after feeding, the temperature is kept for 1h, then the material is unloaded;

[0043] S3, the tail gas and by-products (including carbon dioxide, ammonia, phthalimide and phthalic anhydride) generated in the horizontal reactor enter the settling chamber, the solid by-products are collected, the remaining part enters the bag filter to collect, the tail gas enters the first water absorption tower T0301, the second water absorption tower T0302 and the third water absorption tower T0303 to absorb the tail gas;

[0044] S4, the fresh absorption liquid enters the third water absorption tower for spray absorption to obtain the third absorption liquid, the third absorption liquid is pumped into the second water absorption tower for secondary spray absorption to obtain the second absorption liquid, the second absorption liquid is pumped into the first water absorption tower for primary absorption to obtain the first absorption liquid, and the first absorption liquid is directly transported to the ammonia recovery system for recovery.

[0045] The above is only a preferred embodiment of the present application, and is not used to limit the present application, any modification, equivalent replacement and improvement within the spirit and principle of the present application should be included in the protection scope of the present application.

Claims

1. A copper phthalocyanine solid phase synthesis system, characterized in that: The system includes a raw material mixer, a horizontal reactor for stirring and heating raw materials, a sedimentation and collection device, and a tail gas absorption device connected in sequence. The sedimentation and collection device includes a sedimentation chamber and a bag dust collector connected in sequence. The sedimentation chamber and the bag dust collector are both connected to a solid collector, and the solid collector is connected to the raw material mixer; The tail gas absorption device includes a primary water absorption tower, a secondary water absorption tower and a tertiary water absorption tower which are connected in sequence. The liquid outlet of the primary water absorption tower is connected to the liquid inlet of the primary absorption liquid collecting tank; the liquid outlet of the secondary water absorption tower is connected to the liquid inlet of the secondary absorption liquid collecting tank; the liquid outlet of the tertiary water absorption tower is connected to the liquid inlet of the tertiary absorption liquid collecting tank; the liquid outlet of the tertiary absorption liquid collecting tank is connected to the secondary water absorption tower, the liquid outlet of the secondary absorption liquid collecting tank is connected to the primary water absorption tower, and the liquid outlet of the primary absorption liquid collecting tank is connected to the ammonia recovery system; the liquid inlet of the tertiary absorption liquid collecting tank is connected to the fresh absorption liquid tank; the inlet of the sedimentation chamber is connected to the outlet of the horizontal reactor, and the bag dust collector is connected to the tail gas absorption device through a fan.

2. A copper phthalocyanine solid phase synthesis system according to claim 1, characterized in that: The volume of the horizontal reactor is 3-10m³.

3. A copper phthalocyanine solid phase synthesis system according to claim 1, characterized in that: Metal balls are arranged in the horizontal reactor.

4. A copper phthalocyanine solid phase synthesis system according to claim 1, characterized in that: A quantitative feeding device is arranged in the horizontal reactor.

5. A method for solid-phase synthesis of copper phthalocyanine using the copper phthalocyanine solid-phase synthesis system according to any one of claims 1 to 4, characterized in that: The steps include: S1, put the raw materials into the raw material mixer and mix them, then put them into the horizontal reactor and stir and heat and keep stirring for 1 hour to unload; S2, the tail gas and by-products generated in the horizontal reactor enter the settling chamber, the solid by-products are settled and collected, and the remaining part enters the bag dust collector for collection, and the tail gas then enters the primary water absorption tower, the secondary water absorption tower, and the tertiary water absorption tower to absorb the tail gas; S3. Fresh absorption liquid enters the tertiary water absorption tower for spray absorption to obtain tertiary absorption liquid. The tertiary absorption liquid is pumped into the secondary water absorption tower for secondary spray absorption to obtain secondary absorption liquid. The secondary absorption liquid is pumped into the primary water absorption tower for primary absorption to obtain primary absorption liquid. The primary absorption liquid is directly transported to the ammonia recovery system.

6. The method for solid-phase synthesis of copper phthalocyanine using the copper phthalocyanine solid-phase synthesis system according to claim 5, characterized in that: Before the raw materials are put into the horizontal reactor, the stirring function of the horizontal reactor is turned on and the temperature of the horizontal reactor is raised to 180-240°C.

7. The method for solid-phase synthesis of copper phthalocyanine using the copper phthalocyanine solid-phase synthesis system according to claim 5, characterized in that: In step S1, the mixed materials are added through a feeding device, and the feeding temperature is controlled at 180°C-240°C.

8. The method for solid-phase synthesis of copper phthalocyanine using the copper phthalocyanine solid-phase synthesis system according to claim 5, characterized in that: In step S1, the total feeding time is controlled within 6-10 hours, and after the feeding is completed, the mixture is kept warm and stirred for 1 hour before being unloaded.

Images