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A kind of method for preparing epichlorohydrin

A technology of dichloropropanol and oxides, applied in the direction of organic chemistry, can solve the problems of high salt content industrial wastewater, many by-products, etc., and achieve the effect of high catalytic activity, less side reactions and simple process

Active Publication Date: 2017-04-12
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its reaction form is a liquid-liquid homogeneous reaction. The saponification reaction requires an excessive amount of lye. In this process, a large amount of industrial wastewater with high salt content that is difficult to treat is produced, and there are many by-products. The purification of the product needs to be further improved.

Method used

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  • A kind of method for preparing epichlorohydrin
  • A kind of method for preparing epichlorohydrin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] This example illustrates the reaction process and results when the catalyst is 5CaO / 80NaZSM-5 (the mass of supported CaO is 5% of the mass of NaZSM-5, Si / Al=80).

[0019] (1) First prepare 500ml of NaNO with a concentration of 1mol / L 3 Solution, then take 3g of HZSM-5 (Si / Al=80) molecular sieve powder and dissolve in sufficient amount of the above solution, stir at room temperature for 2~3h, repeat 4 times, after suction filtration and drying, roast at 550°C 6h to get 80NaZSM-5 sample.

[0020] (2) Add 0.4211g of Ca(NO 3 ) 2 4H 2 O was dissolved in 2.5ml of distilled water corresponding to the saturated water absorption volume of 80NaZSM-5, and then 2g of 80NaZSM-5 powder was mixed in the above solution, after drying, it was calcined in air at 550°C for 7 hours to obtain 5CaO / 80NaZSM-5 catalyst powder.

[0021] (3) Press the catalyst obtained above into tablets with a powder tablet press with a pressure of 6 MPa and a holding time of 1 min, and then grind and scree...

Embodiment 2

[0025] This example illustrates the reaction process and results when the catalyst is HY.

[0026] Press the HY molecular sieve powder into tablets, screen out 0.3g of HY molecular sieve particles with a diameter of 80-100 mesh, put the weighed HY molecular sieve particles into the reaction tube (Ф8 mm×1 mm×250 mm), and the temperature of the saturator is 60 °C, the carrier gas flow rate is 200ml / min, and other steps are the same as (4) in Example 1.

[0027] temperature(℃) Conversion rate / % Selective / % Yield / % 300 32.0 83.1 26.3 330 32.4 80.0 26.0 360 32.9 76.0 25.1 390 18.1 61.6 11.1

Embodiment 3

[0029] This example illustrates the reaction process and results when the catalyst is 10MgO / 25NaZSM-5 (the mass of supported MgO is 10% of the mass of NaZSM-5, Si / Al=25).

[0030] The Na exchange process of HZSM-5 (Si / Al=25) molecular sieve is the same as that of Example 1 (1), and 1.2722g of Mg(NO 3 ) 2 ·6H 2 O was dissolved in 2.5ml of distilled water corresponding to the saturated water absorption volume of 25NaZSM-5, and 2g of 25NaZSM-5 powder was mixed in the above solution, and after drying, it was calcined in air at 550°C for 7 hours to obtain 10MgO / 25NaZSM-5 catalyst powder. Other steps are the same as steps (3) (4) in Example 1. The result is as follows:

[0031] temperature(℃) Conversion rate / % Selective / % Yield / % 300 91.7 95.3 87.4 330 97.1 96.8 93.9 360 98.2 96.6 94.9 390 62.7 93.5 58.6

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Abstract

The invention relates to a method for preparing epoxy chloropropane. Material dichloropropanol and carrier gas together enter a fixed bed cyclizing device filled with a catalyst after dichloropropanol is gasified, a gas-phase hydrogen chloride removal and cyclization reaction is carried out in the temperature range of 200-450 DEG C, hydrogen chloride and product epoxy propane are separated through a condensation pipe, and the catalyst is selected from one of a molecular sieve HY, Hbeta, HZSM-5 and sodalite. The optimal catalyst is a solid base catalyst obtained by loading alkaline earth metal oxide on a cation-type molecular sieve. Production cost is low, side effects are few, the conversion rate of the reaction is increased, and product selectivity is improved. By means of a gas-phase cyclizing heterogeneous reaction system, a series of defects, for example, three wastes are difficult to treat, caused by a liquid-liquid homogeneous reaction are successfully avoided, and the obtained product is easy to separate.

Description

technical field [0001] The invention relates to a method for preparing epichlorohydrin, in particular to a method for preparing epichlorohydrin by gas-phase catalysis of 1,3-dichloro-2-propanol. Background technique [0002] Epichlorohydrin (Epichlorohydrin), also known as epichlorohydrin, is an important organic chemical raw material and synthetic intermediate. Among epoxy compounds, the output of epichlorohydrin ranks third, second only to ethylene oxide and propylene oxide. In 2012, the production capacity of epichlorohydrin in the world was about 2.484 million t / a, and that in my country was 1.06 million t / a. In recent years, my country has developed into the world's largest producer of epichlorohydrin, and its self-sufficiency rate has continued to increase. Epichlorohydrin has a wide range of uses, mainly used in the production of epoxy resin, synthetic nitroglycerin explosives, glass fiber reinforced plastics, electrical insulation products, (glycidin) derivatives, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D303/08C07D301/26
CPCC07D301/26C07D303/08
Inventor 李福祥梁云霞罗雄薛建伟吕志平
Owner TAIYUAN UNIV OF TECH
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