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Preparation method of dichloropropanol

A production method and a technology for dichloropropanol, which are applied in the production field of dichloropropanol, can solve the problems of short service life of catalysts, equipment corrosion, organic chloride waste water, etc., and achieve mild reaction conditions, less side reactions, and reduced sewage discharge. Effect

Active Publication Date: 2013-10-02
河北珈奥甘油化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The chlorohydrin method has a history of about 50 years, accounting for 95% of the total output of epichlorohydrin (ECH); the disadvantages of the chlorohydrin method are high chlorine consumption, high material consumption, and high energy consumption; serious equipment corrosion and high maintenance costs; products There are many by-products, and a large amount of organic chloride wastewater is produced (about 50-60m 3 waste water)
The propylene acetate method is a process developed in the 1980s, accounting for about 5% of the total ECH output. The disadvantages of the propylene acetate method are that the process flow is longer, the service life of the catalyst is short, and the equipment is corroded. Stainless steel materials are required to prevent acetic acid corrosion and prevent Allyl alcohol unit gas explosion, one-time investment costs are relatively high

Method used

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  • Preparation method of dichloropropanol
  • Preparation method of dichloropropanol
  • Preparation method of dichloropropanol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Embodiment 1: as figure 1 As shown, it is a 3-stage chlorination reactor series process, in which T102~T104 are tower chlorination reactors, T101 is a tail gas absorption tower, and T105 is a dichloropropanol (DCP) distillation tower.

[0036] Add glycerin ① and tin salt catalyst ② into the R101 kettle to dissolve into a homogeneous phase, and from the outlet of the kettle ③, through the pump P101, measure and transport ④ into the top of the T101 tower, and enter the tower through the distributor. The catalyst is added once, and under normal operating conditions, it is not added and recycled. The other part of glycerol (without catalyst) feed line ⑤ is directly fed from the top of T101 tower according to the set value of the production scale, and enters the tower through the distributor. Hydrogen chloride ⑦ from hydrogen chloride main pipe ⑥ enters the tower from the T101 tower kettle through the gas distributor, glycerin and hydrogen chloride contact and react counter...

Embodiment 2

[0046] Embodiment 2: as figure 2 As shown, it is a 5-stage chlorination reactor series process, in which the chlorination reaction tower is composed of five towers T102, T103a, T103b, T103c and T104 connected in series, T101 is the tail gas absorption tower, T105 is dichloropropanol (DCP) refined Distillation tower.

[0047] 1) Operating temperature: 100°C,

[0048] 2) Operating pressure: 40kPa(G).

[0049] 3) Chlorination reaction time: 12 hours.

[0050] 4) Chlorination catalyst: tin compound salt, add 1%wt catalyst of the total mass of glycerin at one time when starting up for the first time, and recycle it in normal operating state without adding it.

[0051] Other conditions are with embodiment 1.

[0052] 1) The composition of the chlorinated liquid product is detected by gas chromatography as follows:

[0053]

Embodiment 3

[0054] Embodiment 3: as figure 1 As shown, it is a 3-stage chlorination reactor series process, the chlorination reaction temperature is 115°C, the reaction time is 10 hours, the chlorination catalyst is tin compound salt, and 7%wt catalyst of the total mass of glycerin is added at one time when starting up for the first time, and the normal operation The state is recycled and no longer added. Other conditions are with embodiment 1.

[0055] Detect the chlorinated liquid product components by gas chromatography as follows:

[0056]

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Abstract

The invention provides a preparation method of dichloropropanol. Dichloropropanol is obtained by subjecting glycerin and a chloridizing agent (such as hydrogen chloride) to chlorination in a chlorination reaction tower in the presence of a catalyst. A stannum compound salt is used as the catalyst; a one-time investment of the catalyst is needed, and the catalyst is capable of being recycled. Advantages of the tower reactor are that: uniform contact of solid and liquid is ensured, the time of backmixing is reduced, and the tower reactor is suitable for large-scaled industrial production. Advantages of the preparation method of the invention are that: reaction conditions are mild, side reactions are few, and the yield of dichloropropanol is high.

Description

technical field [0001] The invention relates to a production method of epichlorohydrin intermediate dichloropropanol. Background technique [0002] Dichloropropanol is an intermediate in the production of epichlorohydrin and an important organic raw material. In recent years, the rapid growth of demand for epoxy resin has effectively promoted the development of epichlorohydrin, and the development of epichlorohydrin has led to the development of dichlorohydrin production technology and the expansion of the market. [0003] At present, the methods for industrial production of epichlorohydrin mainly include the chlorohydrin method and the allyl acetate method. The chlorohydrin method has a history of about 50 years, accounting for 95% of the total output of epichlorohydrin (ECH); the disadvantages of the chlorohydrin method are high chlorine consumption, high material consumption, and high energy consumption; severe equipment corrosion and high maintenance costs; products Th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/36C07C29/62
CPCC07C29/62
Inventor 宋秀山韩敏华陈旭辉
Owner 河北珈奥甘油化工有限公司
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