Synthesizer for preparing pigment red 254 by using liquid potassium tert-amyl alcohol as raw material

Abstract

The utility model discloses a synthesizer for preparing pigment red 254 by using liquid potassium tert-amyl alcohol as a raw material, which comprises a reaction kettle, a bottom discharge port of the reaction kettle is connected with a shell pass feed port of a film evaporator through a first transfer pump, and a shell pass bottom discharge port of the film evaporator is connected with a feed port of a washing kettle; a discharging hole in the bottom of the washing kettle is connected with a feeding hole of the plate-and-frame filter press through a fourth transfer pump; and a discharge port of the plate-and-frame filter press is connected with a feed port of the spray dryer. In the synthesis device disclosed by the utility model, the liquid potassium tert-amyl alcoholate is used as both a solvent and a catalyst for condensation reaction, and the quality of the liquid potassium tert-amyl alcoholate determines the yield of the condensation reaction and the quality of a product and is a premise and guarantee of high-quality pigment. According to the synthesis device disclosed by the utility model, liquid potassium tert-amyl alcohol is rapidly synthesized by adding high-quality liquid potassium, so that not only is the reaction rate greatly improved, but also the product quality is controlled from the source, the granularity of the product is more uniform, and the stability of the product is obviously improved.

Description

Technical Field

[0001] The utility model belongs to the technical field of pigments, relates to Pigment Red 254, and particularly relates to a synthesis device for preparing Pigment Red 254 by using liquid potassium tert-amylate as a raw material. Background Art

[0002] Pigment Red 254, also known as bis(4-chlorophenyl)-1,4-diketopyrrolo[3,4-c]pyrrole, is a high-performance organic pigment with strong covering power, good dispersibility, bright color, stable temperature and weather resistance, stable chemical structure, not easily decomposed, strong coloring power, and can maintain bright red for a long time. Pigment Red 254 is mainly used for automotive primer, and is also widely used in powder coatings, paints, inks, plastic (PVC, PS, polyolefins, etc.) coloring, etc. With the rapid development of the downstream industries, especially the continuous growth of industries such as packaging, construction, and automotive, the market demand for Pigment Red 254 shows a steady upward trend. This growth trend indicates that the future market capacity of the Pigment Red 254 industry will continue to expand.

[0003] The production process of Pigment Red 254 mainly uses p-chlorobenzonitrile and diisopropyl succinate as raw materials, tert-amyl alcohol as a solvent, through redox reaction, condensation reaction and hydrolysis reaction, and then filtration and rinsing to obtain high-covering power Pigment Red 254. The Pigment Red 254 produced by this process has the characteristics of high yield, good quality, bright color, high coloring power, etc., as mentioned in US Patent US4579949. However, the current process is not perfect, with slow reaction speed, low yield, uneven product particle size and poor stability. Summary of the Invention

[0004] Aiming at the deficiencies of the existing technology, the purpose of the utility model is to provide a synthesis device for preparing Pigment Red 254 by using liquid potassium tert-amylate as a raw material, so as to solve the technical problem that the quality of the products prepared by the existing synthesis device needs to be further improved.

[0005] In order to solve the above technical problems, the utility model is realized by adopting the following technical solutions:

[0006] A synthesis device for preparing Pigment Red 254 by using liquid potassium tert-amylate as a raw material, including a reaction kettle, the bottom discharge port of the reaction kettle is connected to the shell-side feed port of a thin-film evaporator through a first transfer pump, and the bottom discharge port of the shell side of the thin-film evaporator is connected to the feed port of a water-washing kettle.

[0007] The feed port of the reaction kettle is connected to a first storage tank through a second transfer pump, and the feed port of the reaction kettle is also connected to a second storage tank through the second transfer pump.

[0008] The feed inlet of the reactor is also connected to a constant pressure dropping funnel, and the constant pressure dropping funnel is connected to a third storage tank through a third transfer pump; the feed inlet of the reactor is also connected to a solid feeder.

[0009] The utility model also has the following technical features:

[0010] The bottom discharge port of the water washing kettle is connected to the feed inlet of the plate and frame filter press through a fourth transfer pump; the discharge port of the plate and frame filter press is connected to the feed inlet of the spray dryer, and the discharge port of the spray dryer is used to discharge the product pigment red 254.

[0011] The gas inlet of the reactor is connected to a nitrogen cylinder.

[0012] The gas outlet of the reactor is connected to the shell side input end of the first condenser, and the shell side output end of the first condenser is connected to the water washing type tail gas treatment device.

[0013] The gas outlet at the top of the shell side of the thin film evaporator is directly connected to the shell side input end of the second condenser, and the shell side output end of the second condenser is connected to the recovered alcohol storage tank.

