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Preparation method for solvent orange 60

A solvent orange and polar organic solvent technology, applied in the field of preparation of solvent orange 60, can solve the problems of difficult product separation, low product vividness, and low production cost, so as to reduce production costs and avoid relatively low product vividness , the effect of low production cost

Active Publication Date: 2009-10-28
NANTONG LONGXIANG NEW MATERIALS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The solvent method is a method for producing solvent orange 60 with a polar organic solvent as the reaction medium. The product produced by this method has high vividness and high product quality. However, because solvent orange 60 has a certain solubility in organic solvents, the product The separation is relatively difficult, and the solvent needs to be recovered, so the production cost is high
The aqueous phase method is a method of producing solvent orange with hydrochloric acid aqueous solution as the reaction medium. It only needs to be filtered to realize product separation, and the reaction medium does not need to be recycled, only neutralization treatment is required, so the production cost is relatively low, but the produced by this method Product vividness is relatively low, product quality is poor

Method used

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  • Preparation method for solvent orange 60
  • Preparation method for solvent orange 60
  • Preparation method for solvent orange 60

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 200g of 3% hydrochloric acid aqueous solution, 30g of alcohol, 10g of phthalic anhydride, 10.7g of 1,8-naphthalene diamine, and 0.3g of fatty alcohol polyoxyethylene ether into a three-necked flask with a stirring and reflux condenser, and start stirring , be warming up to reaction system slight reflux state, filter after reacting for 8 hours, filter cake is washed with clear water until the filtrate is neutral, and dry to obtain product 17.5g (being 95.9% of theoretical yield). The color shade of the product is similar to that of the standard product (see Table 1 for details), and the intensity is 99.0%.

[0018] Table 1

[0019]

[0020]

[0021] (Where: ΔE-color difference, ΔH-hue difference, ΔL-brightness difference, ΔC-chroma difference,

[0022] Δa-the difference in redness and greenness, Δb-the difference in yellowness and blueness, the smaller the ΔE, the closer the color of the product is to the standard product. Generally, if ΔE is less than 3, the...

Embodiment 2

[0024] Add 1000kg 5% hydrochloric acid aqueous solution, 100kg dimethylformamide (DMF), 100kg phthalic anhydride, 107kg 1,8-naphthalene diamine, 5kg Nonylphenol polyoxyethylene ether, start stirring, heat up to the state of slight reflux of the reaction system, filter after 12 hours of reaction, wash the filter cake with water until the filtrate is neutral, and dry to obtain 177kg of the product (96.8% of the theoretical yield) . The product is similar to the standard product (see Table 2 for details), and the strength is 101.0%.

[0025] Table 2

[0026] light source

Embodiment 3

[0028] Add 300kg of 1% hydrochloric acid solution, 60kg of acetic acid, 20kg of phthalic anhydride, 21.4kg of 1,8-naphthalene diamine, and 5kg of nonylphenol polyoxyethylene into a 500L enamel reactor with frame stirring and reflux condenser. Ether, start stirring, heat up to the state of slight reflux of the reaction system, filter after reacting for 8 hours, wash the filter cake with water until the filtrate is neutral, and dry to obtain 35kg of product (95.7% of theoretical yield). The product is similar to the standard product (see Table 3 for details), and the strength is 98.9%.

[0029] table 3

[0030] light source

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Abstract

The invention discloses a preparation method for solvent orange 60, belonging to chemical industry field, manufactured by: mixing phthalic anhydride and 1, 8- naphthylenediamine with the mass ratio of 1:1 with 1-5% by mass of hydrochloric acid solution, polar organic solvent miscible with water and non-ionic active catalyst, stirring and heating to the refluxing state for reacting 8-15 hours, filtering, washing the filter cake with water till the pH value of the filtrate is neutral, drying to obtain the solvent orange 60, wherein the dosage of the hydrochloric acid solution is 10-20 times of the 1, 8- naphthylenediamine; the dosage of the polar organic solvent is 1-50% of the total amount of the reaction medium and the dosage of the catalyst is 0.01-2% of the total amount of the reaction medium. The method combines the advantages of good quality and low cost of water phase method.

Description

technical field [0001] The invention relates to a preparation method of solvent orange 60, which belongs to the field of chemical industry. Background technique [0002] Solvent Orange 60, English name Solvent Orange 60, molecular formula: C18H10N2O, molecular weight: 270.29, CAS number: 6925-69-5. Appearance is orange powder, insoluble in water, slightly soluble in ethanol, benzene, toluene, xylene and other organic solvents. Mainly used in polystyrene, ABS resin. Its structural formula is: [0003] [0004] The existing preparation process of Solvent Orange 60 is divided into solvent method and aqueous phase method according to the difference of the reaction medium used. The solvent method is a method for producing solvent orange 60 with a polar organic solvent as the reaction medium. The product produced by this method has high vividness and high product quality. However, because solvent orange 60 has a certain solubility in organic solvents, the product The separa...

Claims

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Application Information

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IPC IPC(8): C09B67/20C09B57/00C07D487/06C08J3/20
Inventor 杨彦青杨连飞吴卫东黄东升倪伟王思源
Owner NANTONG LONGXIANG NEW MATERIALS TECH CO LTD
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