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Clean process for preparing epoxy chloropropane by zero discharge glycerin method

An epichlorohydrin, zero-emission technology, applied in the field of cleaning processes, can solve the problems of salt deposition in biochemical systems, deterioration of sludge performance, and high cost, and achieve the effect of huge application potential.

Inactive Publication Date: 2017-06-23
HUIZHI ENG SCI & TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In addition to high salinity, epichlorohydrin production wastewater also contains organic matter, which is difficult and expensive to treat. It is one of the most difficult wastewater to treat in the world.
At present, the method of salt production by evaporation is mainly used in industry, but the salt produced contains a large amount of organic matter, which is difficult to sell and becomes solid waste; the dilution biochemical method will waste a lot of water resources, and this process often leads to salt deposition in biochemical systems, Cause sludge performance deterioration and other phenomena
With the increasingly stringent environmental protection requirements, the treatment of epichlorohydrin wastewater has become an unfavorable factor restricting the development of enterprises, affecting the construction of new enterprises, and even affecting the production of established enterprises.

Method used

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  • Clean process for preparing epoxy chloropropane by zero discharge glycerin method
  • Clean process for preparing epoxy chloropropane by zero discharge glycerin method
  • Clean process for preparing epoxy chloropropane by zero discharge glycerin method

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Embodiment 1 (laboratory scale)

[0031] In a 500ml four-necked flask, add 200g of glycerol, catalyzer (anhydrous acetic acid) 16g, put the stirrer in the mouth of the center, put the thermometer in the side mouth, and the other two mouths are the inlet pipe and the outlet of HCl respectively. React at about 100°C until the amount of HCl gas evolution no longer changes. The reaction yielded a yellow liquid product, which was evaporated to remove water and catalyst on a rotary evaporator to obtain relatively pure 1,3-dichloro-2-propanol (238 g, yield about 85%).

[0032] Mix 1,3-dichloro-2-propanol with NaOH solution (420g solution, 20wt.%), cyclization reaction occurs at about 70°C to generate epichlorohydrin, then distill to obtain crude epichlorohydrin, and rectify to obtain Pure epichlorohydrin (162 g, about 95% yield).

[0033] Add hydrochloric acid into the cyclization wastewater (adding a small amount can remove the excess NaOH in the cyclization reaction and th...

Embodiment 2

[0037] Embodiment 2 (industrial scale, epichlorohydrin output is 10kt / y)

[0038] Glycerin 1555kg / h from the glycerin storage tank is preheated by the glycerin preheater and then enters the chlorination reactor; HCl gas 1666kg / h from the hydrochloric acid synthesis unit is passed into the chlorination reactor for chlorination reaction, and the reaction temperature is 90-105°C , the reaction pressure is a slight positive pressure. In the early stage of the reaction, steam should be passed into the interlayer of the reaction kettle for heating. temperature.

[0039] After the reaction is finished, the reactant dichloropropanol is distilled by means of external circulation heating, and the steamed crude dichloropropanol (containing about 1854kg / h of dichloropropanol) is transported to the transfer tank through a pump, and the excess HCl gas is pumped into another tank. The glycerol in the chlorination reactor is absorbed, and the HCl that is still not fully reacted enters the ta...

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Abstract

The invention relates to a method for preparing epoxy chloropropane by glycerin, in particular to a clean process for preparing epoxy chloropropane by a zero discharge glycerin method. The clean process is characterized in that glycerin and HCl generate substitution reaction to generate dichloropropanol; NaOH is added into dichloropropanol for cyclization reaction to generate epoxy chloropropane; high-salinity wastewater generated by the reaction is decomposed into HCl and NaOH through bipolar membrane electrodialysis; HCl and NaOH are respectively recycled and generate the substitution reaction and the cyclization reaction with glycerin and dichloropropanol, so that cyclic utilization is realized, and the high-salinity wastewater is not discharged. The clean process provided by the invention has the advantages that the substitution reaction between glycerin and HCl, the cyclization reaction between dichloropropanol and NaOH, and the bipolar membrane electrodialysis decomposition of a NaCl aqueous solution are integrated, the clean production of epoxy chloropropane by the glycerin method is realized, the zero discharge is achieved, the environment is not polluted, and an application potential is huge.

Description

technical field [0001] The invention relates to a method for preparing epichlorohydrin from glycerin, more particularly to a clean process for preparing epichlorohydrin by a zero-emission glycerol method. Background technique [0002] Epichlorohydrin is an important organic chemical raw material and fine chemical intermediate, mainly used in the production of epoxy resin, reinforced resin, water treatment resin, etc. In recent years, more and more epoxy resins have been used in electronics, automobiles, aerospace and other industries, resulting in an increasing demand for epichlorohydrin. [0003] At present, epichlorohydrin is mainly produced by high-temperature chlorination of propylene, which mainly includes high-temperature chlorination of propylene to prepare chloropropene, chloropropene and hypochlorous acid to synthesize dichloropropanol, and dichloropropanol to synthesize epichlorohydrin. responses. The process produces 40-50 tons of high-salt wastewater per ton of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/08C07D301/26
CPCC07D301/26C07D303/08
Inventor 齐运峰谭明张杨逯云玲刘庆德郎巧霖
Owner HUIZHI ENG SCI & TECH CO LTD
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