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Method for synthesizing ferrous stearate

A technology of iron stearate and synthesis method, applied in directions such as carboxylate preparation, organic chemistry, etc., can solve problems such as low yield and yield, influence product yield and quality, etc., and achieve high conversion rate and product yield. High, good product purity

Inactive Publication Date: 2008-06-04
TIANJIN UNIVERSITY OF TECHNOLOGY
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

When this product measures melting point, 70-71 ℃ (stearic acid fusing point) just begins to partially melt, and productive rate and yield are all low
[0005] In addition, it is reported in the literature that when the metathesis reaction of sodium stearate is carried out, a temperature of 90 ° C is used, and the iron stearate generated at this temperature is in a molten state, and the molten iron stearate does not form precipitates and sink into the solution The bottom floats on the liquid surface, which prevents the addition of the iron salt solution and forms a package on the iron salt, seriously affecting the yield and quality of the product

Method used

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Examples

Experimental program
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Effect test

preparation example Construction

[0019] (1) Preparation of sodium stearate solution:

[0020] Sodium hydroxide is used to form an aqueous solution with a concentration of 0.5%-3% (W / W), but preferably an aqueous solution with a concentration of 0.5%-1.5% (W / W). Heat to 90-95°C, slowly add stearic acid while stirring. Measure the pH value of the reaction solution at any time. When the pH of the reaction solution reaches 9-10, stop adding stearic acid, and continue to stir and react for 20-25 minutes. Retest the pH value of the reaction solution. If the pH value is greater than 10, add stearic acid to continue the reaction; if the pH value is less than 9, add sodium hydroxide solution to continue the reaction; if the pH value is between 9 and 10 , then the reaction solution is qualified and can be discharged.

[0021] (2) preparation of iron stearate:

[0022] Make the soluble iron salt solution into an aqueous solution with a concentration of 1%-10% (W / W), but it is best to prepare an aqueous solution with ...

Embodiment 1

[0023] Embodiment 1: the synthesis of iron stearate

[0024] Stearic acid is analytically pure or an industrial product, and sodium hydroxide, ferric chloride, ferric sulfate, and ferric nitrate are all analytically pure. Sodium hydroxide was formulated into a 1.0% (W / W) solution with distilled water, heated to 95°C, and stearic acid was added under stirring. Measure the pH value of the reaction solution at any time. When the pH of the reaction solution is 9 to 10, stop adding stearic acid and continue stirring for 20 minutes to obtain a clear and transparent sodium stearate solution. Retest the pH value of the reaction solution, and it is still between 9 and 10.

[0025] Ferric trichloride was made into a solution with a concentration of 3% (W / W) with distilled water, and was preheated to 50° C. for later use. Cool the sodium stearate solution to 80°C, slowly add the ferric chloride solution dropwise with stirring, and an orange-yellow ferric stearate precipitate is formed ...

Embodiment 2

[0026] Embodiment 2: the synthesis of iron stearate

[0027] Sodium hydroxide is made into a 1.0% (W / W) solution with distilled water, heated to 90° C., and stearic acid is added under stirring. When the pH of the reaction solution is 9 to 10, the addition of stearic acid is stopped. Continue to stir and react for 25 minutes to obtain a clear transparent sodium stearate solution. Retest the pH of the reaction solution to be 10, add stearic acid to make the pH between 9-10, and continue to stir and react for 20 minutes. Retest the pH value of the reaction solution between 9 and 10, and the reaction ends.

[0028] Ferric trichloride was prepared into a solution with a concentration of 3% (w / w) with distilled water, and was preheated to 55° C. for later use. Cool the sodium stearate solution to 75°C, slowly add the ferric chloride solution dropwise with stirring, and an orange-yellow ferric stearate precipitate is formed immediately. When the pH of the reaction solution is 3 to...

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Abstract

This invention discloses a synthesis method for a ferrous stearate. Based on the method stearic acid was added into o.5% - 3% of sodium hydroxide solution, when pH value of the reaction solution reaches 9-10, sodium stearate solution was formed, cooling it down to 60-80 DEG C, 1%-10% and 50-70 DEG C of soluble ferrous salt solution was added in, orange ferrous stearate deposit formed; at last after filtration, wash with water and dry, ferrous stearate powder was produced. This invention improves synthesis technique of saponification-double decomposition method for synthesizing ferrous stearate, during the stage of saponification stearic acid can be converted totally, there is no stearic acid in the product; ferrous stearate formed during the double decomposition stage is separated out in the form of deposit, the operation of washing it with water is very convenient. The produced ferrous stearate has high purity, narrow melting point range, near theoretical iron content, yield 93.8%-95.1%.

Description

【Technical field】 [0001] The invention belongs to the technical field of organic compound synthesis, and in particular relates to a new method for synthesizing plastic photosensitizer iron stearate. 【Background technique】 [0002] Iron stearate is a plastic photosensitizer, which has the advantages of low toxicity, low cost, and obvious photosensitization effect, so it has been widely used in the research of degradable plastics. There are few reports on the physical and chemical properties and preparation methods of iron stearate. The synthesis of ferric stearate has two kinds of direct synthesis method and saponification-metathesis synthesis method. The direct synthesis method adopts soluble iron salt (ferric chloride, ferric sulfate, ferric nitrate) and stearic acid as reaction raw materials, and the process route is relatively simple. , but because stearic acid is insoluble in water, and soluble iron salt solution is a kind of aqueous solution, needs to add organic solve...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/41C07C53/126
Inventor 周学永董庆杰邵仕香
Owner TIANJIN UNIVERSITY OF TECHNOLOGY
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