Method for treatment of aluminum alcoholate

FIELD: chemical technology.

SUBSTANCE: invention relates to a method for treatment of aluminum alcoholates. Method involves passing aluminum alcoholates through a column filled with extrudates of aluminum oxide in γ-form with pore volume from 0.4 to 0.8 cm3/g prepared by preliminary hydrolysis of aluminum alcoholates, molding the prepared aluminum oxide to extrudates with diameter from 1.6 to 3 mm and length 3-4 mm and their following purification by calcinations at temperature 400-500°C. As a rule, the treatment of alcoholates is carried out at temperature 20-150°C in column for 1-5 h. Method provides the development of simple and available technology for treatment of aluminum alcoholates with hydrocarbon chain length from C3 to C6 and above from impurities up to the level 10-3-10-4 wt.-%.

EFFECT: improved treatment method.

2 cl, 5 ex

 

The invention relates to chemical technology, in particular to cleaning products, and may find application in chemical industry, petrochemical industry.

The aluminum alcoholate belong to the class alyuminiiorganicheskikh compounds and are used as starting substances for the synthesis of aluminum oxide, regular structure - basis of preparation of the catalysts used in such areas as lighting, electronics. To them have special requirements on the content of impurities. The content of metal impurities upon receipt of the alumina-based alcoholate should be at the level of 10-3÷10-5wt.%.

The achievement of such a high quality product requires additional purification of the intermediate or final products.

The most convenient process is a method of purification of the intermediate liquid aluminum alcoholate, the product of the alcoholysis of metal reactions

2Al+6ROH→2Al(OR)2+3H2

Impurities contained in the original aluminum, provide an alcoholate of various metals. Clearing the alcoholate to a residual content of impurities at the level of 10-4-10-5wt.%, get on the net hydroxide - aluminum oxide

Al(OR)3+3H2O→Al(OH)3+3ROH

2Al(OH)3→Al2O3+3H2About

Cleaning of the aluminum alcoholate perform remote what lazia or filtering. Distillation is possible only for the alcoholate with the length of the hydrocarbon chain of up to 4. Tertiary alcoholate of aluminum have a high boiling point and distillation is difficult. Filtering does not always provide the desired result.

The closest analogue of the claimed method is a method of cleaning alyuminiiorganicheskikh compounds from fine solid impurities by filtration, in which use perlite fraction of 0.3-10 μm, pre-heated at 100-200°in an amount of 0.1 to 3.5 parts 1 parts solids [A.S. USSR 819108, Appl. 23.03.79, publ. 07.04.81. Bulletin no.13]. Perlite is a eutectoid mixture of compounds of iron, ferrite and cementite, which may due to dissolution in the anion impurities containing iron, to contaminate the final product. Moreover, the filtering of the higher alcoholate occurs at a temperature of 60-100°that contributes to the dissolution of iron compounds on the level of the trace.

The disadvantage of this analogue is the low quality of the final product, impurities of large particles are absent, with compounds of iron are at the level of more than 10-3wt.%. due to good solubility of the alcoholate of iron in the aluminum alcoholate.

The present invention is the creation of cost-effective and available treatment technology of aluminum alcoholate with a length of angle is ogorodnoi chain from C 3to C6and above from impurities to the level of 10-3÷10-4wt.%.

This object is achieved by passing the aluminum alcoholate through a column filled with extrudates γ-forms of alumina with a pore volume of 0.4 to 0.8 cm3/g, obtained a preliminary hydrolysis of aluminum alcoholate, the molding of the obtained aluminum hydroxide in extrudates with a diameter from 1.6 to 3 mm and a length of 3-4 mm with subsequent calcination at a temperature of 400-500°C.

Using the preliminary hydrolysis of the alcoholate of aluminum extrudates γ-forms of alumina with a pore volume of 0.4 to 0.8 m3/g with good adsorption ability, enables effective cleaning of impurities of metals.

The use of only one sorbent, obtained by hydrolysis of the intermediate product synthesis ALCOHOLATES aluminum oxide, allows you to have the available technology and cost-effective way to clean the impurities of the metal alcoholate of aluminum with any length of hydrocarbon chain.

The implementation of the method of cleaning the aluminum alcoholate is demonstrated by the following examples.

