RU1817777C - Method of purifying 1,2-epoxy-7-octene - Google Patents

Abstract

The method of purification of 1,2-epoxy-7-octene from: α-methylstyrene. Use: as a monomer for rubber production. Essence: 1.2-epoxy-7-octene. Its purification is carried out by extractive distillation using normal structure Се-Сю alcohols or alkyl aromatic alcohols or distillation products of production of 1.2-epoxy-7-octene in the molar ratio of alcohol: 1.2-epoxy-7-octene as a separating agent. . equal to (1 - 10):: 1.

Description

The invention relates to the purification of epoxy compounds, in particular to a process for the purification of 1,2-epoxy-7-octene. obtained by epoxidation of 1,7-octadiene with isopropylbenzene hydroperoxide.

The purpose of the invention is to simplify the process.

The goal is achieved by the proposed method for the purification of 1,2-eloxy-7-octene by distillation in the presence of alcohols, the distinguishing feature of which is that extractive distillation is carried out using St. alcohols of normal structure as a separating agent. or alkyl aromatic alcohols, or bottoms from the production of 1,2-epoxy-7-octene with a molar ratio of alcohol: 1,2-epoxy-7-octene equal to (1-10): 1.

The method is as follows. A mixture of a-methylstyrene and 1..2-epoxy-7-. octene is fed to a continuous extractive rectification column. The extractant is introduced from above into the column at 60-70 ° C. The top pressure of the column is 2.7 kPa, which ensures the temperature of the bottom of the column is not higher than 120 ° C. On top of the column, about. -methylstyrene, and the bottom residue containing 1,2-epoxy-7-octene and the extractant are subjected to rectification on the second column. Commodity 1,2-eg.oxy-7-octene is taken from above the column, and the extractant, in view of the bottoms product, is sent again for extractive distillation or for regeneration. In the case of periodic process design, a mixture of it. -methylstyrene and 1,2-epoxy-7-octene are loaded into the cube of a distillation column. The extractant is fed from above at the same temperatures and pressures as in the continuous rectification option. The α-methylstyrene fraction was taken and the extractant was stopped. Then, a fraction of marketable 1,2-epoxy-7-octene was selected. A regenerated extractant is selected as the third fraction.

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PRI me R 1.

The initial mixture containing 86.6 wt.% 1,2-epoxy-7-octene and 13.4 may. % a-methylstyrene in an amount of 190 g is loaded into a cube of a laboratory distillation column of periodic operation with an efficiency of 35 theoretical plates. A separation agent 1-octanol is introduced at a speed of 117 g / h at 63 ° C, corresponding to the top temperature. . The top pressure of the column is 2.7 kPa, the reflux value is 5. Fraction 1 weighing 32.0 g consists of 28 wt.% 1,2-epoxy-7-octene and 72 may. % a-methylstyrene. After selection of the first fraction, the extractant supply was stopped and a fraction weighing 151 g containing 98 wt.% 1,2-epoxy-7-octene and 2 wt.% A-methylstyrene was taken. 575 g was fed to the extractant, and the molar ratio of 1-octanol: 1.2-epoxy-7-octene was 3: 1. The yield of 1.2-epoxy-7-octene is 90%.

EXAMPLE 2 An initial mixture containing 92% by weight of 1,2-epoxy-7-octene and 8% by weight of a-methylstyrene is fed to a continuous distillation column with an efficiency of 30 theoretical plates at a speed of 150 g / h. At the top of the column at 63 ° C, corresponding to the top temperature, the 1-decanol extractant is fed at a rate of 170 g / h (molar ratio 1-decanol: 1.2-epoxy-7-octene 10: 1). The pressure of the top of the column is 2.7 kPa, the reflux number is 5, a-methylstyrene containing May 20 is taken from the top of the column. % -1.2-epoxy-7-octene; From the bottom of the column at 120 ° C (bottom pressure of 10 kPa), 1; 2-epoxy-7-octene with a concentration of 45% by weight in 1-decanol is taken. On the second column at a top pressure of 2.7 kPa, a temperature of 66 ° C, 1.2-epoxy-7-octene with a purity of at least 99 wt.% Was selected. The bottoms product is used as a resolving agent. The yield of 1,2-epoxy-7-octene is 96%.

