Anti-oxidation single component aromatic hydrocarbon solvent used in copper phthalocyanine synthesis

An aromatic solvent, oxidation-resistant technology, applied in organic chemistry, chemical instruments and methods, porphine/acridine porphine, etc., can solve the problem of unstable copper phthalocyanine quality and yield, affecting the use range of copper phthalocyanine, and color deviation Green phase and other problems, to achieve the effect of promoting environmental protection, good oxidation resistance, high purity

Inactive Publication Date: 2004-09-29
赵维绳
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to achieve the above purpose, foreign companies use alkylbenzene as a breakthrough point for new solvents, and a large number of alkylbenzene solvents have appeared, such as: o-nitrotoluene, 2,4-dichlorotoluene, dimethylchlorobenzene, isopropyl- 1,2,4-Trimethylbenzene, t-butylbenzene, t-hexylbenzene, t-amylbenzene, 2-chloro-4-isopropyltoluene, diisopropylbenzene, dimethylethylbenzene, diphenyl Methane, diethylbenzene, etc.; according to the Japanese patent (Japanese Patent Application No. 57-65755), Solvent150 uses the side chain as C 4 ~C 5 The mixture of alkylbenzene as the main component has a boiling point of 150-320°C; however, only Nisseki Hisol P developed by Nipponpetrochemical Co.Ltd is actually used in the market. Compounds: 20-25% of t-amylbenzene, 55-60% of t-hexylbenzene, 15% of t-heptylbenzene, 5-10% of unknown components; it has been verified by domestic production that no copper phthalocyanine is formed during the production of copper phthalocyanine PCB, its oxidation resistance is still good, but the quality and yield of the obtained copper phthalocyanine are very unstable, with a large fluctuation range, and the copper phthalocyanine is processed into a pigment (dye) coloring agent, and the shade is very green , affecting the scope of use of copper phthalocyanine; the reason may be due to the different physicochemical properties of various alkylbenzenes, so it is necessary to explore the technical route of synthesizing a single-component aromatic hydrocarbon solvent

Method used

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  • Anti-oxidation single component aromatic hydrocarbon solvent used in copper phthalocyanine synthesis
  • Anti-oxidation single component aromatic hydrocarbon solvent used in copper phthalocyanine synthesis
  • Anti-oxidation single component aromatic hydrocarbon solvent used in copper phthalocyanine synthesis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] In a glass reactor with a volume of 2 liters, add 1000 parts of raw material ethylbenzene (purity ≥ 99%), 650 parts of catalyst concentrated sulfuric acid, stir and cool to below 20 ° C, and put 700 parts of isobutylene (purity ≥ 99%) through dehydration. %), is passed into the reactor from the bottom of the reactor, and during the passage, the reaction temperature is kept at about 30°C. When the amount of monoolefin feed is close to the specified amount, samples are taken from the reactor at any time for GC (gas chromatography) Analysis, when the content of the finished product in the reaction mixture reaches the requirements, stop the reaction, separate and recover the catalyst, and use it for the next batch of synthesis. The product obtained by the separation is purified to obtain about 1335 parts of the crude product solvent, and the content is about 90%; Purified by distillation to obtain 1197 parts of aromatic hydrocarbon solvent compound A, with a content of 98.8-...

Embodiment 2

[0024] In a glass reactor with a volume of 2 liters, add 1000 parts of raw material ethylbenzene (purity ≥ 99%), 150 parts of catalyst anhydrous aluminum trichloride (purity ≥ 97%), stir and cool to below 10°C, and 750 parts of isobutylene (purity ≥ 99%) dehydrated are passed into the reactor from the bottom of the reactor. During the passage, the reaction temperature is kept at 5-10°C. When the amount of single-bond olefin is close to the specified amount, Sampling from the reactor at any time for GC analysis, when the content of the finished product in the reaction mixture reaches the requirements, stop the reaction, separate and recover the catalyst, and use it for the next batch of synthesis. The product obtained from the separation is purified to obtain about 1260 parts of the crude product solvent. The content is about 90%; the crude product is purified by rectification to obtain 1130 parts of pure solvent, the content is 98.2-98.5%, and the yield is 85.3-86.4%; its infra...

Embodiment 3

[0026] According to the same method as in Example 1, the content of aromatic hydrocarbon solvent compound B obtained by synthesis is 98.6~99.3%, the yield is 89~93%, and its infrared absorption characteristic peak is: 3000~2800cm -1 , 1600~1500cm -1 , 900~800cm -1 ;Product appearance: white and transparent water, density 0.875, boiling range 210-216°C, refractive index (n 11 ) 1.5046.

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Abstract

The present invention relates to aromatic hydrocarbon solvent, and is especially oxidationproof single-component aromatic hydrocarbon solvent used in synthesizing copper phthalocyanine. It features the boiling point of 200-220 deg.c, density of 0.86-0.89 and refractivity of 1.5060-1.5080, and has the advantages of being environment friendly and non-toxic, high yield and high purity of copper phthalocyanine product and high oxidation resistance. The solvent may be used in preparing C.I. blue pigment with high strength and pure color.

Description

technical field [0001] The invention relates to an aromatic hydrocarbon solvent, especially an oxidation-resistant single-component aromatic hydrocarbon solvent used in the synthesis of copper phthalocyanine. Background technique [0002] As we all know, trichlorobenzene has been used as a reaction solvent for the production of copper phthalocyanine for a long time, and it is widely used. It is almost considered to be the most ideal solvent, but when it is found that it generates a by-product PCB during the reaction, its application is restricted Therefore, all countries are committed to developing a new solvent to replace trichlorobenzene. According to the description of Japanese patent (Japanese Patent Application No. 57-135866), the organic solvents used to replace trichlorobenzene include: nitrobenzene, diisopropyltoluene, naphthalene, anthracene, alkyl benzoate, carbon tetrachloride, decahydro Naphthalene, chloroalkylbenzene, kerosene, hexachlorobutadiene, C 1 ~C 4 A...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C15/02C07D487/22C09B47/04
Inventor 赵维绳汪维凤
Owner 赵维绳
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