Synthesizer for preparing modified pigment red 254 from di-tert-butyl dicarbonate

Abstract

The utility model discloses a synthesis device for preparing modified pigment red 254 from di-tert-butyl dicarbonate. A discharge hole in the bottom of a first reaction kettle is connected with a feed hole of a second reaction kettle through a first transfer pump; a feeding hole of the second reaction kettle is connected with a tetrahydrofuran storage tank through a second transfer pump; a discharge hole in the bottom of the acyl chloride preparation tank is connected with a constant-pressure dropping device through a third transfer pump, and the constant-pressure dropping device is connected with a feed hole of the second reaction kettle; a gas inlet of the second reaction kettle is connected with a carbon dioxide gas cylinder through an anti-suck-back device; a bottom discharge port of the second reaction kettle is connected with a feed port of the third reaction kettle through a fourth transfer pump; a top gas outlet of the second reaction kettle is connected with the first washing type tail gas treatment equipment. According to the device, tert-butoxycarbonyl is introduced to imino groups of the pigment for modification, so that an intermolecular hydrogen bond net is destroyed, and insoluble pigment is changed into soluble modified pigment.

Description

Technical Field

[0001] The utility model belongs to the technical field of pigments, relates to Pigment Red 254, and specifically relates to a synthesis device for preparing modified Pigment Red 254 from di-tert-butyl dicarbonate. Background Art

[0002] Pigment Red 254 is also known as bis(p-chlorophenyl)-1,4-diketopyrrolopyrrole. Pigment Red 254 is a high-performance organic pigment with the advantages of bright color and strong tinting power. It contains a cyclic amide group in the molecule, has a high molecular polarity, and has excellent heat resistance, light resistance and solvent resistance. It can be widely used in plastics, paints, and coatings. It has high commercial value and development potential, but it is easy to form an intermolecular hydrogen bond network, making it more difficult to disperse. It is insoluble in water and most organic solvents, which affects the pigment's color, transparency and other application properties.

[0003] The traditional dispersion method is to grind or perform surface treatment on the pigment, and add organic amines, rosin, surfactants or molecular dispersants to the pigment dispersion system. The host adsorbed on the surface of the pigment particles can reduce the surface energy of the particles, generate a double electric layer or space barrier around the particles, and use electrostatic repulsion or entropy effect to prevent the particles from approaching and aggregating. Some people also use steam or high pressure methods to disperse pigments. Although the dispersion effect of the pigment has been further improved, in general, physical dispersion is a very energy-consuming and time-consuming process, and it cannot fundamentally eliminate the possibility of pigment particle aggregation. Therefore, improving the dispersibility of the pigment is of great significance to expanding its application field. Summary of the invention

[0004] In view of the shortcomings of the prior art, the purpose of the utility model is to provide a synthesis device for preparing modified Pigment Red 254 from di-tert-butyl dicarbonate, so as to solve the technical problem that the product quality stability of the synthesis device in the prior art needs to be further improved.

[0005] In order to solve the above technical problems, the utility model adopts the following technical solutions:

[0006] A synthesis device comprises a first reaction kettle, a second reaction kettle, an acyl chloride preparation tank and a third reaction kettle.

[0007] The bottom discharge port of the first reactor is connected to the feed port of the second reactor through a first transfer pump.

[0008] The feed inlet of the second reaction kettle is connected to the tetrahydrofuran storage tank through a second feed transfer pump.

[0009] The bottom discharge port of the acyl chloride preparation tank is connected to a constant pressure dropper through a third material transfer pump, and the constant pressure dropper is connected to a feed port of the second reaction kettle.

[0010] The air inlet of the second reaction kettle is connected to the carbon dioxide cylinder through an anti-backflow device.

[0011] The bottom discharge port of the second reactor is connected to the feed port of the third reactor through a fourth transfer pump.

[0012] The top gas outlet of the second reactor is connected to the first water-washing tail gas treatment equipment.

[0013] The utility model also has the following technical features:

[0014] The top gas outlet of the third reactor is connected to the shell side inlet of the first condenser, and the shell side outlet of the first condenser is connected to the tetrahydrofuran storage tank through the fifth material transfer pump.

