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CN-121974918-A - Application of benzoate compound in copper phthalocyanine synthesis process

CN121974918ACN 121974918 ACN121974918 ACN 121974918ACN-121974918-A

Abstract

The invention provides an application of benzoate compounds in a copper phthalocyanine synthesis process, which comprises the following steps of S1, adding 3 g of benzoate compounds, 310 g of 100% phthalic anhydride, 231 g of urea and 1500 ml of solvent alkylbenzene into a 3000 ml three-port bottle provided with a stirring device, a thermometer and a condenser, uniformly heating to 170 ℃ in 4 hours under stirring, preserving heat for 2 hours, S2, adding 231 g of urea, uniformly heating to 190 ℃ in the hour, preserving heat for 2 hours, and S3, adding 61 g of 100% cuprous chloride and 4 g of 100% ammonium molybdate, uniformly heating to 210 ℃ in the 5 hour, preserving heat, stirring, reacting for 6 hours, and cooling to 100 ℃. The invention provides the application of benzoate compounds in the copper phthalocyanine synthesis process, and the proper amount of benzoate compounds is added in the copper phthalocyanine synthesis process to improve the product yield, reduce the raw material consumption and reduce the three-waste emission, thereby reducing the production cost and the environmental pollution.

Inventors

  • ZHANG XUESHAN
  • ZHU JIANJUN
  • QIU RONGZHOU
  • DONG WEI

Assignees

  • 双乐颜料股份有限公司

Dates

Publication Date
20260505
Application Date
20260202

Claims (10)

  1. 1. The application of the benzoate compound in the synthesis process of copper phthalocyanine is characterized by comprising the following steps: s1, adding 3 g of benzoate compound, 310 g of 100% phthalic anhydride, 231 g of urea and 1500 ml of solvent alkylbenzene into a 3000 ml three-port bottle provided with a stirring device, a thermometer and a condenser, uniformly heating to 170 ℃ for 4 hours under stirring, and preserving heat for 2 hours; S2, adding 231 g of urea, uniformly heating to 190 ℃ in an hour period, and preserving heat for 2 hours; s3, adding 61 g of 100% cuprous chloride and 4g of 100% ammonium molybdate, uniformly heating to 210 ℃ in 5 hours, preserving heat, stirring and reacting for 6 hours, and cooling to 100 ℃; S4, adding 50 g of 30% sodium hydroxide solution, and distilling to recover solvent alkylbenzene by steam, wherein no solvent is distilled out after about 5 hours, and the distillation is completed; s5, after filtration, water washing and drying, 295 g of copper phthalocyanine is obtained, the content is 90%, and the yield is 88%.
  2. 2. The application of the benzoate compound in the copper phthalocyanine synthesis process according to claim 1, wherein the benzoate compound in the step 1 is methyl benzoate, ethyl benzoate, n-propyl benzoate, isopropyl benzoate, n-butyl benzoate, isobutyl benzoate, tert-butyl benzoate.
  3. 3. The application of the benzoate compound in the synthesis process of copper phthalocyanine according to claim 1, wherein an adjusting rod is fixedly arranged at the top of the stirring device, and an adjusting device is fixedly arranged on the surface of the adjusting rod.
  4. 4. The use of a benzoate compound according to claim 3 in a copper phthalocyanine synthesis process, wherein the stirring device comprises a controller, a stirring motor, a stirring rod and two stirring blades, the stirring motor is fixedly installed at the top of the adjusting device, one end of the stirring rod is fixedly installed at the output end of the stirring motor, and the two stirring blades are respectively and rotatably connected to two sides of one end of the stirring rod.
  5. 5. The application of benzoate compound in copper phthalocyanine synthesis process according to claim 4, wherein the surface of the stirring rod is provided with a folding device, the folding device comprises a fixing piece, a sliding sleeve, two connecting rods, two moving grooves and two moving blocks, the fixing piece is arranged on the surface of the stirring rod, the sliding sleeve is arranged at one end of the fixing piece, one ends of the two connecting rods are respectively connected to two sides of one end of the sliding sleeve in a rotating mode, the two moving grooves are respectively arranged in the two stirring blades, and the two moving blocks are respectively connected to the two moving grooves in a sliding mode.
  6. 6. The use of benzoate compounds according to claim 5, wherein said fastener is a threaded sleeve threadably attached to the surface of said stirring rod.
  7. 7. The use of benzoate compounds according to claim 5, wherein two ends of said connecting rod are rotatably connected to the surfaces of said sliding sleeve and said moving block, respectively.
  8. 8. The application of the benzoate compound in the synthesis process of copper phthalocyanine according to claim 1, wherein a heating device is arranged on the surface of the three-necked flask, a fixing clamp is arranged on the top of the heating device, and a protection pad is fixedly arranged on the surface of the fixing clamp.
  9. 9. The use of benzoate compounds according to claim 8, wherein a limiting device is provided inside the heating device, and the limiting device is used for limiting the space between the fixing clip and the heating device.
  10. 10. The application of benzoate compound according to claim 9, wherein the limiting device comprises a limiting groove, a limiting block and a limiting pin, the limiting groove is formed in the heating device, the limiting block is slidably connected in the limiting groove, and the limiting pin is in threaded connection with the limiting block.

