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Synthesis method of ion pair reagent

The technology of an ion pair reagent and a synthesis method is applied in the field of ion pair reagent synthesis, which can solve the problems of low product purity, influence on chromatographic analysis results, and high product ultraviolet absorption signal, and achieve high purity, high yield, and improved production efficiency. Effect

Inactive Publication Date: 2020-12-29
永华化学股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The catalyst mixed in the ion-pair reagent product is difficult to completely remove even after multiple purifications. The residual catalyst will lead to low purity of the product (generally about 98.5%), resulting in high UV absorption signal of the product and affecting chromatographic analysis. result

Method used

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  • Synthesis method of ion pair reagent
  • Synthesis method of ion pair reagent
  • Synthesis method of ion pair reagent

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preparation example Construction

[0042] The invention provides a method for synthesizing an ion-pairing reagent. The ion-pairing reagent is sodium butanesulfonate, sodium pentanesulfonate, sodium hexanesulfonate, sodium heptanesulfonate, sodium octanesulfonate or decane Sodium alkanesulfonate, comprising the following steps:

[0043] (1) Under the condition of no catalyst, water, sodium sulfite and brominated alkanes are mixed for high-pressure reaction to obtain product feed liquid; the temperature of the high-pressure reaction is 180-300° C., and the pressure is 10-15 kg;

[0044] (2) directly cooling and crystallizing the product feed liquid, and performing first washing on the obtained solid to obtain a crude product;

[0045] (3) The crude product is recrystallized, and the obtained recrystallized product is sequentially subjected to second washing and drying to obtain an ion-pairing reagent.

[0046] In the present invention, under the condition of no catalyst, water, sodium sulfite and brominated alka...

Embodiment 1

[0070] (1) Add 5000g of pure water, 900g of anhydrous sodium sulfite and 1500g of 1-bromoheptane into the autoclave, heat to 200°C, keep the pressure at 13kg, and react for 6 hours.

[0071] (2) After the reaction is over, pump the product liquid into the glass crystallization tank, turn on the stirring device, control the stirring speed at 10rpm, control the crystallization temperature at 2-6°C, and the crystallization time for 3h, and pump the crystallization liquid with a suction filter bottle Dried, then centrifuged at high speed, washed 3 times with n-hexane during centrifugation, using 500mL of n-hexane each time, and collected 1560g of crude sodium heptanesulfonate.

[0072] (3) Take 1560g of the crude product and put it into a glass reactor, add 5000g of absolute ethanol and 850g of pure water, heat and stir to dissolve, the dissolution temperature is controlled between 80-100°C, after the crude product is completely dissolved, add 8g of activated carbon, and stir for 1...

Embodiment 2

[0080] (1) Add 4000g of pure water, 900g of anhydrous sodium sulfite and 1000g of 1-bromopentane into the autoclave, heat to 195°C, keep the pressure at 10kg, and react for 5 hours.

[0081] (2) After the reaction is over, pump the product liquid into the glass crystallization tank, turn on the stirring device, control the stirring speed at 10rpm, control the crystallization temperature at 2-6°C, and the crystallization time for 4h, and pump the crystallization liquid with a suction filter bottle Dry, then centrifuge at high speed to dry, wash with petroleum ether 3 times during centrifugation, use petroleum ether 500mL each time, collect 1310g of crude sodium pentanesulfonate.

[0082] (3) Take 1310g of the crude product and put it into a glass reactor, add 5000g of absolute ethanol and 850g of pure water, heat and stir to dissolve, the dissolution temperature is controlled between 80-100°C, after the crude product is completely dissolved, add 5g of activated carbon, and stir ...

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Abstract

The invention relates to the technical field of high-end reagent synthesis, and provides a synthesis method of an ion pair reagent, and the ion pair reagent is butane sodium sulfonate, pentane sodiumsulfonate, hexane sodium sulfonate, heptane sodium sulfonate, octane sodium sulfonate or decane sodium sulfonate. The method comprises the following steps: mixing water, sodium sulfite and bromoalkaneunder the condition of no catalyst, carrying out high-pressure reaction, directly cooling and crystallizing the obtained product feed liquid, carrying out first washing, recrystallizing the obtainedcrude product, and sequentially carrying out second washing and drying to obtain the ion pair reagent. According to the method provided by the invention, the sodium heptanesulfonate plasma pair reagent is synthesized under a high-pressure condition, a catalyst is not required to be used, residues of the catalyst in a product are avoided, the reaction time is short, side reactions are few, the yield is high, the purity of the obtained product is high, an absorption signal of the product in an ultraviolet band is extremely small, and a chromatographic analysis result is not influenced.

Description

technical field [0001] The invention relates to the technical field of high-end reagent synthesis, in particular to a synthesis method of ion-pair reagents. Background technique [0002] Ion-pair reagents are a class of high-end reagents that can improve the separation effect of liquid chromatography. For some samples with strong ionization ability in aqueous solution, the corresponding ion-pair reagent must be added to make the sample have a good separation effect in the chromatographic column. [0003] Sodium butanesulfonate, sodium pentanesulfonate, sodium hexanesulfonate, sodium heptanesulfonate, sodium octanesulfonate, sodium decanesulfonate are commonly used ion-pairing reagents. Good-quality ion-pair reagents have no or very small absorption signals in the ultraviolet band. If they have strong ultraviolet absorption characteristics, they will seriously interfere with the accuracy of the high-performance liquid chromatography ultraviolet absorption detector, resulting...

Claims

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Application Information

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IPC IPC(8): C07C303/32C07C309/04
CPCC07C303/32
Inventor 顾学峰戴惠明张路家
Owner 永华化学股份有限公司
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