[0015] The feed inlet of the first reactor is connected to the tert-butyl alcohol storage tank through the sixth transfer pump, the feed inlet of the first reactor is also connected to the liquid potassium storage tank through the seventh transfer pump, and the air inlet of the first reactor is connected to the nitrogen bottle; the air outlet of the first reactor is connected to the shell side inlet of the second condenser, and the shell side outlet of the second condenser is divided into two branches, one branch is connected to the second water-washing tail gas treatment equipment, and the other branch is connected to the tert-butyl alcohol storage tank through the eighth transfer pump.

[0016] The feed inlet of the acyl chloride preparation tank is connected to the acyl chloride storage tank through a ninth transfer pump, and the feed inlet of the acyl chloride preparation tank is also connected to the tetrahydrofuran storage tank through a second transfer pump.

[0017] The bottom discharge port of the first reactor is also connected to the feed port of the fourth reactor through the tenth transfer pump; the feed port of the fourth reactor is also connected to the diisopropyl succinate storage tank through the tenth transfer pump, and the air inlet of the fourth reactor is connected to the nitrogen bottle; the bottom discharge port of the fourth reactor is also connected to the feed port of the third reactor through the eleventh transfer pump; the top air outlet of the fourth reactor is connected to the shell side inlet of the third condenser, and the shell side outlet of the third condenser is connected to the recovered alcohol storage tank through the twelfth transfer pump.

[0018] Compared with the prior art, the utility model has the following beneficial technical effects:

[0019] (I) This device introduces tert-butoxycarbonyl into the imino group of the pigment for modification, destroying the hydrogen bond network between molecules and turning the insoluble pigment into a soluble modified pigment. When used, the modified pigment is converted back into the parent pigment after proper treatment. The solubility of the modified pigment and its parent pigment are used to convert into each other to disperse the pigment and expand the application range of the pigment.

[0020] (II) In this device, the liquid potassium tert-butoxide synthesized from liquid potassium and tert-butanol is used as both the reaction solvent and catalyst of Pigment Red 254 and the synthetic raw material of the modifier di-tert-butyl dicarbonate; tetrahydrofuran is used as both the solvent for synthesizing the modifier and the solvent for synthesizing the modified Pigment Red 254; the crude di-tert-butyl dicarbonate does not need to be refined, evaporated, or other post-processing, and can be directly used to modify Pigment Red 254, or it can be refined in the next step to obtain the di-tert-butyl dicarbonate product. This closed-loop operation not only saves energy and simplifies the process, but also controls the quality of the product from the source. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 Schematic diagram of the connection relationship of the synthesis device for preparing modified Pigment Red 254 from di-tert-butyl dicarbonate.

[0022] The meanings of the numbers in the figure are: 1-first reactor, 2-second reactor, 3-acyl chloride preparation tank, 4-third reactor, 5-fourth reactor, 6-first transfer pump, 7-second transfer pump, 8-tetrahydrofuran storage tank, 9-third transfer pump, 10-constant pressure dropper, 11-anti-backflow device, 12-carbon dioxide cylinder, 13-fourth transfer pump, 14-first water-washing tail gas treatment equipment, 15-first condenser, 16-fifth transfer pump, 17-sixth transfer Material pump, 18-tert-butyl alcohol storage tank, 19-the seventh material transfer pump, 20-liquid potassium storage tank, 21-nitrogen bottle, 22-the second condenser, 23-the eighth material transfer pump, 24-the ninth material transfer pump, 25-acyl chloride storage tank, 26-the tenth material transfer pump, 27-diisopropyl succinate storage tank, 28-the eleventh material transfer pump, 29-the third condenser, 30-the twelfth material transfer pump, 31-recovered alcohol storage tank, 32-the second water-washed tail gas treatment equipment, 33-pipeline, 34-valve.

[0023] The specific contents of the utility model are further explained in detail below in conjunction with the embodiments. DETAILED DESCRIPTION

[0024] It should be noted that, unless otherwise specified, all parts and materials in the present invention are parts and materials known in the prior art.

[0025] In the utility model, each device is connected mainly through a pipeline 33, and each pipeline is provided with a valve 34 as required, and is opened or closed according to the process requirements. All valves 34 in the utility model are 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 all equivalent changes made on the basis of the technical solution of this application fall within the protection scope of the present utility model.

[0027] Example:

[0028] This embodiment provides a synthesis device for preparing modified Pigment Red 254 from di-tert-butyl dicarbonate. Figure 1 As shown, it includes a first reaction kettle 1, a second reaction kettle 2, an acyl chloride preparation tank 3 and a third reaction kettle 4.