[0014] The top feed inlet of the water washing kettle is connected to the distilled water storage tank through a fifth transfer pump.

[0015] The first storage tank is a tert-amyl alcohol storage tank; the second storage tank is a liquid potassium storage tank; the third storage tank is a diisopropyl succinate storage tank; the solid feeder is a p-chlorobenzonitrile solid feeder.

[0016] Compared with the prior art, the utility model has the following beneficial technical effects:

[0017] (Ⅰ) In the synthesis device of the utility model, liquid potassium tert-amylate serves both as a solvent and as a catalyst for the condensation reaction, and its quality determines the yield of the condensation reaction and the quality of the product, which is a prerequisite guarantee for high-quality pigments. The synthesis device of the utility model quickly synthesizes liquid potassium tert-amylate by adding high-quality liquid potassium, which not only greatly improves the reaction rate but also controls the product quality from the source, making the product particle size more uniform and significantly improving the product stability.

[0018] (Ⅱ) The synthesis device of the utility model uses a thin film evaporator for distillation pretreatment, which has high heat transfer efficiency, fast evaporation speed. The use of a scraping film device reduces the thickness of the liquid film in the turbulent state, reduces the thermal resistance, and inhibits the wall and scale formation of the material on the heating surface.

[0019] (Ⅲ) The synthesis device of the present utility model adopts a plate and frame filter press for low-pressure filtration and high-pressure pressing, which can greatly shorten the entire filtration cycle. The maximum filtration pressure can reach 25 MPA, thereby greatly reducing the moisture content, saving drying costs, and increasing the yield. The plate and frame filter press saves the consumption of operating power. In the later stage of filtration, the flow rate is small and the pressure is high. This process is completed in a very short time, saving power consumption. The plate and frame filter press improves the dryness of the mud cake and reduces the moisture content of the mud cake. The diaphragm press performs secondary pressing on the filter cake after static filtration, rearranging the structure of the filter cake and increasing its density, thereby displacing a part of the moisture and increasing the dryness.

[0020] (Ⅳ) The synthesis device of the present utility model adopts a spray dryer for product drying, simplifying the production process and facilitating operation and control. For liquids with a moisture content of less than 60%, they can be dried into powder products in one step. After drying, there is no need for crushing and screening, reducing the production process and improving product purity. For the product particle size, bulk density, and moisture content, they can be adjusted within a certain range by changing the operating conditions, and both control and management are very convenient. Description of the Drawings

[0021] Figure 1 It is a synthesis device for preparing pigment red 254 using liquid potassium tert-amylate as a raw material.

[0022] The meanings of the labels in the figure are as follows: 1 - reaction kettle, 2 - first transfer pump, 3 - thin-film evaporator, 4 - washing kettle, 5 - second transfer pump, 6 - first storage tank, 7 - second storage tank, 8 - constant-pressure drip feeder, 9 - third transfer pump, 10 - third storage tank, 11 - solid feeder, 12 - fourth transfer pump, 13 - plate and frame filter press, 14 - spray dryer, 15 - nitrogen cylinder, 16 - first condenser, 17 - water-washing type tail gas treatment equipment, 18 - second condenser, 19 - recovered alcohol storage tank, 20 - fifth transfer pump, 21 - distilled water storage tank, 22 - pipeline, 23 - valve.

[0023] The following further elaborates on the specific content of the present utility model in combination with embodiments. Specific Embodiments

[0024] It should be noted that all the equipment and raw materials in the present utility model, unless otherwise specified, are all the equipment and raw materials known in the prior art.

[0025] In the present utility model, the main connection between each equipment is through pipeline 22, and valves 23 are provided on each pipeline according to needs and are opened or closed according to process requirements. All the valves 23 in the present utility model are the commonly used valves in the prior art.

[0026] In accordance with the above technical solution, specific embodiments of the present utility model are given below. It should be noted that the present utility model is not limited to the following specific embodiments, and any equivalent transformation based on the technical solution of this application falls within the protection scope of the present utility model.

[0027] Embodiment:

[0028] This embodiment provides a synthesis device for preparing Pigment Red 254 using liquid potassium tert-amylate as a raw material. As Figure 1 shown, it includes a reaction kettle 1. The bottom discharge port of the reaction kettle 1 is connected to the shell-side feed port of a thin-film evaporator 3 through a first transfer pump 2. The bottom discharge port of the shell side of the thin-film evaporator 3 is connected to the feed port of a water-washing kettle 4.

