Solid-phase synthesis system and method for copper phthalocyanine

Abstract

The invention belongs to the technical field of organic pigments, and particularly relates to a system and a method for synthesizing copper phthalocyanine by a solid-phase method. The system comprises a raw material mixer, a horizontal reactor used for stirring and heating raw materials, a sedimentation collection device and a tail gas absorption device which are connected in sequence, the sedimentation collection device comprises a sedimentation chamber and a cloth bag dust removal collector which are connected in sequence, and the sedimentation chamber and the cloth bag dust removal collector are both connected with a solid collector; the solid collector is connected with the raw material mixer. The customized horizontal reactor is used for replacing a vertical reactor, and the efficiency problem of three-transmission and one-reaction in the reaction process is effectively solved, so that 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 to produce 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 in the product, does not involve solvents in the production process, and greatly improves the inherent safety. 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 for reaction. The adding speed is controlled by the reaction temperature and the 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, and the subsequent batches are repeated in the same way.

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

[0004] 1. Since the reaction device is a vertical structure, all materials in the production process act on the longitudinal 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 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, low input-output ratio and lack of economy.

[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 realize the automation and digitalization of the production process, and a large amount of manpower is consumed;

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

[0008] 5. Due to the defects of the vertical reaction system, the system cannot be closed, 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] In order to overcome the defects in the above-mentioned prior art, the present invention provides a copper phthalocyanine solid phase synthesis system and method. The present invention adopts a horizontal reactor to replace the vertical reactor, effectively solving the efficiency problem of the "three-pass and 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 solution:

[0011] A copper phthalocyanine solid phase synthesis system comprises a raw material mixer, a horizontal reactor for stirring and heating the raw material, a sedimentation collection device and a tail gas absorption device which are connected in sequence. The sedimentation 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 comprises 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, 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, and through the quantitative feeding method, it is ensured that after a single feeding, the added materials can react in time within a specified time.

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

[0018] S1, put the raw materials into the raw material mixer and mix them, then put them into the horizontal reactor, stir and heat and keep them warm for 1 hour before unloading;

[0019] S2, the tail gas and by-products generated in the horizontal reactor enter the settling chamber, the solid by-products are precipitated and collected, and the remaining part enters the bag filter for collection, and the tail gas enters the primary water absorption tower, the secondary water absorption tower, and the tertiary water absorption tower to absorb the tail gas;

[0020] 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 to recover ammonia water.

[0021] Preferably, 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.

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

[0023] Preferably, in step S1, the total feeding time is controlled within 6-10 hours, and after the feeding is completed, the material is kept warm and stirred for 1 hour before unloading.

[0024] The advantages of the present invention are:

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

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

[0027] (3) Since the reaction process of the system of the present invention runs smoothly, the failure rate of the reaction device is low, the system stability is high, automation and digitization can be achieved, and the manpower consumption is low.

[0028] (4) The horizontal reactor is heated by passing heat transfer 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 evenly stressed during the reaction process and the torque is small. Therefore, the size of the reactor is less restricted by the stirring system. Therefore, the volume of the horizontal reactor is 3-10m 3, which can reach 3-20 times that of the vertical reactor, greatly increasing the production capacity of a single device. Under the condition of achieving the same production capacity, the use of horizontal reactors requires less fixed asset investment, has a higher input-output ratio and better economy.

[0029] (5) In the process of producing copper phthalocyanine by the solid phase method of the present invention, the material is easy to agglomerate and stick to the wall. In order to further improve the effect of the reaction, corresponding metal balls are added to the kettle, which not only ensures that the balls do not participate in the reaction, but also increases the crushing effect, making the reaction more sufficient.

[0030] (6) The horizontal reactor of the present invention can effectively solve the problem of system airtightness. The horizontal reactor has the characteristics of efficient "three transfers and one reaction" (momentum transfer, heat transfer, mass transfer, and chemical reaction process), complete reaction, and improved reaction efficiency; no masterbatch is required in the production process, and the production can be organized by a process of one-time feeding, gradual temperature increase, and final insulation reaction until the reaction is completed. This process can effectively increase the batch output. At the same time, the airtightness of the system can be achieved, that is, the feeding port is closed after the feeding is completed, so that the reaction process can be carried out in a relatively closed system, and the on-site environment can be effectively controlled, meeting the occupational health requirements.

[0031] (7) The tail gas of copper phthalocyanine synthesized by the solid phase method mainly contains ammonia, carbon dioxide and organic sublimates. Since the horizontal reaction system can achieve good airtightness, 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. After multi-stage acid absorption and water absorption, the ammonia resource can be effectively recovered. In addition, the organic sublimates collected by the sedimentation collection device are returned to the reaction system to participate in the reaction, so as to achieve full utilization of resources and effectively reduce raw material consumption and production costs.