[0029] The bottom discharge port of the first reaction kettle 1 is connected to the feed port of the second reaction kettle 2 through the first transfer pump 6 .

[0030] The feed inlet of the second reaction kettle 2 is connected to the tetrahydrofuran storage tank 8 through the second transfer pump 7 .

[0031] The bottom discharge port of the acyl chloride preparation tank 3 is connected to a constant pressure dropper 10 through a third transfer pump 9 , and the constant pressure dropper 10 is connected to a feed port of the second reaction kettle 2 .

[0032] The air inlet of the second reactor 2 is connected to a carbon dioxide gas cylinder 12 via an anti-backflow device 11 .

[0033] The bottom discharge port of the second reactor 2 is connected to the feed port of the third reactor 4 through the fourth transfer pump 13 .

[0034] The top gas outlet of the second reactor 2 is connected to the first water-washing tail gas treatment equipment 14 .

[0035] As a preferred solution of this embodiment, Figure 1 As shown, the top gas outlet of the third reactor 4 is connected to the shell side inlet of the first condenser 15 , and the shell side outlet of the first condenser 15 is connected to the tetrahydrofuran storage tank 8 through the fifth material transfer pump 16 .

[0036] As a preferred solution of this embodiment, Figure 1 As shown, the feed port of the first reactor 1 is connected to the tert-butyl alcohol storage tank 18 through the sixth transfer pump 17, and the feed port of the first reactor 1 is also connected to the liquid potassium storage tank 20 through the seventh transfer pump 19, and the air inlet of the first reactor 1 is connected to the nitrogen bottle 21; the air outlet of the first reactor 1 is connected to the shell side inlet of the second condenser 22, and the shell side outlet of the second condenser 22 is divided into two branches, one branch is connected to the second water-washing tail gas treatment equipment 32, and the other branch is connected to the tert-butyl alcohol storage tank 18 through the eighth transfer pump 23.

[0037] As a preferred solution of this embodiment, Figure 1 As shown, the feed inlet of the acyl chloride preparation tank 3 is connected to the acyl chloride storage tank 25 via the ninth transfer pump 24 , and the feed inlet of the acyl chloride preparation tank 3 is also connected to the tetrahydrofuran storage tank 8 via the second transfer pump 7 .

[0038] As a preferred solution of this embodiment, Figure 1As shown, the bottom discharge port of the first reactor 1 is also connected to the feed port of the fourth reactor 5 through the tenth transfer pump 26; the feed port of the fourth reactor 5 is also connected to the diisopropyl succinate storage tank 27 through the tenth transfer pump 26, and the air inlet of the fourth reactor 5 is connected to the nitrogen bottle 21; the bottom discharge port of the fourth reactor 5 is also connected to the feed port of the third reactor 4 through the eleventh transfer pump 28; the top air outlet of the fourth reactor 5 is connected to the shell side inlet of the third condenser 29, and the shell side outlet of the third condenser 29 is connected to the recovered alcohol storage tank 31 through the twelfth transfer pump 30.

[0039] In this embodiment, the first reaction kettle 1 , the second reaction kettle 2 , the acyl chloride preparation tank 3 , the third reaction kettle 4 and the fourth reaction kettle 5 are all provided with stirring paddles and temperature control jackets.

[0040] In this embodiment, the liquid potassium storage tank 20 is provided with a temperature control jacket, and the delivery pipeline is wrapped with heating and insulation measures.

[0041] In this embodiment, the seventh material transfer pump 19 can withstand a high temperature of 100°C.

[0042] The working process of the synthesis device for preparing modified Pigment Red 254 from di-tert-butyl dicarbonate given in this embodiment is as follows:

[0043] Step 1, preparation of potassium tert-butoxide:

[0044] The tert-butyl alcohol is transferred from the tert-butyl alcohol storage tank 18 to the first reactor 1 , and the nitrogen in the nitrogen bottle 21 is introduced into the air inlet of the first reactor 1 , and nitrogen replacement is performed three times, and the air inlet of the first reactor 1 is closed.

[0045] Start stirring the first reactor 1, set the speed to 300rpm; control the temperature at 100-120°C. Start dripping liquid potassium through the seventh transfer pump 19, and the tail gas is condensed by the second condenser 22 and enters the second water-wash tail gas treatment equipment 32 for subsequent treatment. The condensate returns to the first reactor 1 through the outlet of the first reactor 1. Adjust the speed of dripping liquid potassium according to the tail gas flow rate and temperature change, and complete the dripping within 1 hour, and continue the reaction until no tail gas is released. The reaction is completed in 2-3 hours to generate a tert-butanol solution of potassium tert-butoxide.

