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Preparation method for combined production of chromatographically pure isobutanol and high-purity chromatographic standard isobutanol

An isobutanol and chromatographically pure technology is applied in the field of preparation of high-purity chromatographic standard products and chromatographically pure isobutanol, which can solve the problems of high water content, low isobutanol content and high impurity content, and achieve high profits and equipment Simple, easy-to-craft effects

Inactive Publication Date: 2017-02-15
TIANJIN GUANGFU TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to provide a co-production preparation method of chromatographically pure grade isobutanol and high-purity chromatographic standard isobutanol, aiming to overcome the current shortcomings of low isobutanol content, high water content, and high impurity content, and provide A preparation method of chromatographic isobutanol with high purity and qualified transmittance, and isobutanol with content ≥ 99.9%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A kind of preparation method of high-purity chromatographic standard substance and chromatographically pure isobutanol, the steps are as follows:

[0019] (1) Add 50g of anhydrous calcium sulfate to 1 liter of industrial isobutanol, stir for 20min, and filter;

[0020] (2) Add 50g of anhydrous potassium carbonate to the filtrate, stir for 30min, and filter;

[0021] (3) Add 20 g of calcium oxide to the filtrate, stir, leave for 12 hours, and filter;

[0022] (4) Add 10 g of calcium hydride to the filtrate, stir, let stand for 12 hours, and filter;

[0023] (5) Add 10ml cyclohexane to the filtrate, rectify, collect fractions at 68-69°C, and recover cyclohexane;

[0024] (6) Continue to rectify, collect the 107°C fraction with a content of 99.96% (GC) as a chromatographic standard, and the front and rear fractions with a content of 99.5% (GC) as a chromatographic pure reagent.

Embodiment 2

[0026] A kind of preparation method of high-purity chromatographic standard substance and chromatographically pure isobutanol, the steps are as follows:

[0027] (1) Add 50g of anhydrous calcium chloride and 20g of calcium sulfate to 1 liter of industrial isobutanol, stir for 20min, and filter;

[0028] (2) Add 50g of anhydrous potassium carbonate to the filtrate, stir for 20min, and filter;

[0029] (3) Add 50 g of calcium hydride to the filtrate, stir and place for 12 hours, and filter;

[0030] (4) Filtrate rectification, add cyclohexane azeotropic dehydration, recover cyclohexane, pay attention to fraction collection and detection. When the transmission rate is qualified, start to contact the liquid, which is a chromatographic pure reagent. When the content is ≥99.96%, it is a chromatographic standard product.

Embodiment 3

[0032] A kind of preparation method of high-purity chromatographic standard substance and chromatographically pure isobutanol, the steps are as follows:

[0033] (1) 1 liter of industrial isobutanol, add 100g of calcium oxide, stir for 20min and leave overnight, filter;

[0034] (2) Add 50g of anhydrous potassium carbonate to the filtrate, stir for 20min, let stand overnight, and filter;

[0035] (3) Add 20ml cyclohexane to the filtrate, rectify, and collect different grades of products;

[0036] (4) Recycling cyclohexane, adding anhydrous calcium chloride, drying for 12 hours, and filtering to obtain AR grade cyclohexane.

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Abstract

The invention relates to a preparation method for combined production of chromatographically pure isobutanol and high-purity chromatographic standard isobutanol. The preparation method comprises the following steps: (1) adding anhydrous calcium sulfate into industrial isobutanol, carrying out stirring for 20 to 30 min and then carrying out filtering; (2) adding anhydrous potassium carbonate into a filtrate obtained in the previous step, carrying out stirring for 20 to 30 min and then carrying out filtering; (3) adding calcium oxide or calcium hydride into a filtrate obtained in the previous step, carrying out standing for 12 h and then carrying out filtering; (4) allowing a filtrate obtained in the previous step to pass through an active carbon chromatography column; and (5) subjecting chromatographic liquid to rectification. The preparation method for combined production of chromatographically pure isobutanol and high-purity chromatographic standard isobutanol has the advantages of simple process, simple equipment and easily controllable operation and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of organic chemical industry, relates to deep dehydration and purification of alcohol, and provides a high-purity chromatographic standard product and a preparation method of chromatographically pure isobutanol. Background technique [0002] Isobutanol is a colorless, flammable, organic compound with a special odor. Its isomers include n-butanol, sec-butanol, and tert-butanol. It is widely used in organic synthesis and advanced solvents, and is also an important analytical reagent and chromatographic analysis reagent. GB2760-2011 stipulates that it is allowed to use edible flavors for the manufacture of artificial musk, fruit essential oils and synthetic drugs. [0003] Isobutanol is somewhat toxic and should never be used to make agricultural plastics because it can cause crop death. Therefore, as a chromatographic reagent and a chromatographic standard for detection, it has a wide range of uses and is al...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/76C07C31/12
CPCC07C29/76C07C31/12
Inventor 杨万龙张勇
Owner TIANJIN GUANGFU TECH DEV
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