Description

Application of benzoate compound in copper phthalocyanine synthesis process Technical Field The invention relates to the field of copper phthalocyanine production, in particular to application of benzoate compounds in the synthesis process of copper phthalocyanine. Background Phthalocyanine blue is also called CuPc, pigment blue 15, chemical formula C32H16CuN8, CAS number 147-14-8, molecular weight 576.07, is a blue organic pigment. The appearance is bright green blue rod-shaped crystals or powder, the crystal is flammable, and two crystal forms exist, wherein the crystal forms are more stable, the melting point is 600 ℃, the crystal is insoluble in water, alcohol and hydrocarbon solvents, and the crystal is soluble in concentrated sulfuric acid to form olive-colored solution, and blue suspension is separated out after dilution. In the existing copper phthalocyanine synthesis process, raw material consumption is large, and three wastes are discharged in large quantity, so that the production cost is increased, and meanwhile, the environment is polluted. Therefore, there is a need to provide the application of benzoate compounds in the synthesis process of copper phthalocyanine to solve the above technical problems. Disclosure of Invention The invention provides application of benzoate compounds in the synthesis process of copper phthalocyanine, and solves the problems of larger raw material consumption and large discharge amount of three wastes in the existing synthesis process of copper phthalocyanine. In order to solve the technical problems, the application of the benzoate compound in the synthesis process of copper phthalocyanine provided by the invention comprises the following steps: s1, adding 3 g of benzoate compound, 310 g of 100% phthalic anhydride, 231 g of urea and 1500 ml of solvent alkylbenzene into a 3000 ml three-port bottle provided with a stirring device, a thermometer and a condenser, uniformly heating to 170 ℃ for 4 hours under stirring, and preserving heat for 2 hours; S2, adding 231 g of urea, uniformly heating to 190 ℃ in an hour period, and preserving heat for 2 hours; s3, adding 61 g of 100% cuprous chloride and 4g of 100% ammonium molybdate, uniformly heating to 210 ℃ in 5 hours, preserving heat, stirring and reacting for 6 hours, and cooling to 100 ℃; S4, adding 50 g of 30% sodium hydroxide solution, and distilling to recover solvent alkylbenzene by steam, wherein no solvent is distilled out after about 5 hours, and the distillation is completed; s5, after filtration, water washing and drying, 295 g of copper phthalocyanine is obtained, the content is 90%, and the yield is 88%. Preferably, the benzoate compound in the step 1 is methyl benzoate, ethyl benzoate, n-propyl benzoate, isopropyl benzoate, n-butyl benzoate, isobutyl benzoate, or tert-butyl benzoate. Preferably, an adjusting rod is fixedly arranged at the top of the stirring device, and an adjusting device is fixedly arranged on the surface of the adjusting rod. Preferably, the stirring device comprises a controller, a stirring motor, a stirring rod and two stirring blades, wherein the stirring motor is fixedly arranged at the top of the adjusting device, one end of the stirring rod is fixedly arranged at the output end of the stirring motor, and the two stirring blades are respectively and rotatably connected to two sides of one end of the stirring rod. Preferably, the surface of puddler is provided with folding device, folding device includes mounting, slip cap, two connecting rods, two movable grooves and two movable blocks, the mounting set up in the surface of puddler, the slip cap set up in the one end of mounting, two the one end of connecting rod rotate respectively connect in the both sides of slip cap one end, two the movable groove is seted up respectively in two the inside of stirring leaf, two the movable block sliding connection respectively in two the inside of movable groove. Preferably, the fixing piece is a threaded sleeve, and the threaded sleeve is in threaded connection with the surface of the stirring rod. Preferably, two ends of the connecting rod are respectively connected to the surfaces of the sliding sleeve and the moving block in a rotating manner. Preferably, the surface of three mouthfuls of bottles is provided with heating device, heating device's top is provided with the fixation clamp, the surface fixed mounting of fixation clamp has the protection pad. Preferably, a limiting device is arranged in the heating device, and the limiting device is used for limiting the space between the fixing clamp and the heating device. Preferably, the limiting device comprises a limiting groove, a limiting block and a limiting pin, wherein the limiting groove is formed in the heating device, the limiting block is slidably connected to the inside of the limiting groove, and the limiting pin is in threaded connection with the inside of the limiting block. Compared with the related art, the application of the