Method for preparing dichlorohydrin by glycerol hydrochlorination

A technology of dichloropropanol and hydrochlorination, applied in the direction of introducing halogen preparation, organic chemistry, etc., can solve the problems of high process energy consumption, difficult scale-up production, low utilization rate of equipment, etc., and achieve simple operation control and easy scale-up production , The effect of small investment in equipment

Active Publication Date: 2008-12-17
SHANGHAI CHLOR ALKALI CHEM
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Problems solved by technology

In addition, a non-volatile catalyst is used, so the amount of catalyst is small, but this process has high energy consumption and low equipment utilization
[0018] The method introduced in patent CN101182283A is to add glycerin and catalyst together into the jet reactor, and the liquid phase circulation pump will extract the glycerin and catalyst from the jet reactor, and then enter the jet reactor from the top of the jet reactor in a jet mode, from The hydrogen chloride gas sucked into the side of the jet reactor fully reacts with the liquid phase material in the reactor, and at the same time, the negative pressure generated by the jet will take out the water, di

Method used

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  • Method for preparing dichlorohydrin by glycerol hydrochlorination
  • Method for preparing dichlorohydrin by glycerol hydrochlorination
  • Method for preparing dichlorohydrin by glycerol hydrochlorination

Examples

Experimental program
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Effect test

Embodiment 1

[0044] use figure 1 The process uses 3 stirred reactors.

[0045] The process conditions and operation process are as follows:

[0046] The gas containing hydrogen chloride is produced by the cracking of dichloroethane, and the weight content is 99.5%;

[0047] Catalyst is propionic acid, and consumption is 5% of glycerol weight;

[0048] Propionic acid and glycerol (98% secondary product) are mixed in the storage tank 1, and pumped into the absorption reaction tower shown at a rate of 6.0kg / h through the metering pump 2, and at the same time, the gas containing hydrogen chloride is sent into the absorption reaction tower from the bottom. Reaction tower 3, the flow rate is 0.5m 3 / h;

[0049] The material part at the bottom of the absorption reaction tower 3 is sent back to the top of the absorption reaction tower 3 through the liquid phase circulation pump 4, and the part is divided into the first stirred tank 8;

[0050]Then the reaction solution enters the second stirr...

Embodiment 2

[0057] use figure 1 The process uses 3 stirred reactors.

[0058] The process conditions are as follows:

[0059] Catalyst is propionic acid, and consumption is 5% of glycerol weight;

[0060] The gas containing hydrogen chloride is produced by the cracking of dichloroethane, and the weight content is 99.5%;

[0061] After the catalyst and glycerin (98% industrial product) are mixed in the storage tank 1, they are pumped into the absorption reaction tower shown at a rate of 10.0kg / h through the metering pump 2, and at the same time, the gas containing hydrogen chloride is sent into the absorption reaction tower from the bottom 3. The flow rate is 1.1m 3 / h;

[0062] The weight ratio of the material sent back to the top of the absorption reaction tower 3 to the first stirred tank 8 is 100:1;

[0063] The temperatures of the absorption reaction tower 3 and the stirred tank are respectively controlled at 90°C, 105°C, 110°C and 110°C;

[0064] The residence time of the react...

Embodiment 3

[0068] use figure 1 The process uses 3 stirred reactors.

[0069] The process conditions are as follows:

[0070] Catalyst is adipic acid, and consumption is 10% of glycerin weight;

[0071] The gas containing hydrogen chloride is hydrogen chloride gas;

[0072] After the catalyst and glycerin are mixed in the storage tank 1, they are pumped into the absorption reaction tower shown by the metering pump 2 at a rate of 6.0kg / h. At the same time, the gas containing hydrogen chloride is sent into the absorption reaction tower 3 from the bottom with a flow rate of 0.4m 3 / h;

[0073] The weight ratio of the material sent back to the top of the absorption reaction tower 3 to the first stirred tank 8 is 150:1;

[0074] The temperatures of the absorption reaction tower 3 and the stirred tank are respectively controlled at 90°C, 90°C, 110°C and 130°C;

[0075] Other conditions are the same as example 1. After the reaction is stable, the weight flow rate and component content of th...

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Abstract

The invention provides a method for preparing dichloropropanol from glycerol through hydrochlorination, which comprises the steps as follows: (1) the mixing raw material liquid of activator and the glycerol is poured into an absorption reaction tower from the top thereof, hydrogen chloride is put into the absorption reaction tower from the bottom thereof, the materials at the bottom of the absorption reaction tower are partially sent back to the absorption reaction tower and parts are put into the first stirring vessel of n stirring vessels; (2) the hydrogen chloride is let into the first stirring vessel for carrying out reaction and then reaction solution enters into the second stirring vessel of the n stirring vessels to react with the hydrogen chloride, and the reaction solution reacts with the hydrogen chloride in the n stirring vessels in turn according to the process; (3) the condensate of the gaseous phase mixtures braised out from the tops of the stirring vessels are gaseous phase products and the mother liquor comes out from the nth stirring vessel is aqueous phase product. The method of the invention is low in investment on equipment, simple in operation and control and high in reaction speed, thus being easy for expanding production with the yield of dichloropropanol per pass higher than 90 percent and the use ratio of the hydrogen chloride higher than 70 percent.

Description

technical field [0001] The present invention relates to a process for the preparation of dichloropropanol. Background technique [0002] At present, the industrial production methods of dichloropropanol mainly use propylene as a raw material for propylene high-temperature chlorination and propylene acetate method. [0003] Among them, more than 90% of dichloropropanol intermediates in the world are produced by high-temperature chlorination of propylene. The process mainly includes two reaction units: high-temperature chlorination of propylene to produce allyl chloride, and hypochlorination of allyl chloride to synthesize dichloropropanol. The reaction formula is: [0004] [0005] The process method is characterized by flexible production process, mature process, stable operation, and can also produce various organic synthesis intermediates. However, there are shortcomings such as serious equipment corrosion, high energy consumption, high chlorine consumption, many by-p...

Claims

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Application Information

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IPC IPC(8): C07C29/62C07C31/42C07C31/36
Inventor 马斌全陈斌武岳群袁茂全胡妹华
Owner SHANGHAI CHLOR ALKALI CHEM
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