[0046] A portion of the tert-butanol solution of potassium tert-butoxide is subsequently directly input into the fourth reactor 5 for the preparation of crude Pigment Red 254; another portion of the tert-butanol solution of potassium tert-butoxide needs to be distilled to obtain solid potassium tert-butoxide, which is subsequently input into the second reactor 2 for the preparation of di-tert-butyl dicarbonate.

[0047] The specific distillation process is as follows: the first reactor 1 is gradually heated to 140°C and distilled for 4 hours. The gaseous tert-butyl alcohol produced by distillation is cooled by the second condenser 22 and then transferred to the tert-butyl alcohol storage tank 18 for storage and standby through the eighth transfer pump 23. The solid produced by distillation is solid potassium tert-butylate.

[0048] Step 2, preparation of di-tert-butyl dicarbonate:

[0049] The tetrahydrofuran in the tetrahydrofuran storage tank 8 is transferred to the second reactor 2 through the second transfer pump 7, stirring is started, and the temperature of the reactor is controlled at 0°C to -5°C. The solid potassium tert-butoxide is directly transported into the second reactor 2 through the first transfer pump 6, and stirred for 30 minutes until the potassium tert-butoxide is completely dissolved. The dissolution process will release heat and the temperature will drop to 0°C to -5°C, and then the carbon dioxide in the carbon dioxide cylinder 12 is introduced into the second reactor 2 for reaction, and the reaction is completed in 1 hour.

[0050] At the same time, prepare the acyl chloride solution, transfer the tetrahydrofuran in the tetrahydrofuran storage tank 8 into the acyl chloride preparation tank 3. Transfer the acyl chloride in the acyl chloride storage tank 25 into the acyl chloride preparation tank 3, stir and dissolve for 0.5h for later use.

[0051] The prepared acyl chloride solution is added dropwise to the second reaction kettle 2 through the third material transfer pump 9 and the constant pressure dropper 10 for 1 hour and reacted for 2 hours to obtain a crude di-tert-butyl dicarbonate reaction liquid for standby use.

[0052] Step 3, preparation of crude Pigment Red 254:

[0053] Chlorobenzonitrile was added through the manual feeding port of the fourth reactor 5, and nitrogen replacement was performed 3 times. The tert-butyl alcohol solution of potassium tert-butylate in the first reactor 1 was transferred to the fourth reactor 5 through the tenth transfer pump 26, stirring was started, the material temperature was controlled at 90-100°C, and stirring was performed for 10-30 minutes until the system was uniform. The diisopropyl succinate in the diisopropyl succinate storage tank 27 was also transferred to the fourth reactor 5 through the tenth transfer pump 26, and the reaction was carried out at a constant temperature for 3 hours, and the stirring was stopped to obtain the crude reaction liquid of Pigment Red 254.

[0054] For the crude reaction liquid of Pigment Red 254, the temperature in the fourth reactor 5 is set to 120°C to start distillation, and tert-butyl alcohol and by-product alcohol generated by the reaction, i.e., mixed alcohol, are distilled out. The mixed alcohol is condensed by the third condenser 29 and then enters the recovery alcohol storage tank 31 for storage through the twelfth transfer pump 30. The distillation is completed in 2-3 hours to obtain crude Pigment Red 254.

[0055] Step 4: Preparation of modified Pigment Red 254:

[0056] The crude di-tert-butyl dicarbonate reaction liquid obtained in step 2 is transferred into the third reaction kettle 4 through the fourth transfer pump 13, and stirring is started. The crude pigment red 254 obtained in step 3 is transferred into the third reaction kettle 4 through the eleventh transfer pump 28, and the reaction is carried out at room temperature for 3 hours.

[0057] After the reaction is completed, the temperature of the third reaction kettle 4 is set to 35-40° C., and distillation is started. The distilled tetrahydrofuran is cooled by the first condenser 15 and then transferred to the tetrahydrofuran storage tank 8 by the fifth transfer pump 16 for standby use. After the distillation is completed, modified Pigment Red 254 is obtained.

