Method for preparing dichloropropanol

A technology of dichloropropanol and chloropropene, which is applied in the direction of chemical instruments and methods, the introduction of hydroxyl and halogen preparation, molecular sieve catalysts, etc., can solve the problems of intensified side reactions, large wastewater discharge, and serious equipment corrosion. Simple, safe and efficient process, mild reaction conditions

Active Publication Date: 2018-04-24
CHINA PETROLEUM & CHEM CORP +1
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  • Description
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Problems solved by technology

The raw materials of this method are easy to get, the reaction conditions are mild, and allyl chloride and hypochlorous acid can be mixed to react. The process is simple and efficient. However, the use of chlorine in the reaction process has brought some adverse effects to the method.
First of all, the equipment corrosion caused by the raw material chlorine is serious, and the requirements for the material and operation safety of the reactor are relatively high.
Secondly, chlorine gas dissolves in water to generate equal amounts of hypochlorous acid and hydrochloric acid, only hypochlorous acid is an effective reactant, and the effective utilization rate of chlorine gas is low
In addition, chlorine gas directly reacts with chloropropene to generate a certain amount of low-value by-products such as trichloropropane, and the existence of trichloropropane phase leads to intensified side reactions. In order to reduce the formation of by-products, it is usually necessary to add a large amount of water to dissolve to avoid Phase separation leads to the concentration of the product dichloropropanol solution being only about 4%, the subsequent separation process of the product is difficult, the energy consumption is high, and the waste water discharge is large

Method used

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  • Method for preparing dichloropropanol
  • Method for preparing dichloropropanol
  • Method for preparing dichloropropanol

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preparation example Construction

[0035] The preparation method of the TS-1 molecular sieve adopted in the embodiment is: add about 3 / 4 amount of tetrapropylammonium hydroxide (TPAOH, 20%, purchased from American Aldrich Company) solution to tetraethyl orthosilicate (TEOS) solution, obtain a liquid mixture with a pH of about 13, and then add a required amount of n-butyl titanate [Ti(OBu) dropwise to the obtained liquid mixture under vigorous stirring. 4 ] in anhydrous isopropanol solution, and after stirring for 15 minutes, a clear liquid was obtained. Finally, the remaining TPAOH was slowly added to the clear liquid, and stirred at 348-353K for about 3 hours to obtain a chemical composition of 0.03TiO 2 : SiO 2 :0.36TPA:35H 2 The sol of O was then crystallized at 443K for 3 days, and then the obtained solid was filtered, washed with distilled water, dried at 373K for 5 hours, and then calcined at 823K for 10 hours to obtain a molecular sieve sample. Wherein, the consumption of TEOS is 42g, the consumption o...

Embodiment 1

[0045] Allyl chloride, 30 mass % hydrogen peroxide aqueous solution, 37 mass % hydrochloric acid and required amount of water are put into the reactor to obtain the chloropropene, hydrogen peroxide, hydrogen chloride and water in a molar ratio of 1: 1.5: 1.5: 20 of the reaction mixture, put TS-1 molecular sieve into the reaction kettle, the mass ratio of TS-1 molecular sieve to chloropropene is 0.25, and then react the reaction mixture in the reaction kettle at a temperature of 20°C for 2 hours, and take a sample after the reaction is completed Analysis, analysis results are shown in Table 1.

Embodiment 2

[0047] Allyl chloride, 30 mass % hydrogen peroxide aqueous solution, 37 mass % hydrochloric acid and required amount of water are put into the reactor to obtain the chloropropene, hydrogen peroxide, hydrogen chloride and water in a molar ratio of 1: 1.5: 1.5: 20 of the reaction mixture, put the hollow titanium-silicon molecular sieve HTS into the reactor, the mass ratio of the hollow titanium-silicon molecular sieve HTS to chloropropene is 0.25, and then react the reaction mixture in the reactor at a temperature of 20°C for 2 hours, and the reaction is completed After sampling and analysis, the analysis results are shown in Table 1.

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Abstract

The invention discloses a method for preparing dichloropropanol. The method comprises the steps of performing a contact reaction on allyl chloride, hydrogen chloride and an oxidant in the presence ofa catalyst, wherein the catalyst is a titanium silicate molecular sieve catalyst. The method has the characteristics of no use of toxic chlorine, simple operation process, mild reaction conditions, high raw material conversion rate, high selectivity of dichloropropanol, and easy separation of the catalyst.

Description

technical field [0001] The invention relates to a method for preparing dichloropropanol. Background technique [0002] Dichloropropanol is a raw material for the synthesis of various chemical products such as dichloroacetone, cellulose acetate, and water treatment agents, and is also an important intermediate for the synthesis of epichlorohydrin, epoxy resin, ion exchange resin, etc., and its market demand is very high. Big. The preparation methods of dichloropropanol in the prior art mainly include the chloroalcoholization method of allyl chloride, the chlorination method of allyl alcohol and the chlorination method of glycerin and the like. Among them, the chloroalcoholization of allyl chloride was developed earlier, its process is simple and mature, and it has a large market share. [0003] The traditional method of chloroalcoholization of allyl chloride to prepare dichloropropanol firstly dissolves chlorine gas in water to generate hypochlorous acid, and then chloroalc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/64C07C31/36B01J29/89
CPCB01J29/89C07C29/64C07C31/36
Inventor 林民彭欣欣舒兴田朱斌夏长久
Owner CHINA PETROLEUM & CHEM CORP
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