Method for preparing dichloropropanol

A technology of dichloropropanol and chloropropene, applied in chemical instruments and methods, catalyst activation/preparation, introduction of hydroxyl and halogen preparation, etc., can solve the problems of intensified side reactions, large waste water discharge, high energy consumption, etc., and achieve the goal of reaction The effect of mild conditions, safe and efficient process, and high conversion rate of raw materials

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

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

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preparation example Construction

[0046] The preparation method of the TS-2 molecular sieve adopted in the embodiment is as follows: a certain amount of tetrabutylammonium hydroxide solution (TBAOH, 20%) is mixed with ethyl orthosilicate (TEOS), and then added to the obtained solution under vigorous stirring conditions. Add the required amount of n-butyl titanate [Ti(OBu) 4 ] in anhydrous isopropanol, stirred for 30 minutes to obtain a clear liquid after the hydrolysis was completed. Finally, 2 times the required amount of distilled water was added, and the resulting sol was stirred at 348-353 K for 2 h to remove the 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. The obtained crystallized product was filtered, washed with water, dried at 373K for 6h, and then calcined at 823K for 16h to obtain a molecular sieve sample. Among them, the amount of TEOS is 42g, the amount of TBAOH is 52g, Ti(OBu) 4 The dosage of 2g ...

Embodiment 1

[0054] The TS-1 molecular sieve was added to the mixed aqueous solution containing hydrochloric acid and hydrogen peroxide, and the activation treatment was carried out under stirring. In the mixed aqueous solution, hydrochloric acid (as HCl): hydrogen peroxide: water: TS-1 molecular sieve (as silica The molar ratio of TS-1 molecular sieve was 0.02:0.1:16:1, the treatment temperature was 30°C, and the treatment time was 20h, and then the activated TS-1 molecular sieve was recovered.

[0055] The chloropropene, 30 mass % aqueous hydrogen peroxide solution, 37 mass % hydrochloric acid and required water are put into the reactor, and the mol ratio that obtains propene chloride, hydrogen chloride, hydrogen peroxide and water is 1: 0.2: 0.2: 5 reaction mixture, put the above-mentioned activated TS-1 molecular sieve into the reaction kettle, so that the weight ratio of TS-1 molecular sieve and chloropropene is 0.1, then the reaction mixture in the reaction kettle is heated to 70 ℃ an...

Embodiment 2

[0057] The hollow titanium silicon molecular sieve HTS is added to the mixed aqueous solution containing hydrochloric acid and hydrogen peroxide, and the activation treatment is carried out under stirring. In the mixed aqueous solution, hydrochloric acid (as HCl): hydrogen peroxide: water: hollow titanium silicon molecular sieve HTS (as two The molar ratio of silicon oxide) is 0.02:0.1:16:1, the treatment temperature is 30°C, and the treatment time is 20h, and then the activated hollow titanium-silicon molecular sieve HTS is recovered.

[0058]The chloropropene, 30 mass % aqueous hydrogen peroxide solution, 37 mass % hydrochloric acid and required water are put into the reactor, and the mol ratio that obtains propene chloride, hydrogen chloride, hydrogen peroxide and water is 1: 0.2: 0.2: 5 reaction mixture, put the above activated hollow titanium-silicon molecular sieve HTS into the reaction kettle, so that the weight ratio of the hollow titanium-silicon molecular sieve HTS to...

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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 contains a titanium silicate molecular sieve subjected to activation treatment and the activation treatment comprises the step of contacting a titanium silicate molecular sieve with an aqueous solution containing an acid and a selectable peroxide. 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 present 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, water treatment agent, etc. It is also an important intermediate for the synthesis of epichlorohydrin, epoxy resin, ion exchange resin and other substances, and its market demand is very high. big. The preparation methods of dichloropropanol in the prior art mainly include chloropropene chlorohydrin method, allyl alcohol chlorination method, glycerol chlorination method and the like. Among them, the chloropropene chlorohydrin method developed earlier, its technological process is simple and mature, and has a large market share. [0003] To prepare dichloropropanol by the traditional chloropropene chlorohydrin method, firstly, chlorine gas is dissolved in water to generate hypochlorous acid, and then hypochlorous acid and chl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/64C07C31/36B01J29/89B01J37/00
CPCB01J29/89B01J37/00C07C29/64C07C31/36
Inventor 彭欣欣舒兴田林民朱斌夏长久
Owner CHINA PETROLEUM & CHEM CORP
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