[0029] The feed port of the reaction kettle 1 is connected to a first storage tank 6 through a second transfer pump 5. The feed port of the reaction kettle 1 is also connected to a second storage tank 7 through the second transfer pump 5.

[0030] The feed port of the reaction kettle 1 is also connected to a constant-pressure drip feeder 8. The constant-pressure drip feeder 8 is connected to a third storage tank 10 through a third transfer pump 9. The feed port of the reaction kettle 1 is also connected to a solid feeder 11.

[0031] As a further scheme of this embodiment, as Figure 1 shown, the bottom discharge port of the water-washing kettle 4 is connected to the feed port of a plate-and-frame filter press 13 through a fourth transfer pump 12. The discharge port of the plate-and-frame filter press 13 is connected to the feed port of a spray dryer 14. The discharge port of the spray dryer 14 is used to discharge the product Pigment Red 254. The plate-and-frame filter press 13 uses low-pressure filtration and high-pressure pressing, which can greatly shorten the entire filtration cycle. A spray dryer 14 is used for product drying, simplifying the production process and facilitating operation control.

[0032] In this embodiment, further, the waste liquid discharge port of the plate-and-frame filter press 13 is connected to a subsequent wastewater treatment system. The wastewater treatment system adopts a commonly known wastewater treatment system in the art.

[0033] As a preferred scheme of this embodiment, as Figure 1 shown, the air inlet of the reaction kettle 1 is connected to a nitrogen cylinder 15. It is used to displace the air in the reaction kettle 1 with the inert gas nitrogen.

[0034] As a preferred scheme of this embodiment, as Figure 1 shown, the air outlet of the reaction kettle 1 is connected to the shell-side input end of a first condenser 16. The shell-side output end of the first condenser 16 is connected to a water-washing type tail gas treatment device 17. It is used to treat the tail gas generated during the reaction process to avoid environmental pollution. The water-washing type tail gas treatment device 17 adopts a commonly known water-washing type tail gas treatment device in the art.

[0035] As a preferred scheme of this embodiment, asFigure 1 As shown, the gas outlet at the top of the shell side of the thin-film evaporator 3 is directly connected to the input end of the shell side of the second condenser 18, and the output end of the shell side of the second condenser 18 is connected to the recovered alcohol storage tank 19.

[0036] As a preferred solution of this embodiment, as Figure 1 shown, the top feed port of the water washing kettle 4 is connected to the distilled water storage tank 21 through the fifth transfer pump 20.

[0037] As a preferred solution of this embodiment, as Figure 1 shown, the first storage tank 6 is a tert-amyl alcohol storage tank; the second storage tank 7 is a liquid potassium storage tank; the third storage tank 10 is a diisopropyl succinate storage tank; the solid feeder 11 is a p-chlorobenzonitrile solid feeder.

[0038] In this embodiment, stirring paddles are provided on both the reaction kettle 1 and the water washing kettle 4, and the reaction kettle 1 is provided with a temperature control jacket. Both the reaction kettle 1 and the water washing kettle 4 are made of 316L stainless steel.

[0039] In this embodiment, the second storage tank 7 is provided with a temperature control jacket, and the conveying pipeline is wrapped with heat tracing and heat preservation measures; the second transfer pump 5 is resistant to high temperature of 100 °C.

[0040] The working process of the synthesis device for preparing pigment red 254 using liquid potassium tert-amylate as a raw material given in this embodiment is as follows:

[0041] Step 1, preparation of liquid potassium tert-amylate:

[0042] Transfer tert-amyl alcohol from the first storage tank 6 to the reaction kettle 1 through the second transfer pump 5, and displace the air in the reaction kettle 1 three times with nitrogen from the nitrogen cylinder 15. Start the stirring of the reaction kettle 1, and set the rotation speed to 300 rpm; control the temperature at 100 - 120 °C.

[0043] Dropwise add liquid potassium from the second storage tank 7 to the reaction kettle 1 through the second transfer pump 5. The tail gas is condensed by the first condenser 16 and then enters the water washing type tail gas treatment device 17 for subsequent treatment. Adjust the dropping speed of the liquid potassium according to the tail gas flow rate and temperature change, finish dropping within 1 h, and continue the reaction until no tail gas is released. The reaction is completed in 2 - 3 h to generate liquid potassium tert-amylate.

[0044] Step 2, preparation of pigment red 254:

[0045] The reactor 1 continues to stir, and the material temperature is controlled at 90 - 100 °C. p-Chlorobenzonitrile is added into the reactor 1 through the solid feeder 11, and stirring continues for 10 - 30 min until the system is homogeneous. Meanwhile, diisopropyl succinate in the third storage tank 10 is transferred into the constant pressure dropping funnel 8 through the third transfer pump 9, and diisopropyl succinate is added dropwise through the constant pressure dropping funnel 8. The addition is completed within 2 h. After the addition, the reaction is carried out at a constant temperature for 3 h, and then the stirring is stopped to obtain the reaction completion liquid.

