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Method for preparing 1,3-dichloro-2-propanol

A technology of propanol and chloropropene, which is applied in the field of preparing 1,3-dichloro-2-propanol, can solve the problems of many by-products and low selectivity of 1,3-dichloro-2-propanol, and achieve The operation process is simple, the separation energy consumption is low, and the process is safe and efficient.

Active Publication Date: 2018-04-24
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Generally speaking, there are more by-products in the product obtained by the above-mentioned existing methods, and the selectivity of 1,3-dichloro-2-propanol is lower

Method used

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  • Method for preparing 1,3-dichloro-2-propanol

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preparation example Construction

[0045] The preparation method of the TS-2 molecular sieve adopted in the embodiment is: a certain amount of tetrabutylammonium hydroxide solution (TBAOH, 20%) is mixed with tetrabutylammonium hydroxide solution (TBAOH, 20%) and tetraethyl orthosilicate (TEOS), then under the condition of violent stirring, to the obtained Add the required amount of n-butyl titanate [Ti(OBu) 4 ] of anhydrous isopropanol solution, stirred for 30 minutes to obtain a clear liquid after the completion of hydrolysis. Finally, 2 times the required amount of distilled water was added, and the resulting sol was stirred at 348-353K for 2 h to remove alcohol. The chemical composition of the obtained sol is 0.20TBAOH: SiO 2 : 0.03TiO 2 : 20H 2 O. The sol was crystallized at 443K for 3 days, and the obtained crystallized product was filtered, washed with water, dried at 373K for 6 hours, and then calcined at 823K for 16 hours to obtain a molecular sieve sample. Wherein, the consumption of TEOS is 42g, ...

Embodiment 1

[0052] Put chloropropene, 30 mass % hydrogen peroxide aqueous solution, 37 mass % hydrochloric acid, ethanol and the required amount of water into the reaction kettle to obtain chloropropene, hydrogen peroxide, hydrogen chloride, ethanol and water in a molar ratio of 1: 1.5: 1.5: 0.1: 30 reaction mixture, put TS-1 molecular sieve into the reaction kettle, the mass ratio of TS-1 molecular sieve to chloropropene is 0.28, and then make the reaction mixture in the reaction kettle react at a temperature of 30°C 5h, after the reaction was completed, samples were taken for analysis, and the analysis results are shown in Table 1.

Embodiment 2

[0054] Put chloropropene, 30 mass % hydrogen peroxide aqueous solution, 37 mass % hydrochloric acid, trifluoroethanol and required amount of water into the reaction kettle to obtain chloropropene, hydrogen peroxide, hydrogen chloride, trifluoroethanol and water moles Ratio is 1: 1.5: 1.5: 0.1: 30 reaction mixture, put TS-1 molecular sieve into this reactor, the mass ratio of TS-1 molecular sieve and chloropropene is 0.28, then make the reaction mixture in the reactor at 30 ℃ Under the temperature of reaction 3h, take a sample analysis after completion of reaction, analysis result is shown in Table 1.

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Abstract

The present invention discloses a method for preparing 1,3-dichloro-2-propanol. The method comprises the following steps: performing a contact reaction on allyl chloride, hydrogen chloride, an oxidantand an oxygen-containing hydrocarbon in the presence of a catalyst, wherein the oxygen-containing hydrocarbon is an alcohol and / or a carboxylic acid, and the catalyst is a titanium silicate molecularsieve catalyst. The method has the advantages of no use of toxic chlorine, simple operation process, mild reaction conditions, high selectivity of 1,3-dichloro-2-propanol, and easy separation of thecatalyst.

Description

technical field [0001] The invention relates to a method for preparing 1,3-dichloro-2-propanol. Background technique [0002] 1,3-dichloro-2-propanol is an important intermediate for the preparation of epichlorohydrin and has a large market demand. According to existing knowledge, 1,3-dichloro-2-propanol can be obtained by chlorohydrination of allyl chloride, chlorination of allyl alcohol, and chlorination of glycerin. [0003] Taking the chlorohydrin method as an example, the chloroalcoholization of propylene chloride was developed earlier, and its process is simple and mature, and it has a relatively large market share. The method prepares dichloropropanol by mixing allyl chloride, chlorine gas and water through the chlorohydrinization reaction of hypochlorous acid. Due to the direct addition of chlorine gas and allyl chloride to generate by-products such as trichloropropane, generally speaking, the choice of dichloropropanol 1,3-dichloro-2-propanol accounted for 70%, 2,...

Claims

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Application Information

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IPC IPC(8): C07C31/36C07C29/66
CPCC07C29/66C07C31/36
Inventor 彭欣欣林民朱斌夏长久舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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