Example 3. The initial mixture containing 87.2 wt.% 1,2-epoxy-7-octene and 12.8 wt.% A-methylstyrene, in an amount of 250 g, was loaded into a cube of a laboratory distillation column of periodic action with an efficiency of 35 theoretical plates, The extractant, 2-phenylpropanol-2, is fed to the top of the column at 63 ° C. The top pressure of the column is 2.7 kPa. The feed rate of the extractant is 85 g / h, reflux number 5. After the selection of the first fraction weighing 40 g containing May 80. % a-methylstyrene and 20 wt.% 1,2-epoxy-7-octene, the extractant was stopped and a second 210 g fraction was taken consisting of 99% of 1.2 epoxy-7-octene and 1% in May. a-methylstyrene. The extractant is recovered as a 3rd fraction and recycled. A total of 470 g of extractant was fed; the molar ratio of 2-phenylpropanol-2: 1,2-epoxy-7-octene was 2: 1. The yield of the target product 96.5%,

PRI me R 4. The initial mixture containing 87.2 wt.% 1,2-epoxy-7-octene and 12.8 wt.%

a-methylstyrene, in an amount of 250 g, is loaded into a cube of a laboratory distillation column with an efficiency of 35 tons. An extractant is introduced into the upper part of the column at 63 ° С corresponding to the top temperature — a mixture of bottoms from the synthesis of 1,2-epoxy-7- octene containing 92 wt.% 2-phenylpropanol-2, 2.0 wt.% acetophenone, 1.4 wt.% 1,2,7,8-diepoxy octane, 4.0 wt.% undecanol-1 and 0.6 wt. .% phenol,

at a speed of 85 g / h. The top pressure of the column is 2.7 kPa, the reflux value is 5.0. After selection of the first fraction, weighing 40.0 g and consisting of 25.4 wt.% 1,2-epoxy-7-octene and May 74.6.% A. -methyl styrene, stop feeding the extractant and select the second fraction weighing 210 g of composition: 99.0% of 1,2-epoxy-7-octene and 1.0 wt.% α-methylstyrene. The temperature of the top of the column 66 - 67 ° C. An extractant was selected as the third fraction. A total of 234 g of extractant was applied (molar ratio of 1,2-epoxy-7-octene: extractant 1: 1). The yield of the target product 95.4%.

Example 5. An initial mixture containing 92 wt.% 1,2-epoxy-7-octene and 8 wt.% Α-methylstyrene, in an amount of 200 g, was loaded into a cube of a laboratory distillation column of periodic action with an efficiency of 35 tons. t. To the top of the column

The extractant 1-phenylethanol is fed. The top pressure of the column is 2.7 kPa. The feed rate of the extractant is 150 g / h, the reflux ratio is 6. After selection of the first fraction weighing 16 g, containing 89.6 wt.% Of its α-methylstyrene and

10.4 wt.% 1,2-epoxy-7-octene, stop the flow of extractant and select the second fraction weighing 184 g of the composition: 99.1 wt.% 1,2-epoxy-7-octene and 0.9 wt.% "-Methyl- styrene. The temperature of the top of the column 63 64 ° C. Extragelt was selected as the third fraction. A total of 890 g of extractant was fed (molar ratio of 1,2-epoxy-7-octene: 1-phenylpropanol is 5: 1).

The presented data indicate that the proposed method allows to isolate 1,2-epoxy-7-octene from its mixture with α-methylstyrene with a purity of not less than 98% and with a yield of more than 90% and substantial

significantly simplifies the process of regeneration; separation is carried out using as

Claims (1)

separating agent. separating agent of alcohols Ce Xiu nor Formula of the invention of small building or alkyl aromatic The method of purification of 1,2-epoxy-7-octene p-alcohols or distillation products is carried out by rectification in the presence of alcohols, 5 of 1.2-epoxy-7-octene with a molar ratio of which for the purpose of alcohol: 1,2-epoxy-7-octene. simplification of the process, extractive recti-equal (1 - 10): 1.