[0058] In the utility model, liquid potassium tert-amyl alcohol is used as both a solvent and a catalyst for the condensation reaction, which not only greatly improves the reaction rate, but also controls the product quality from the source; a thin film evaporator is used for distillation pretreatment, which has high heat transfer efficiency and fast evaporation speed; a plate and frame filter press is used for low-pressure filtration and high-pressure pressing, which can greatly shorten the entire filtration cycle; a spray dryer is used for product drying, which simplifies the production process and is convenient for operation and control, thereby solving the technical problems of low efficiency, low yield and unstable quality of the device disclosed in the prior art.

[0059] In the utility model, the liquid potassium tert-butoxide synthesized from liquid potassium and tert-butanol is used as both the reaction solvent and catalyst of Pigment Red 254 and the synthetic raw material of the modifier di-tert-butyl dicarbonate; tetrahydrofuran is used as both the solvent for synthesizing the modifier and the solvent for synthesizing the modified Pigment Red 254; the crude di-tert-butyl dicarbonate does not need to be refined, evaporated, and other post-processing, and can be directly used to modify Pigment Red 254, so that the insoluble pigment becomes a soluble modified pigment, thereby improving the dispersibility of the pigment and expanding the application range of the pigment, and can also be refined in the next step to obtain the di-tert-butyl dicarbonate product. This closed-loop operation not only saves energy and simplifies the process, but also controls the quality of the product from the source.

Claims

1. A synthesis device for preparing modified Pigment Red 254 from di-tert-butyl dicarbonate, comprising a first reaction kettle (1), a second reaction kettle (2), an acyl chloride preparation tank (3) and a third reaction kettle (4), characterized in that: The bottom discharge port of the first reaction kettle (1) is connected to the feed port of the second reaction kettle (2) via a first transfer pump (6); The feed inlet of the second reaction kettle (2) is connected to the tetrahydrofuran storage tank (8) via a second transfer pump (7); The bottom discharge port of the acyl chloride preparation tank (3) is connected to a constant pressure dropper (10) via a third transfer pump (9), and the constant pressure dropper (10) is connected to a feed port of the second reaction kettle (2); The air inlet of the second reaction kettle (2) is connected to the carbon dioxide gas cylinder (12) via the anti-backflow device (11); The bottom discharge port of the second reaction kettle (2) is connected to the feed port of the third reaction kettle (4) via a fourth transfer pump (13); The top gas outlet of the second reaction kettle (2) is connected to the first water-washing tail gas treatment equipment (14).

2. The synthesis device according to claim 1, characterized in that The top gas outlet of the third reaction kettle (4) is connected to the shell side inlet of the first condenser (15), and the shell side outlet of the first condenser (15) is connected to the tetrahydrofuran storage tank (8) via a fifth transfer pump (16).

3. The synthesis device according to claim 1, characterized in that The feed inlet of the first reactor (1) is connected to the tert-butyl alcohol storage tank (18) via a sixth transfer pump (17), and the feed inlet of the first reactor (1) is also connected to the liquid potassium storage tank (20) via a seventh transfer pump (19). The air inlet of the first reactor (1) is connected to a nitrogen bottle (21); the air outlet of the first reactor (1) is connected to the shell side inlet of the second condenser (22), and the shell side outlet of the second condenser (22) is divided into two branches, one branch is connected to the second water-washing tail gas treatment equipment (32), and the other branch is connected to the tert-butyl alcohol storage tank (18) via an eighth transfer pump (23).

4. The synthesis device according to claim 1, characterized in that The feed inlet of the acyl chloride preparation tank (3) is connected to the acyl chloride storage tank (25) via a ninth transfer pump (24), and the feed inlet of the acyl chloride preparation tank (3) is also connected to the tetrahydrofuran storage tank (8) via a second transfer pump (7).

5. The synthesis device according to claim 1, characterized in that The bottom discharge port of the first reactor (1) is also connected to the feed port of the fourth reactor (5) via a tenth transfer pump (26); the feed port of the fourth reactor (5) is also connected to the diisopropyl succinate storage tank (27) via a tenth transfer pump (26), and the air inlet of the fourth reactor (5) is connected to the nitrogen bottle (21); the bottom discharge port of the fourth reactor (5) is also connected to the feed port of the third reactor (4) via an eleventh transfer pump (28); the top air outlet of the fourth reactor (5) is connected to the shell side inlet of the third condenser (29), and the shell side outlet of the third condenser (29) is connected to the recovered alcohol storage tank (31) via a twelfth transfer pump (30).

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