The method of separation of 2,6-di-tert.-butylphenol products from the alkylation of phenol with isobutylene

 

(57) Abstract:

Usage: in the process of vacuum distillation selection of products of alkylation of phenol in the presence of an activator-dioxide. The inventive selection of 2,6-di-tert-butylphenol from the products of alkylation of phenol with isobutylene by distillation under vacuum is carried out in the presence of carbon dioxide, taken in an amount from 0.01 to 0.10% by weight of 2,6-di-tert-butylphenol, exported from the column. 1 C.p. f-crystals.

The invention relates to petrochemical synthesis, namely to obtain 2,6-di-tert-butylphenol (2,6-DTBP) emitted from the products of alkylation of phenol with isobutylene by rectification method.

A known method for separating 2,6-DTBP from the products of alkylation method of rectification, pre-treating the products of alkylation of oxalic, citric or tartaric acid and water (Japan's Bid N 58-14413; CL 07 With 39/06, 1983).

However, this method is accompanied by intensive corrosion of the equipment, a large number of acidic wastewater. (A. S. N 405243, 1971, N 707902, 1977) products of alkylation before allocating the rectification process water, alkaline solutions. But this method, like the previous, characterized

A known method for separating 2,6-DTBP by rectification when the stability of 2,6-DTBP is saved due to the fact that the reaction mass is treated with propylene oxide or its corresponding derivative (A. S. N 1216944, class C 07 C 39/06, 1984).

However, although the method allows to allocate 2,6-DTBP high enough concentration to 99.8 wt.% but it also has its drawbacks: the presence of the target product as impurities 3,3,5,5-Tetra-tert-butylperoxide.

The content of the named Difenoxin is not large (0,001-0,05%), but these quantities are enough to paint the end product, which dramatically reduces its consumer properties.

Also known is a method for separating 2,6-DTBP from the products of alkylation by distillation with preliminary treatment of the products of the alkylation of propylene oxide with propilenglikolem (A. S. N 167422, class C 07 C 39/06, published. 1991). Although the target product according to the invention receives and high concnetrate, but the disadvantages of this process should include high consumption of propylene oxide and propylene glycol, which generally leads to higher process, and also deficiency of propylene glycol. And the main disadvantages include a relatively low target 2,6-DTBP, namely CEE the WMD - the prototype is a way of separating 2,6-DTBP, ongoing in the industry at the Sterlitamak petrochemical plant, process regulations (TR-1.03260-86 "Process regulation of experimental-industrial production of 2,6-di-tert-butylphenol method of alkylation of phenol with isobutylene", Sterlitamak, 1986]. The process is carried out in a distillation column with number plates 20, the temperature of the cube 160-230aboutWith the pressure of 20 ml RT.art., reflux the number of 1.66 in a stream of nitrogen. The purity of the target product of 99.5%. The disadvantages of the known method can also be attributed to the relatively low quality of the target product, in particular color, as a main indicator, which have consumers of foreign firms and which dramatically changed for the worse, especially with a long shelf life.

The aim of the invention is ostranenie these disadvantages, namely improving the quality of the target product and the preservation of color in a long time.

This objective is achieved in that the selection of the target product are carried out by distillation in the presence of carbonic acid or carbon dioxide.

Obviously CO2or carbonic acid ingibiruet the H OO

The process of separating 2,6-DTBP carried out in a distillation column in the prototype.

P R I m e R 1 (the prototype). 100 g of 2,6-di-tert-butylphenol raw, obtained by alkylation of phenol with isobutylene composition, wt.%: 2-tert-butylphenol 0,05 2,6-di-tert-butylphenol 99,20 2,5-di-tert-butylphenol 0,65 2,4,6-tri-tert-butylphenol 0,10 subjected to distillation column with 20 theoretical plates at reflux 12 and the residual pressure of the top of column 20 mm RT.article When selecting the top 70% of the product from the feedstock received the product of the following composition, wt.%: 2-tert-butylphenol 0,50 2,6-di-tert-butylphenol 99,40 2,4-di-tert-butylphenol 0.10 Product was cooled, kept in nitrogen atmosphere and measured chromaticity scale ARNA in time.

The data are given in table.1.

P R I m e R e 2 (comparative). In the conditions of example 1. 2,6-di-tert-butylphenol was allocated on a column of the same efficiency and at the same reflux. In the flow phlegmy added adipic acid at the rate of 0.01 wt.% on the finished product. Target product (70 g) had the following composition, wt.%: 2-tert-butylphenol 0,40 2,6-di-tert-butylphenol 99,56 2,4-di-tert-butylphenol 0,04 Measured chromaticity.

The data are given in table. 2.

P R I m e R 3. In the conditions of example 1 2,6 - product was 0.01 wt%.

The composition of the finished product (70 g), wt.%: 2-tert-butylphenol 0,03 2,6-di-tert-butylphenol 99,95 2,4-di-tert-butylphenol 0.02

Data on the color shown in the table.3.

P R I m e R 4. In the conditions of example 1 to produce 2,6-DTBP by distillation, adding a steam flow of 0.5 wt.% CO2. The finished product (70 g) has the following composition, wt.%: 2-tert-butylphenol - 0,02 2,6-di-tert-butylphenol 99,97 2,4-di-tert-butyl 0,01

Data on the color shown in the table.4.

P R I m e R 5. In the conditions of example 1 to produce 80 g of 2,6-DTBP by distillation, adding steam flow 0.1 wt.% CO2.

Target 2,6-DTBP receive the following composition, wt.%: 2-tert-butylphenol 0,02 2,6-di-tert-butylphenol of 99.98 2,4-di-tert-butylphenol UTS.

Data on the color shown in the table.5.

When carrying out rectification, adding a smaller amount of CO2than 0.1 wt.% in steam flow does not improve the quality of the target product and the color index correspond to the prototype. A greater number of CO2than 0.1% apply impractical, since it practically affects improvement.

P R I m e R 6 (comparative). In the conditions of example 1 dedicated 2,6-DTBP rectification after cooling, kept it in atmospheres is nitely). In the conditions of example 1 dedicated 2,6-DTBP by distillation at the same reflux. In the flow phlegmy add nitrogen at the rate of 0.05 wt.% on the finished product. Selected 2,6-DTBP the following composition, wt. %: 2-tert-butylphenol 0,06 2,6-di-tert-butylphenol 99,85 2,4-di-tert-butylphenol 0,09

Measured chromaticity scale ARNA in time. The data are given in table.7.

Thus, as seen from the above examples, conducting rectification 2,6-DTBP in the presence of carbon dioxide allows to obtain the target product of higher quality and to keep the color in time that satisfies the requirements of the consumer.

1. The METHOD of separation OF 2,6-DI-TERT-BUTYLPHENOL FROM the PRODUCTS of ALKYLATION of PHENOL with ISOBUTYLENE by distillation in a vacuum, characterized in that, with the aim of improving the quality in terms of color under conditions of prolonged storage of the product, the distillation is carried out in the presence of carbon dioxide.

2. The method according to p. 1, characterized in that the amount of carbon dioxide is from 0.01 to 0.10% by weight of 2,6-di-tert-butylphenol, taken from the top of the column.

 

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