High-content potassium isooctanoate composition and preparation method thereof

Abstract

The invention discloses a high-content potassium isooctanoate composition. In the composition, the content of potassium isooctanoate is not less than 99 percent and the water content is not higher than 1 percent. After being accelerated for 6 months, the composition still can keep a solid state, unchanged color, stability and prolonged shelf life. The invention also discloses a preparation method of the composition; the potassium isooctanoate and potassium hydroxide are selected as raw materials, and purified water or alcohols and esters are selected as solvents; the preparation method has the technical characteristics that after neutralization reaction, a decolorising agent subjected to extraction and special treatment is used for decolorizing, purification refinement and spray drying are carried out to obtain the composition; the quality of a product fully meets standard requirements of medicinal raw materials.

Description

technical field

[0001] The invention belongs to the technical field of medicine, and in particular relates to a high-content potassium isooctanoate composition and a preparation method thereof. Background technique

[0002] Potassium isooctanoate, the chemical name is potassium 2-ethylhexanoate, light yellow viscous liquid or solid, easy to absorb moisture, mainly used in the synthesis of salt-forming agent of cephalosporin antibiotic potassium clavulanate, and heat stabilizer of plastic products, Catalyst for polymerization reaction, crosslinking agent for polymer materials, etc. Potassium isooctanoate is an upgraded product of potassium naphthenate. The main raw material for its synthesis, isooctanoic acid, is an isomeric acid of carboxylic acids, which is weakly acidic and easily forms chelates with most metal ions. Isooctanoate is suitable for all applications of naphthenates, and its performance is significantly higher than that of similar naphthenates. The product h...

Examples

Embodiment 1

[0037] a. Put 13g of potassium hydroxide (content ≥ 90.0%) into 15ml of water, and prepare a solution for later use.

[0038] b. Add 32g of isooctanoic acid (content ≥ 99.0%) into the reaction flask, add the above solution a into the isooctanoic acid dropwise within 10-20 minutes, the pH value is 9-12, and gradually raise the temperature to 60°C. The reaction was incubated for 3 hours.

[0039] c. Add 3ml of n-butanol and 12ml of ethyl acetate to the reacted b solution, stir and extract for 30 minutes, then separate the phases, and take the heavy phase.

[0040] d. Add 0.5 g of serine protease to the heavy phase c solution and incubate for 30 minutes for decolorization.

[0041] e. After filtering the material d, send it to a spray dryer for drying.

[0042] f. Obtain 37.1 g of finished product (content ≥ 99.0%, moisture ≤ 0.6%), the appearance is white.

[0043] Potassium isooctanoate crude drug product testing results are as follows:

[0044] character content...

Embodiment 2

[0046] a. Put 13g of potassium hydroxide (content ≥ 90.0%) into 15ml of water, and prepare a solution for later use.

[0047] b. Add 32g of isooctanoic acid (content ≥ 99.0%) into the reaction flask, add the above solution a into the isooctanoic acid dropwise within 10 to 20 minutes, the pH value is 9 to 12, and gradually heat up to 60°C. The reaction was incubated for 3 hours.

[0048] c. Add 3ml of n-butanol and 15ml of ethyl acetate to the reacted b solution, stir and extract for 30 minutes, then separate the phases, and take the heavy phase.

[0049] d. Add 0.3 g of serine protease to the heavy phase c solution and incubate for 30 minutes for decolorization.

[0050] e. After filtering the material d, send it to a spray dryer for drying.

[0051] f. Obtain 37.1 g of finished product (content ≥ 99.0%, moisture ≤ 0.6%), the appearance is white.

[0052] Potassium isooctanoate crude drug product testing results are as follows:

[0053] character content moist...

Embodiment 3

[0055] a. Put 13g of potassium hydroxide (content ≥ 90.0%) into 15ml of water, and prepare a solution for later use.

[0056] b. Add 32g of isooctanoic acid (content ≥ 99.0%) into the reaction flask, add the above solution a into the isooctanoic acid dropwise within 10-20 minutes, the pH value is 9-12, and gradually raise the temperature to 60°C. The reaction was incubated for 3 hours.

[0057] c. Add 3ml of n-butanol and 9ml of ethyl acetate to the reacted b solution, stir and extract for 30 minutes, then separate the phases, and take the heavy phase.