[0046] Step 3, post-treatment:

[0047] First, set the temperature of the thin-film evaporator 3 to be stable at 105 - 110 °C. The reaction completion liquid in the reactor 1 is evaporated through the thin-film evaporator 3. The tert-amyl alcohol and by-product alcohol generated by evaporation enter the second condenser 18 through the top gas outlet of the shell side of the thin-film evaporator 3 and are condensed and then stored in the recovered alcohol storage tank 19. The concentrated liquid generated by evaporation enters the feed port of the water washing kettle 3 through the bottom discharge port of the shell side of the thin-film evaporator 3 for the next treatment.

[0048] The distilled water in the distilled water storage tank 21 is transferred into the water washing kettle 3 through the fifth transfer pump 20. Stirring is turned on, and water washing is carried out for 0.5 h, and then the stirring is stopped.

[0049] Open the discharge port 402, the second transfer pump 7 and the corresponding valves.

[0050] The water-washed completion liquid in the water washing kettle 4 is transferred into the plate and frame filter press 13 through the fourth transfer pump 12 through the bottom discharge port of the water washing kettle 4. After comprehensive treatment by low-pressure filtration and high-pressure pressing, the wastewater enters the wastewater treatment system through the waste liquid discharge port of the plate and frame filter press 13, and the filter cake is transferred into the spray dryer 14 from the discharge port of the plate and frame filter press 13 for drying to obtain Pigment Red 254.

Claims

1. A synthesis device for preparing Pigment Red 254 using liquid potassium tert-amyl alcohol as a raw material, comprising a reaction kettle (1), characterized in that: The bottom discharge port of the reaction kettle (1) is connected to the shell side feed port of the thin film evaporator (3) through a first transfer pump (2), and the shell side bottom discharge port of the thin film evaporator (3) is connected to the feed port of the water washing kettle (4); The feed inlet of the reaction kettle (1) is connected to the first storage tank (6) via a second material transfer pump (5), and the feed inlet of the reaction kettle (1) is also connected to the second storage tank (7) via the second material transfer pump (5); The feed inlet of the reaction kettle (1) is also connected to a constant pressure dropper (8), and the constant pressure dropper (8) is connected to a third storage tank (10) via a third material transfer pump (9); the feed inlet of the reaction kettle (1) is also connected to a solid feeder (11).

2. A synthesis device for preparing Pigment Red 254 using liquid potassium tert-amyl alcoholate as claimed in claim 1 as a raw material, characterized in that: The bottom discharge port of the water washing kettle (4) is connected to the feed port of the plate-frame filter press (13) via a fourth transfer pump (12); the discharge port of the plate-frame filter press (13) is connected to the feed port of the spray dryer (14).

3. A synthesis device for preparing Pigment Red 254 using liquid potassium tert-amyl alcohol as claimed in claim 1 as a raw material, characterized in that: The air inlet of the reaction kettle (1) is connected to a nitrogen bottle (15).

4. A synthesis device for preparing Pigment Red 254 using liquid potassium tert-amyl alcohol as a raw material as claimed in claim 1, characterized in that: The gas outlet of the reactor (1) is connected to the shell side input end of the first condenser (16), and the shell side output end of the first condenser (16) is connected to the water-washing tail gas treatment equipment (17).

5. A synthesis device for preparing Pigment Red 254 using the liquid potassium tert-amyl alcoholate as claimed in claim 1 as a raw material, characterized in that: The shell side top gas outlet of the thin film evaporator (3) is directly connected to the shell side input end of the second condenser (18), and the shell side output end of the second condenser (18) is connected to the recovered alcohol storage tank (19).

6. A synthesis device for preparing Pigment Red 254 using the liquid potassium tert-amyl alcoholate as claimed in claim 1 as a raw material, characterized in that: The top feed port of the water washing kettle (4) is connected to the distilled water storage tank (21) via a fifth transfer pump (20).

7. A synthesis device for preparing Pigment Red 254 using the liquid potassium tert-amyl alcoholate as claimed in claim 1 as a raw material, characterized in that: The first storage tank (6) is a tert-amyl alcohol storage tank; the second storage tank (7) is a liquid potassium storage tank; the third storage tank (10) is a diisopropyl succinate storage tank; and the solid feeder (11) is a p-chlorobenzonitrile solid feeder.

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