CS223060B3 - A method for producing alkylated 1-hydroxy-2,6-dimethylbenzene - Google Patents

Abstract

The invention solves the technology for the production of alkylated 1-hydroxy-2,6-dimethylbenzene with polymers or copolymers of "-alkenes" with an average polymerization degree of 5 to 50, under the catalytic effect of boron halides, tetravalent titanium, bleaching clay, or activated phosphoric acid. It describes the individual technological nodes of production and their production conditions. The invention can be used in the field of organic technology.

Description

3 4 223060

The present invention relates to methods for the preparation of alkyl alcohol hydroxy-2,6-dimethylbenzene by polymers or copolymers of α-alkenes having a moderate polymerization degree of 5 to 50, with the catalytic effect of boron halides, tetravalent titanium, bleaching earth alone or activated] phosphoric acid. The alkylation of hydroxyarenes is described in U.S. Patent Nos. 17 46 79 and 20 00 55. The essence of the present invention is to optimally arrange the technological nodes and finish the product to achieve the desired quality parameters.

In the process of the present invention, unreacted hydroxyarenes and alkylated hydroxyarenes are removed, wherein alkyl is a lower fraction of C4-C8 polypropylene oil by providing a distillation node in the manufacturing process. yenfinishing with bleaching earth or powder metals II. and III. of the periodic group.

In view of the above, the production has been divided into these technological features with the "following."

By feeding the appropriate amount of dry matter and catalysis of the toro at 80 to 200 ° C, the feed is alkylated for 6 to 20 hours in a stirred apparatus to maintain the catalyst in suspension.

Separation of the catalyst after alkylation and cooling of the feed is removed from the reaction mixture by the catalyst.

Distillation:

The distillation process is designed so that the product is as low as possible to heat - therefore a pre-feed preheater is preheated in front of the film rotor to heat the injected alkylate from 80 to 100 ° C at 1160 to 200 ° C and at the filed rotor the evaporator is distilled at a temperature of 120 to 300 ° C with a flask of 0.2 to 5 kPa, the residence time of the alkylate in the preheater and the evaporator being 2 to 10 minutes.

Raíinácia:.

The distilled (darker) product is refined in a blended apparatus at 80 ° C with bleaching earth or powder metals II. and III. groups of periodic states.

After refining, the refining agent used is separated and the product obtained can be used in liquid form or applied with a suitable carrier, such as some polyethylene, polypropylene, or inorganic salts of silica, such as Siloxide (precipitated acid The method provides an antioxidant addition of the desired parameters for the polyolefins.

The process of the present invention removes unreacted hydroxyarenes and alkylated hydroxyarenes, where alkyl has 9 carbon atoms, by including a distillation node. Subsequent refining yields the product of the desired quality parameters. Example 1

To 1200 kg of polypropylene oil of 500-550 < -1 >, in the blended apparatus, 382 kg of 1-hydroxy-2,6-dimethylbenzene and 60 kg of bleaching clay were added. The mixture was heated to 140 ° C and alkylation continued for 12 hours. After separation of the solids at 80 ° C, the mixture was heated to 120 ° C and distilled on a film rotor evaporator, heated to 250 ° C and a pressure at the evaporator head of 1.5 kPa. A product was obtained whose color was 2000 Hazen units. After subsequent refinement with the bleaching clay, the Oi product of 800 Hazen units was obtained. Example 1

575 kg of 1-hydroxy-2,6-dimethylbenzene and 125 kg of bi-casting clay were added to 1800 kg of polypropylene oil in a blended apparatus. This mixture is heated to 140 ° C and alkylated for 12 hours. After separating the solid particles, the alkylation mixture is injected through a pre-injector onto a film crucible evaporator heated to 240 ° C and 1 kPa pressure on the head. After distillation, 2025 kg of a product of 1200 Hazen units and a bound 1-hydroxy-2,6-diethylbenzene of 7.3 wt% and 0.1 wt% of free 1-hydroxy-2,6-dimethylbenzene are obtained. . After refining in a mixer at 80 [deg.] C. and filtering off the bleaching earth, a product was obtained, coloring 600 Hazen units. Example 3

Up to 1800 kg of polypropylene oil adds 575 kg of 1-hydroxy-2,6-dimethylbenzene and 125 kg of bleaching clay. After heating to 130 ° C, the mixture is alkylated for 14 hours under a nitrogen atmosphere. After separating off the particulates at 80 ° C, the alkylate is heated to 120 ° C and the temperature is raised to 180 ° C through the preheater and sprayed on a 100-milliliter rotor evaporator, heated to 250 ° C and a pressure of 1.5 kPa on the head is recovered after distillation. 1700 kg of product with a composition of 8.4% by weight bound and 0.07% by weight of free 1-hydroxy-2,6-dimethylbenzene with a color of 800Hazen units. Example 4

575 kg of 1-hydroxy-2,5-dimethylbenzene are added to 1800 kg of polypropylene oil

Claims (2)

1. Preparation of an alkylated 1-hydroxy-2,6-dimethylbenzene according to Author's Certificate AO 174 679 characterized in that the alkylation of l ^J hydroxy-2,6-dimethylbenzene polypropylene oil having an average molecular weight of 380 at a temperature of 80 to 200 degrees Celsius, preferably 140 ° C for 6 to 20 hours, preferably 12 hours, to form the crude alkylated 1-hydroxy-2,6-dimethylbenzene, the crude alkylated product is OF THE INVENTION preheats from 80 to 100 ° C to 160 to 200 ° C and distills at 120 to 300 ° C, preferably at 220 ° C under a pressure of 0.2 to 5 kPa, the preheating time being 2 to 10 minutes and the product obtained Refined at 80 ° C. 2. The process according to claim 1, wherein the alkylation of 2,6-dimethylbenzene is carried out by catalytic deposition of bleaching clay.