Example 1

Isopropoxide aluminum hydrolyzing 1% aqueous ammonia solution, the suspension is filtered, separating the aluminum hydroxide. Of aluminum hydroxide after drying it at 100-130°formed With baptizati the th in nitric acid extrudates with a diameter of 1.6-2 mm, the length of 3-3,5 mm, which are calcined at a temperature of 400°C.

The obtained extrudates of alumina with a pore volume of 0.7-0.8 cm3/g fill column skip to clear isopropoxide aluminum for 3.5 hours at a temperature of 100°C.

Get the content of impurities (% wt.) source - Fe2About3- 0,0032; Na2O - 0,001; SiO2- 0,03; TiO2- 0,002; end - Fe2About3- 0,0009; Na2O - 0,0006; Si - 0,0040; TiO2is 0.0001.

Example 2

Isopropoxide aluminum handle, as in example 1, get the aluminum hydroxide is formed into extrudates with a diameter of 2-3 mm, length 4 mm, annealed at a temperature of 500°received by the extrudates of alumina with a pore volume of 0.4-0.45 cm3/g fill column and flow for cleaning isopropoxide aluminum at a temperature of 20°within 1 hour.

The original content of impurities, as in example 1. Get in purified product impurities content (% wt): Fe2About3is 0.0015; Na2O - 0,0008; SiO2- 0,008; TiO2- 0,0007%.

Example 3

Geksanalem aluminum handle, as in example 1, to form extrudates with a diameter of 2-2 .5 mm and a length of 3.5-4 mm, Annealed at 500°receive extrudates with a pore volume of 0.5 to 0.55 cm3/g, fill the column and pass geksanalem aluminum at a temperature of 145-150°C for 3 hours.

Get: the content of primase the original (% wt.) - Fe2About3- 0,0026; Na2O - 0,0019; SiO2- 0,0060; TiO2is 0.001, the final Fe2About3- 0,0008; Na2O - 0,0007; SiO2- 0,0006; TiO2- 0,0008.

Example 4

Piperonyl aluminum handle, as in example 1, formed into extrudates with a diameter of 1.6-1.8 mm, length 4 mm, annealed at 550°receive extrudates with a pore volume of 0.4-0.45 cm3/g and for cleaning geksanalem aluminum at a temperature of 130-135°C for 5 hours.

Get the content of impurities (% wt.) source - Fe2About3- 0,0030; Na2O - 0,0030; SiO2- 0,0058; TiO2- 0,0020, end - Fe2O3- 0,0009; Na2O - 0,0008; SiO2- 0,0008; TiO2- 0,0009.

Example 5

Proposed aluminum handle, as in example 1, formed into extrudates with a diameter of 1.6 to 2 mm, a length of 3-3,5 mm, annealed at 450°receive extrudates with a pore volume of 0.65-0.7 cm3/, Fill the column and passed to empty proposed aluminum at 150°C for 4 hours.

Get the content of impurities (% wt.) original, as in example 1, the end - Fe2O3- 0,0007; Na2O - 0,0008; SiO2- 0,0006; TiO2is 0.0001.

Thus, using the proposed method, it is possible a simple and affordable technology to clean aluminum alcoholate of impurities at the level of 10-3-10-4wt.%, that will allow for appropriate processing to obtain the hydroxide - aluminum oxides is of high purity.

1. The best way to clean the aluminum alcoholate, including the transmission of alcoholate of aluminum through a column filled with extrudates γ-forms of alumina with a pore volume of 0.4 to 0.8 cm3/g, obtained a preliminary hydrolysis of aluminum alcoholate, the molding of the obtained aluminum hydroxide in extrudates with a diameter from 1.6 to 3 mm and a length of 3-4 mm, with subsequent calcination at a temperature of 400-500°C.

2. The method according to claim 1, characterized in that the cleaning of the alcoholate is carried out at a temperature in the column 20-150°and time 1-5 PM



 

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3 cl, 3 tbl, 2 ex

FIELD: chemistry of metalloorganic compounds, chemical technology.

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2 cl, 1 tbl, 1 ex

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< / BR>
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Treatment of glycol // 2265584

FIELD: chemical technology.

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