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Synthesis method of orange intermediate

An intermediate, orange technology, applied in the field of orange intermediates, can solve the problems of excessive hydrolysis of phthalic anhydride, low yield, and excessive production of three wastes, and achieve the effects of reducing COD, increasing yield, and reducing consumption of three wastes

Active Publication Date: 2020-10-13
ZHEJIANG YIDE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003]However, in the above method, phthalic anhydride is hydrolyzed more, the yield is low, and the three wastes are generated more

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Prepare a clean reaction vessel, add 200g of sulfuric acid with a mass percentage of 107% into the reaction vessel as a solvent, 8g of catalyst boron anhydride and then heat up to 60°C, then add 50g of phthalic anhydride, then heat up to 120-130°C, add 36g dropwise to melt After the addition of p-chlorophenol, heat it to 195°C, and keep it warm for 5 hours. After the end point is detected by sampling, phthalic anhydride is recovered by distillation under reduced pressure, and then cooled to 160°C, then added to 80°C hot water, and then heated to 100-105 ℃, stand still for 5 hours, separate the upper layer of mother liquor water, add 80 ℃ hot water for beating, filter and wash, and obtain 64.0 g of orange intermediate.

Embodiment 2

[0032] Prepare a clean reaction vessel, add 200g of sulfuric acid with a mass percentage of 107% into the reaction vessel as a solvent, 8g of catalyst boron anhydride and then heat up to 60°C, then add 43.5g of phthalic anhydride, then heat up to 120-130°C, add 36g dropwise Melted p-chlorophenol, heated to 195°C after adding, kept the temperature for 5 hours, and after the end point was detected by sampling, phthalic anhydride was recovered by distillation under reduced pressure, then cooled to 160°C, added to 80°C hot water, and then heated to 100- Stand at 105°C for 5 hours, separate the upper layer of mother liquid water, add 80°C hot water for beating, filter, and wash with water to obtain 62.2g of an orange intermediate.

Embodiment 5

[0038] Example 1 2 3 4 intermediate g 64.0 62.2 43.5 38.9 Catalyst dosage g 8 8 16 16 Phthalic anhydride dosage g 50 43.5 68 68 COD mg / L 3400 3100 21000 20500

[0039] Comparative Analysis Example 1, 3 and 4 and Comparative Analysis Example 2, 3 and 4, we find that adopting 107% sulfuric acid as solvent, boric anhydride as catalyst, compared to adopting 105% sulfuric acid or 98% sulfuric acid as solvent, boric acid as Catalyst, the yield of the orange intermediate 1,4 dihydroxyanthraquinone prepared is higher, the dosage of phthalic anhydride is reduced, the hydrolysis of phthalic anhydride is reduced at the same time, and the three wastes COD are greatly reduced.

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PUM

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Abstract

The invention discloses a synthesis method of an orange intermediate, and belongs to the field of orange intermediates. The synthesis method of the orange intermediate comprises the following steps: 1, preparing 106-110% sulfuric acid as a solvent; 2, adding p-chlorophenol and excessive phthalic anhydride into a clean reaction container, adding a catalyst boric anhydride, and pouring the sulfuricacid solvent obtained in step 1 into the reaction container; 3, heating the reaction container to 190-200 DEG C, and reacting the p-chlorophenol and phthalic anhydride added in step 2 under the actionof a catalyst; and 4, after the reaction is finished, cooling, diluting, separating out upper wastewater, and filtering to obtain the orange intermediate. According to the scheme, 106-110% sulfuric acid is adopted as the solvent, boric anhydride is adopted as the catalyst, and hydrolysis of phthalic anhydride can be greatly reduced, so the use amount of phthalic anhydride is reduced, the yield isgreatly increased, phthalic anhydride is recycled, and COD of three wastes is greatly reduced.

Description

technical field [0001] The present invention relates to the field of orange intermediates, more specifically, relates to the synthesis of an orange intermediate. Background technique [0002] At present, the orange intermediate, that is, 1,4 dihydroxyanthraquinone, its conventional production process is: p-chlorophenol and phthalic anhydride in 98% sulfuric acid or 105% sulfuric acid solvent, add boric acid catalyst to react at a temperature of 160-190 ° C, and then After cooling down, dilute and wash with water. [0003] However, in the above method, phthalic anhydride is hydrolyzed more, the yield is low, and the three wastes are generated more. [0004] The three wastes refer to waste water, waste gas and waste residue. Pollution refers to water, air, soil and other ecological factors that are polluted to a certain extent by chemical substances, radioactive substances, pathogens, noise and waste heat produced in the process of human production and life, which will endan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C50/34C07C46/00C07C46/10
CPCC07C46/00C07C46/10C07C2603/24C07C50/34
Inventor 卢林德蒋志平孟胜锋
Owner ZHEJIANG YIDE CHEM