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Preparation method of 4-chlorophthalic acid monosodium salt and 4-chlorophthalic anhydride

A technology of chlorinated phthalic acid and chlorophthalic anhydride, applied in the direction of carboxylate preparation, organic compound preparation, chemical instruments and methods, etc., can solve the problem of 4-chlorophthalic acid monosodium salt Low conversion rate and other problems, to achieve the effect of improving conversion rate and solubility

Pending Publication Date: 2022-06-14
HEBEI HAILI FRAGRANCES CO LTD
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  • Abstract
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Problems solved by technology

The Chinese patent with publication number CN1824638A discloses a production method of 4-chlorophthalic acid monosodium salt, which specifically adopts phthalic anhydride, sodium hydroxide and chlorine to produce 4-chlorophthalic acid monosodium salt; the above preparation Method 4 - Low conversion of chlorophthalic acid monosodium salt

Method used

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preparation example Construction

[0022] The invention provides a preparation method of 4-chlorophthalic acid monosodium salt, comprising the following steps:

[0023] Phthalic anhydride, sodium hydroxide, polar solvent and tetrabutylammonium chloride are mixed, and chlorine gas is introduced into the obtained reaction feed liquid to carry out chlorination reaction to obtain the 4-chlorophthalic acid monohydrate. sodium salt.

[0024] In the present invention, in parts by weight, the parts by weight of the phthalic anhydride are preferably 70-120 parts, more preferably 80-110 parts, and more preferably 90-100 parts.

[0025] Based on the parts by weight of phthalic anhydride, the parts by weight of the sodium hydroxide are preferably 30 to 60 parts, more preferably 35 to 55 parts, more preferably 40 to 50 parts, and most preferably 45 parts .

[0026] Based on the weight parts of phthalic anhydride, the weight parts of the polar solvent is preferably 200-500 parts, more preferably 300-500 parts, and more pre...

Embodiment 1

[0048] Preparation materials: water, solid sodium hydroxide, phthalic anhydride, chlorine gas (liquid chlorine), tetrabutylammonium chloride, 1,4-dioxane and 30 wt% hydrochloric acid.

[0049] Formula: Phthalic anhydride: 100g, sodium hydroxide: 45g, water: 200g, 1,4-dioxane: 170g, tetrabutylammonium chloride: 7.5g, chlorine gas (liquid chlorine): 72g, 30wt % Hydrochloric acid: 362 g.

[0050] Preparation:

[0051] Put the formula amount of raw water and 1,4-dioxane into a 1000mL three-necked round-bottomed flask, turn on the stirring device, add solid sodium hydroxide, tetrabutylammonium chloride, and add the Phthalic anhydride, after being completely dissolved, pass chlorine gas 72g at 0.11L / min, keep the temperature at 44°C, and use 35wt% NaOH solution to adjust the pH to 5 during the reaction process. Liquid chromatograph measures 4-chlorophthalic acid monosodium salt), after the reaction, the cooling water is cooled to 25 ° C, and the pH is adjusted to be about 5.0 and ...

Embodiment 2

[0054] Preparation materials: water, solid sodium hydroxide, phthalic anhydride, chlorine gas (liquid chlorine), tetrabutylammonium chloride, 1,4-dioxane and 30 wt% hydrochloric acid.

[0055] Formulation: Phthalic Anhydride: 120g, Sodium Hydroxide: 54g, Water: 240g, 1,4-Dioxane: 204g, Tetrabutylammonium Chloride: 9g, Chlorine (Liquid Chlorine): 86g, 30wt% Hydrochloric acid: 428.5 g.

[0056] Preparation:

[0057] Put the formula amount of raw water and 1,4-dioxane into a 1000mL three-necked round-bottomed flask, turn on the stirring device, add solid sodium hydroxide, tetrabutylammonium chloride, and add the Phthalic anhydride, after being completely dissolved, pass chlorine 86g at 0.13L / min, keep the temperature at 44°C, and use 35wt% NaOH solution to adjust the pH to 5 during the reaction process. Liquid chromatograph measures 4-chlorophthalic acid monosodium salt), after the reaction, the cooling water is cooled to 25 ° C, and the pH is adjusted to be about 5.0 and centr...

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Abstract

The invention belongs to the technical field of organic synthesis, and provides a preparation method of 4-chlorophthalic acid monosodium salt and 4-chlorophthalic anhydride. The preparation method of the 4-chlorophthalic acid monosodium salt provided by the invention comprises the following steps: mixing phthalic anhydride, sodium hydroxide, a polar solvent and tetrabutylammonium chloride, and introducing chlorine into the obtained reaction feed liquid for chlorination reaction to obtain the 4-chlorophthalic acid monosodium salt. According to the preparation method provided by the invention, tetrabutylammonium chloride is used as a phase transfer catalyst, so that the conversion rate of the 4-chlorophthalic acid monosodium salt is increased; meanwhile, a large amount of 3-chloro phthalic acid monosodium salt and dichloro compounds are prevented from being generated in the chlorination reaction process, the subsequent purification and refining process is reduced, then generation of acid wastewater is greatly reduced, and the environmental protection requirement is met. The data of the embodiment shows that the conversion rate of the 4-chlorophthalic acid monosodium salt is 92.1 to 96.5 percent.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of 4-chlorophthalic acid monosodium salt and 4-chlorophthalic anhydride. Background technique [0002] At present, polyimide is a new generation of high-performance film materials in the world. It is mainly used in flexible displays, aerospace and other fields that require high dimensional stability, high insulation, high durability and high and low temperature resistance. 4-Chlorophthalic anhydride is a very important basic raw material in the synthesis of polyimide raw materials. The Chinese patent with publication number CN1824638A discloses a production method of 4-chlorophthalic acid monosodium salt, and specifically adopts phthalic anhydride, sodium hydroxide and chlorine to produce 4-chlorophthalic acid monosodium salt; the above preparation The conversion rate of the method 4-chlorophthalic acid monosodium salt is low. SUMMARY OF THE INVE...

Claims

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Application Information

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IPC IPC(8): C07C51/363C07C63/68C07D307/89
CPCC07C51/363C07D307/89C07C51/412C07C63/20C07C63/68
Inventor 张云堂王益民张健李文革王飞扬于玉秀
Owner HEBEI HAILI FRAGRANCES CO LTD
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