[0058] d. Add 1.0 g of serine protease to the heavy phase c solution and incubate for 30 minutes for decolorization.

[0059] e. After filtering the material d, send it to a spray dryer for drying.

[0060] f. Obtain 37.1 g of finished product (content ≥ 99.0%, moisture ≤ 0.6%), the appearance is white.

[0061] Potassium isooctanoate bulk drug product testing results are as follows:

[0062] character content m...

technical field

[0001] The invention belongs to the technical field of medicine, and in particular relates to a high-content potassium isooctanoate composition and a preparation method thereof. Background technique

[0002] Potassium isooctanoate, the chemical name is potassium 2-ethylhexanoate, light yellow viscous liquid or solid, easy to absorb moisture, mainly used in the synthesis of salt-forming agent of cephalosporin antibiotic potassium clavulanate, and heat stabilizer of plastic products, Catalyst for polymerization reaction, crosslinking agent for polymer materials, etc. Potassium isooctanoate is an upgraded product of potassium naphthenate. The main raw material for its synthesis, isooctanoic acid, is an isomeric acid of carboxylic acids, which is weakly acidic and easily forms chelates with most metal ions. Isooctanoate is suitable for all applications of naphthenates, and its performance is significantly higher than that of similar naphthenates. The product h...

Examples

Embodiment 1

[0037] a. Put 13g of potassium hydroxide (content ≥ 90.0%) into 15ml of water, and prepare a solution for later use.

[0038] b. Add 32g of isooctanoic acid (content ≥ 99.0%) into the reaction flask, add the above solution a into the isooctanoic acid dropwise within 10-20 minutes, the pH value is 9-12, and gradually raise the temperature to 60°C. The reaction was incubated for 3 hours.

[0039] c. Add 3ml of n-butanol and 12ml of ethyl acetate to the reacted b solution, stir and extract for 30 minutes, then separate the phases, and take the heavy phase.

[0040] d. Add 0.5 g of serine protease to the heavy phase c solution and incubate for 30 minutes for decolorization.

[0041] e. After filtering the material d, send it to a spray dryer for drying.

[0042] f. Obtain 37.1 g of finished product (content ≥ 99.0%, moisture ≤ 0.6%), the appearance is white.

[0043] Potassium isooctanoate crude drug product testing results are as follows:

[0044] character content...

Embodiment 2

[0046] a. Put 13g of potassium hydroxide (content ≥ 90.0%) into 15ml of water, and prepare a solution for later use.

[0047] b. Add 32g of isooctanoic acid (content ≥ 99.0%) into the reaction flask, add the above solution a into the isooctanoic acid dropwise within 10 to 20 minutes, the pH value is 9 to 12, and gradually heat up to 60°C. The reaction was incubated for 3 hours.

[0048] c. Add 3ml of n-butanol and 15ml of ethyl acetate to the reacted b solution, stir and extract for 30 minutes, then separate the phases, and take the heavy phase.

[0049] d. Add 0.3 g of serine protease to the heavy phase c solution and incubate for 30 minutes for decolorization.

[0050] e. After filtering the material d, send it to a spray dryer for drying.

[0051] f. Obtain 37.1 g of finished product (content ≥ 99.0%, moisture ≤ 0.6%), the appearance is white.

[0052] Potassium isooctanoate crude drug product testing results are as follows:

[0053] character content moist...

Embodiment 3

[0055] a. Put 13g of potassium hydroxide (content ≥ 90.0%) into 15ml of water, and prepare a solution for later use.

[0056] b. Add 32g of isooctanoic acid (content ≥ 99.0%) into the reaction flask, add the above solution a into the isooctanoic acid dropwise within 10-20 minutes, the pH value is 9-12, and gradually raise the temperature to 60°C. The reaction was incubated for 3 hours.

[0057] c. Add 3ml of n-butanol and 9ml of ethyl acetate to the reacted b solution, stir and extract for 30 minutes, then separate the phases, and take the heavy phase.

[0058] d. Add 1.0 g of serine protease to the heavy phase c solution and incubate for 30 minutes for decolorization.

[0059] e. After filtering the material d, send it to a spray dryer for drying.

[0060] f. Obtain 37.1 g of finished product (content ≥ 99.0%, moisture ≤ 0.6%), the appearance is white.

[0061] Potassium isooctanoate bulk drug product testing results are as follows:

[0062] character content m...

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