Method for preparing epoxy chloropropane by using glycerol method

A technology of epichlorohydrin and glycerol, applied in the direction of organic chemistry, etc., can solve the problems of inability to separate the product conversion rate, selectivity, high cost of three waste treatment, and more waste water and residues, etc., to achieve large market competitiveness and production. Low cost and less corrosive effect

Inactive Publication Date: 2007-07-25
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the production methods of epichlorohydrin in the industry mainly include propylene high-temperature chlorination method, propylene acetate method and glycerin method, and the product yields of propylene high-temperature chlorination method and allyl acetate method are less than 90%. At the same time, there are still disadvantages such as low conversion rate, many by-products, high unit consumption, serious corrosion of equipment, high cost of waste water and waste treatment, and high investment.
With the large excess of glycerol, a by-product of oleochemicals, the preparation of epichlorohydrin by glycerol, that is, the preparation of epichlorohydrin with glycerol as a raw material, has become an ideal method for preparing epichlorohydrin, while the existing glycerol method for preparing epichlorohydrin The method of propane is to use glycerol as raw material to prepare epichlorohydrin. The basic catalysts commonly used in the process are liquid alkalis such as NaOH and KOH. The reaction form is a homogeneous liquid-liquid reaction. , there are problems in the purification of products and the separation and treatment of catalysts, and the conversion rate and selectivity of products cannot be separated well. Product quality and production costs need to be optimized

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Under stirring, 5.02 g of calcium nitrate tetrahydrate was dissolved in 10.78 ml of deionized water, and stirring was continued for 60 minutes. 180 milliliters of deionized aqueous solution with 8.33 grams of potassium carbonate dissolved therein was slowly added dropwise to the above solution, and 5.02 grams of triethanolamine was added under the action of stirring, and 9.82 grams of fully calcined γ-alumina was added after fully dispersed to form White gelatinous substance. Stand in a dark place at 20°C for 72 hours. Wash 5 times with deionized water. After removing water by using a rotary evaporator, the solid matter was further dried overnight in a vacuum oven at 25° C., and 12 g of a solid catalyst precursor were recovered. 6 g of this solid catalyst precursor were then calcined. Calcination is carried out by placing the solid substance in an air atmosphere, then heating it to 275°C at a rate of 10°C / min and maintaining it in an air atmosphere at 275°C for 1 hou...

Embodiment 2

[0030] 6 g of the solid catalyst precursor prepared in Example 1 were calcined in the following manner: the solid matter was placed in an air atmosphere, then heated to 275° C. at a rate of 10° C. / min and kept in an air atmosphere at 275° C. for 1 hour the air atmosphere was then changed to argon and the mass was heated from 275°C to 600°C at a rate of 2°C / min and the mass was maintained at 600°C under argon for 5 hours. Finally, the granular solid superbase catalyst CK2 is obtained.

[0031] 10 grams of glycerol with a purity of 95% was continuously passed through dried hydrogen chloride gas at 100° C. for 2 hours in the presence of anhydrous acetic acid (amount equivalent to 10% of the glycerol mass), to obtain 12.5 grams of dichloropropanol. Then add it to a 200-ml round-bottomed flask with 0.5 grams of CK2 placed in advance, install a condenser tube and a drying tube, heat up to 70°C for 5 hours under stirring, and stop the reaction to obtain 9.2 grams of epichlorohydrin. ...

Embodiment 3

[0033]Under stirring, 5.26 g of calcium nitrate tetrahydrate, 1.68 g of sodium nitrate and 0.84 g of potassium chloride were dissolved in 250 ml of de-ethanol, and stirring was continued for 30 minutes. 200 milliliters of deionized aqueous solution having 10.26 grams of sodium carbonate dissolved therein was slowly added dropwise to the above solution, and 7.21 grams of triethanolamine was added under stirring, and 12.82 grams of fully calcined γ-alumina was added after fully dispersed to form White gelatinous substance. Stand in a dark place at 20°C for 72 hours. Wash 5 times with deionized water. After removing water by using a rotary evaporator, the solid matter was further dried overnight in a vacuum oven at 25° C., and 18 g of a solid catalyst precursor were recovered. 9 g of this solid catalyst precursor were then calcined. Calcination is carried out by placing the solid substance in an air atmosphere, then heating it to 275°C at a rate of 10°C / min and maintaining it ...

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Abstract

This invention discloses a glycerol method for preparing epoxy chloropropane. The method comprises: (1) introducing dried HCl gas through 95% glycerol at 90-110 deg.C in the presence of absolute acetic acid, and reacting for 1-3 h; (2) adding the obtained dichloropropanol into a round bottom flask loaded with solid super-strong alkali catalyst, equipping condensing and drying tubes, stirring, heating to 70-90 deg.C, reacting for 3-5 h, filtering, and separating the catalyst to obtain chloropropane.

Description

technical field [0001] The present invention relates to a kind of method for preparing epichlorohydrin, more specifically relate to a kind of method for preparing epichlorohydrin by glycerol method. Background technique [0002] Glycerin is an important raw material for military industry, light industry, and chemical industry. In recent years, with the continuous expansion of oleochemicals, especially biodiesel, the by-product glycerin has been seriously oversupplied and its price has fallen sharply. It is important to develop downstream products using glycerin as a raw material. It is a good method to solve the excess of glycerin, if a suitable production method of downstream products can be developed, the production cost of downstream products can be reduced. Epichlorohydrin (3-Chloro-1, 2-epoxypropene), also known as epichlorohydrin, is an important organic chemical raw material and fine chemical product with a wide range of uses. It is the main raw material of epoxy res...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D301/26C07D303/08
Inventor 蒋剑春罗振扬顾晓利何明李书龙聂小安李翔宇
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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