Preparation method of dichloro propanol from glycerin

A technology of dichloropropanol and glycerol, which is applied in the chemical industry, can solve the problems of low reaction efficiency, low equipment utilization rate, easy coke formation, etc., and achieves the effects of reducing energy consumption, improving equipment utilization rate, and improving reaction rate.

Active Publication Date: 2007-08-01
溧阳常大技术转移中心有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Such a process has a mature process and sufficient sources of raw material propylene, which can meet the huge market demand, but this process route also has serious disadvantages: ①High temperature chlorination, high energy consumption, and many side reactions; ②The reaction process is prone to coking, The equipment needs to be shut down frequently to clean the coke; ③The utilization rate of chlorine gas in the reaction process is only about 38%, and the concentration of the product dichloropropanol is generally controlled at 4%, so a very large amount o

Method used

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  • Preparation method of dichloro propanol from glycerin
  • Preparation method of dichloro propanol from glycerin
  • Preparation method of dichloro propanol from glycerin

Examples

Experimental program
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Example

[0038] Example 1. Combine glycerol (95% industrial product) with 0.6mol / h (containing 2% acetic acid as a catalyst) and HCl (from PCl 3 With H 2 O is produced in a reaction of 1:3.5) at 0.6 mol / h. The pre-mixing pump is used to pump into the reaction system shown in Figure 1. The temperature of the oil bath of the tubular reactor is 105°C and is adjusted by the outlet flow regulating valve 5 so that the residence time of the material in the tubular reactor is 6h. The gas chromatography analysis of sampling valve 4 shows that the conversion rate of glycerol is 93.6%, the generation rate of monochloropropanediol is 84.4%, and the generation rate of dichloropropanol is 8.9%. The acid concentration of the reaction solution was calibrated by NaOH to 0.49mol / L.

[0039] The reaction liquid flowing out of the tubular reactor directly enters the HCl bubble column reactor, the reaction temperature is controlled at 108°C, the HCl input amount is 1.2 mol / h, and the flow rate of the outlet va...

Example

[0041] Example 2. Change the residence time of the material in the bubbling reactor. Industrial glycerol (95%) is pumped into the reaction system shown in Figure 1 through premixing at 0.6 mol / h (with 2% acetic acid as catalyst) and HCl at 0.6 mol / h. The oil bath of the tubular reactor The temperature is 100°C, and the outlet pressure and flow are adjusted. The residence time of the material in the tubular reactor is 6h.

[0042] Control the temperature of the bubbling reactor at 110℃, adjust the outlet flow, make the residence time of the material in the bubbling reactor 7h, and the HCl feed rate is 0.8mol / h, and the azeotrope produced will be condensed with the tail gas. Liquid separation and collection.

[0043] Within 5 hours of steady-state operation, glycerol was fed 295 g (3 mol), HCl was fed 9 mol, and glycerol was completely converted. The tail gas of the bubbling reactor was condensed to obtain 198 g of condensate (containing 39.1 g of dichloropropanol, 62 g of HCl, 91.8...

Example

[0044] Example 3. Change the residence time of the material in the tubular reactor. Industrial glycerol (95%) is fed at 1.0 mol / h (including 2% acetic acid) and HCl 1.0 mol / h. The temperature of the tubular reactor is controlled at 105°C. The residence time of the material in the tubular reactor is about 3.5 hours. The conversion rate of glycerol at the outlet of the reactor is 81.6, the production rate of monochloropropanediol is 79.2, and the production rate of dichloropropanol is 2.0%. The calibrated acid value of NaOH is 1.4 mol / L.

[0045] The reaction liquid of the tubular reactor enters the HCl bubbling reactor to continue the reaction. The HCl feed rate is 2 mol / h, the temperature of the bubbling reactor is controlled at 110°C, and the residence time is 10 h.

[0046] Within 5 hours of steady-state operation, glycerol was fed with 5 mol and HCl was fed with 15 mol, and glycerol was completely converted. Condensed from the bubbling reactor tail gas to obtain 257.2g of conde...

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Abstract

The invention discloses a preparing method of dichlorohydrin from glycerol, which comprises the following steps: adding glycerol and HCl and carboxyl acid activator into mixer; charging into tubular reactor continually to proceed chlorination reaction; reacting through chlorination reaction; transforming glycerol swiftly; entering into HCl bubbling still to react continually; evaporating azeotropic material comprised by water through reaction, dichlorohydrin, HCl and part of activator from the top of bubbling still; recycling product through condensation; separating liquid of bubbling still in the fractionating tower; getting dichlorohydrin from the top of fractionating tower; delivering liquid of fractionating tower to proceed circular response.

Description

technical field [0001] The invention belongs to the field of chemical industry, and relates to a preparation method of a propylene oxide intermediate. More specifically a process for the preparation of dichloropropanol from glycerol. Background technique [0002] Dichloropropanol is a key intermediate in the production of epichlorohydrin, and its annual output is close to 2 million tons. The main method of producing dichloropropanol worldwide is based on the high-temperature chlorination of propylene developed by the American shell company in 1948. The preparation process includes: [0003] CH 2 =CHCH 3 +Cl 2 →CH 2 =CHCH 2 Cl [0004] CH 2 =CHCH 2 Cl+Cl 2 +H 2 O→CH 2 ClCH(OH)CH 2 Cl+CH 2 (OH)CHClCH 2 Cl [0005] Such a process has a mature process and sufficient sources of raw material propylene, which can meet the huge market demand, but this process route also has serious disadvantages: ①High temperature chlorination, high energy consumption, and many side ...

Claims

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Application Information

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IPC IPC(8): C07C29/62C07C29/74C07C31/42C07C31/34B01J31/04
Inventor 单玉华韩蕾蕾徐正华李明时朱建军
Owner 溧阳常大技术转移中心有限公司
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