[0032] (8) The volume of a single horizontal reactor is 3-20 times that of a vertical reactor, and the output of a single reactor can reach 3-20 times, with high batch output and exponentially increased production efficiency; energy consumption is reduced, automation is improved, labor intensity is greatly reduced, and the number of workers is reduced.

[0033] (9) The present invention utilizes a settling chamber and a bag filter to collect organic matter in the reaction exhaust gas, and recycles the recovered organic matter, thereby effectively reducing the difficulty of wastewater treatment and avoiding waste of resources, and meeting the requirements of green manufacturing. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] Figure 1 It is a process flow chart of the present invention. DETAILED DESCRIPTION

[0035] In order to make the purpose, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with the accompanying drawings and embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in the field without making creative work are within the scope of protection of the present invention.

[0036] like Figure 1 As shown, a copper phthalocyanine solid phase synthesis system includes a reactor for stirring and heating the raw materials. The reactor is a horizontal reactor specially made for copper phthalocyanine, and its volume is 3-10m 3 , so that the remaining space of the reactor is increased compared with the existing vertical reactor, and the contact time of the materials is increased. The inlet of the horizontal reactor is connected to a raw material mixer, which is used to preliminarily mix the raw materials for feeding. The raw materials will partially melt after being heated in the horizontal reactor, and then a state of solid and liquid coexisting will appear. Therefore, the horizontal reactor not only has the function of heating the reaction, but also has the function of continuing to mix the raw materials, ensuring that the raw materials continue to be fully mixed, achieving better mass transfer and heat transfer effects, and ensuring the effect of the synthesis reaction.

[0037] Specifically, the system also includes a sedimentation collection device, which is composed of a connected sedimentation chamber and a bag dust collector. The inlet of the sedimentation chamber is connected to the outlet of the horizontal reactor. The sedimentation chamber can collect solid by-products by sedimentation, and the remaining part enters the bag dust collector collector. The sedimentation chamber and the bag dust collector are also connected to the solid collector, and the solid collector is connected to 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 solids in the waste gas are first separated from the waste gas after sedimentation in the sedimentation chamber. The fine particulate solids in the waste gas enter the bag dust collector together with the waste gas and are separated from the waste gas after being intercepted by the bag. Then the solids in the sedimentation chamber and the solids captured by the bag are concentrated in the solid collector. The function of the solid collector is to collect the solids in the sedimentation chamber and the bag dust collector for reuse.

[0038] Furthermore, the system also includes a tail gas absorption device, which 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, and the liquid outlet of the primary absorption liquid collecting tank is connected to the 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 enhance the stirring effect.

[0040] A solid phase synthesis method for copper phthalocyanine comprises the following steps:

[0041] S1, putting the raw materials into a raw material mixer for preliminary mixing;

[0042] S2, open the heat transfer oil inlet and outlet valves of the horizontal reactor, and then turn on the stirring function of the horizontal reactor to ensure that the materials are stirred and mixed immediately when entering the horizontal reactor. After the horizontal reactor is heated to 180-240°C, the mixed materials in the raw material mixer are added through the quantitative feeding device. The feeding temperature is controlled at 180-240°C, and the total feeding time is controlled at 6-10h. After the addition is completed, keep warm and stir for 1h before unloading;

[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 precipitated and collected, and the remaining part enters the bag filter for collection, and the tail gas enters the primary water absorption tower T0301, the secondary water absorption tower T0302, and the tertiary water absorption tower T0303 to absorb the tail gas;

[0044] S4. 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 for recovery.

[0045] The above are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A copper phthalocyanine solid phase synthesis system, characterized in that: The system comprises a raw material mixer, a horizontal reactor for stirring and heating raw materials, a sedimentation collection device and a tail gas absorption device which are connected in sequence. The sedimentation 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.

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

3. A copper phthalocyanine solid phase synthesis system according to claim 1, characterized in that: The tail gas absorption device comprises a primary water absorption tower, a secondary water absorption tower and a tertiary water absorption tower which are connected in sequence, wherein 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.

4. A copper phthalocyanine solid phase synthesis system according to claim 1, characterized in that: 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.

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

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

7. A solid phase synthesis method for copper phthalocyanine according to any one of claims 1 to 6, 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, stir and heat and keep them warm for 1 hour before unloading; S2, the tail gas and by-products generated in the horizontal reactor enter the settling chamber, the solid by-products are precipitated and collected, and the remaining part enters the bag filter for collection, and the tail gas 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.

8. The solid phase synthesis method of copper phthalocyanine according to claim 7, 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.

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

10. The solid phase synthesis method of copper phthalocyanine according to claim 7, characterized in that: In step S1, the total feeding time is controlled within 6-10 hours, and after the feeding is completed, the material is kept warm and stirred for 1 hour before unloading.

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