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Preparation method of deuterated trifluoroacetic acid

A technology of deuterated trifluoroacetic acid and trifluoroacetic anhydride, which is applied in the field of preparation of deuterated trifluoroacetic acid, can solve the problems of decreased conversion rate of heavy water, difficulty in cleaning, and increased production costs of enterprises, so as to improve conversion rate and improve Purity, the effect of reducing the amount of use

Pending Publication Date: 2022-04-15
山东汉峰新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in this method, phosphorus pentoxide is used as a raw material, so that the obtained trifluoroacetic anhydride contains a large amount of pyrophosphoric acid and phosphoric acid by-products, and it is difficult to remove them through rectification.
Both pyrophosphoric acid and phosphoric acid can exchange hydrogen and deuterium with deuterium in heavy water, resulting in a decrease in the conversion rate of heavy water and increasing the production cost of the enterprise.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Preparation of dehydrating agent:

[0019] The first step is to ultrasonically disperse 100g of artificial zeolite in 1000mL of absolute ethanol, then add 30g of 3-aminopropyltrimethoxysilane, heat and reflux for 1.5h, then cool down to room temperature, perform ultrafiltration, and dry to obtain amino artificial zeolite;

[0020] The second step is to soak the amino artificial zeolite in the ammonium dihydrogen phosphate solution for 1 hour by equal volume immersion method, filter it with suction, wash it with deionized water, then dry it at 100°C, and heat it up to 500°C at a rate of 2°C / min for roasting After 4 hours, grind through a 150-mesh sieve to obtain a dehydrating agent, and the mass concentration of the ammonium dihydrogen phosphate solution is 25%.

Embodiment 2

[0022] Preparation of dehydrating agent:

[0023] The first step is to ultrasonically disperse 100g of artificial zeolite in 1500mL of absolute ethanol, then add 50g of 3-aminopropyltrimethoxysilane, heat and reflux for 2h, then lower to room temperature, perform ultrafiltration, and dry to obtain amino artificial zeolite;

[0024] The second step is to immerse the amino artificial zeolite in the ammonium dihydrogen phosphate solution for 1.5 hours by equal-volume immersion method, filter it with suction, wash it with deionized water, then dry it at 120°C, and heat it up to 550°C at a rate of 2°C / min Roasting for 4 hours, grinding through a 300-mesh sieve to obtain a dehydrating agent, the mass concentration of ammonium dihydrogen phosphate solution is 45%

Embodiment 3

[0026] A preparation method of deuterated trifluoroacetic acid, comprising the following steps:

[0027] Step 1. Add 400mL of toluene and 75g of the dehydrating agent prepared in Example 1 into a dry reactor, and stir at 600r / min for 20min, then add 150g of trifluoroacetic acid dropwise under stirring at a rate of 2 drops / second, after the dropwise addition is complete, heat up and reflux for 6 hours, then distill under normal pressure, collect the front fraction at 40-50°C, and then rectify the obtained front fraction to obtain trifluoroacetic anhydride;

[0028] Step 2. Add 0.1mol trifluoroacetic anhydride into the dry reaction kettle, pass in argon gas, and form argon bubbling, then add 0.105mol heavy water dropwise at 0±3°C, and the dropping rate is 2 drops / sec, after the dropwise addition is complete, bubble argon at 0°C for 1 hour, and then rectify to obtain deuterated trifluoroacetic acid.

[0029] The calculated conversion rate of heavy water was 98.8%.

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Abstract

The invention relates to a preparation method of deuterated trifluoroacetic acid, which belongs to the technical field of fine chemical engineering, and comprises the following steps: step 1, soaking amino artificial zeolite in an ammonium dihydrogen phosphate solution, carrying out suction filtration, washing, drying, roasting, grinding and sieving to obtain a dehydrating agent; step 2, adding a solvent and a dehydrating agent into a dry reaction kettle, stirring and mixing, then dropwise adding trifluoroacetic acid in a stirring state, after dropwise adding is completed, heating for reflux reaction, then distilling at normal pressure, collecting a front fraction at 40-50 DEG C, and rectifying the obtained front fraction to obtain trifluoroacetic anhydride; and step 3, adding trifluoroacetic anhydride into the dry reaction kettle, introducing argon gas to form argon gas bubbles, then dropwise adding weighted water at the temperature of 0 + / -3 DEG C, carrying out argon gas bubbles for 1-1.5 hours after dropwise adding is completed, and then carrying out rectification to obtain the deuterated trifluoroacetic acid. By adopting the dehydration effect of the dehydrating agent, the purity of trifluoroacetic anhydride is improved, and the conversion rate of heavy water is improved.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a preparation method of deuterated trifluoroacetic acid. Background technique [0002] Deuterated trifluoroacetic acid is one of the deuterated reagents. It is often used as a detection reagent for nuclear magnetic detection of polymers. Its role: to increase the solubility of the analyte; to exchange hydrogen and deuterium with hydrogen in the system to be tested to eliminate active The NMR peak of hydrogen; destroys the hydrogen bond in the system to be tested. The preparation of deuterated trifluoroacetic acid is first made into trifluoroacetic anhydride, and then obtained by hydrolysis of trifluoroacetic anhydride and heavy water. Among them, the way to obtain trifluoroacetic anhydride has the following methods: trifluoroacetyl chloride reacts with sodium trifluoroacetate; 2,2-dichloroacetic anhydride is used as a dehydrating agent to dehydrate trifluoroac...

Claims

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Application Information

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IPC IPC(8): C07C53/18C07C51/087C07C51/56C07C51/44C07B59/00
Inventor 林崇熙张坤王化建殷浩战垒刘锦辉
Owner 山东汉峰新材料科技有限公司
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