SU749417A1 - Method of producing catalyst for preparing 2-ethylhexanol by condensation and hydrogenation of butyr aldehyde or for buthyl alcohol condensation - Google Patents

Description

This invention relates to methods for producing 2.-ethihexanol. A method of producing 2-ethylhexanop is known by heating for 98 hours at a temperature of 14 ° C butyl alcohol in the presence of sodium hydroxide, toluene and a hydrogenation catalyst (NL on kieselguhr) in an iron reactor. The output of 2-athexanol - l. The disadvantage is the length of the process. The closest technical solution to the present invention is with the preparation of 2-ethylhexanol: co-sensation of oil apdepad to 2-ethyl. hexanal in the presence of a homogeneous cobalt catalyst, and hydrogenation of the obtained product in two stages on an alumina-zinc and nickel-chromium catalyst to 2-ethylhexanol at a hydrogen pressure of ZOO atm and a temperature of 2. The disadvantage of this method is the multistage process and the use of high pressures. The aim of the invention is to simplify the method. For this, 2-ethylhexanol is obtained by catalytic condensation and hydrogenation of oil aldehyde in the presence of a catalyst of the following composition, wt.%: Titanium dioxide 5O-6O Copper oxide 40-5O at a temperature of 225-250 C and supply of oil aldehyde 0,7-O, 8 l and hydrogen 36O-420 l per 1OOO cm catalyst per hour. Distinctive features of the invention are to conduct the process in the presence of a catalyst containing, in wt.%; Titanium dioxide ОО-60 Copper oxide 40-50 with the above technological parameters of the process. Catalysis can be repeatedly regener ated, for which it is activated by oxidation directly in the reactor with an oxygen-containing mixture (5% Og) at a temperature of 25 ° -3.0 C for hours, after the end of oxidation it is heated in air at 300-32 5 ° C for 2-4 hours, and then restore the hydrogen-nitrogen mixture (1: 3) at a temperature of 24 ° 27 ° C. Butyl alcohol, which is formed as a by-product of the solution, can be returned to the process and subjected to concretion in 2-ethylhexanol. This method of producing 2-ethyhexanol allows the process to be carried out in a single step at a lower temperature of 225,. Example. A catalyst of the following composition is prepared, wt.%: Oxide of copper 40 Titanium dioxide 60. For this, 75 O ml of a 15% solution of titanium sulphate (III) in sulfuric acid is oxidized by the gradual addition of concentrated nitric acid (until the violet color disappears). 750 ml of distilled water is added to the obtained solution of quadruple titanium and titanium hydroxide is precipitated with a solution of caustic soda (1: 2) and the solution is neutralized to pH 5 using universal indicator paper. About 530 ml of alkali solution is used for osisation. The precipitate obtained is repeatedly decanted with warm (4O-5O C) distilled water to remove io-HaNO. For better precipitation at the end of the rinse, 50100 ml of a saturated solution of nitric sodium are added to the precipitate, mixed and the final run from the sulfate ions is carried out. Water is drained from the washed precipitate of titanium hydroxide and a solution of 121 g Cu (NO) 2 NH2, O is added to 38 O ml of water, heated to 85-90 ° C, 50 ml of 9 Sodium chloride (H 1: 2) are quickly added with vigorous stirring). and then, added in small portions of alkali, the pH is adjusted to 7-8.

The crawled black-brown precipitate is decanted with boiling distilled water until the ion N0 is removed, filtered off on a Büchner funnel, and air dried. The catalyst is then transferred to

npojqyKTOB reactions When oil aldehyde condenses in the presence of hydrogen on a catalyst containing 50% of copper and titanium oxides under the conditions as in Example 1 at a temperature.

As can be seen, the composition of the condensate varies slightly. 174 porcelain cup and dried in a thermostat at 40-50 C for 5 hours, and then - at 2OO With more than 5 hours. The obtained solid black catalyst is crushed into pieces of 3-5 mm in size, sifted out from dust. The dry catalyst code is 11O-115 g (95-100%). The catalyst loaded into the reactor is reduced by hydrogen-nitrogen mixture (1: 3) at a temperature of 240-270 ° C before synthesis of higher alcohols. Table. 1 shows the composition and yield of the reaction products during the condensation of oil aldehyde in the presence of hydrogen in a molar ratio of 1: 2 on the catalyst at a temperature of 22 5 ° C, the supply of oil aldehyde 0.7-0.8 l and hydrogen 36O-42O l on 1 liter of catalyst per hour. In tab. 2 shows the composition and yield of condensation products of butyl alcohol on the proposed catalyst in the presence of hydrogen in a molar ratio of 1: 2 at a temperature and supply of butyl alcohol 0, 8 l and hydrogen 36O-42O l per 1 liter of catalyst per hour. In this way, butyl alcohol which is formed during the conversion of aldehyde oil can also be converted to 2-ethylhexanol. EXAMPLE 2 A catalyst is prepared containing, in wt%: Copper oxide 50; Titanium dioxide SOAP 625 MP 15% solution of titanium sulfate (III) in sulfuric acid, is oxidized as in Example 1, 625 ml of distilled water is added and titanium hydroxide is precipitated with a solution of sodium hydroxide to pH 3, 430 MP of alkali solution is precipitated. The precipitate of titanium hydroxide is treated with a solution of 151 g of Cd (LO,) in 96 O ml of water and all the catalyst preparation operations described in Example 1 are carried out. In tab. 3 shows the composition and outputs

Reaction products

2-Etoggeksanop

2 Ethylhexanal

Oil aldehyde

Butyl alcohol

Butyl butyrate

Water condensate

VAT residue (

Composition, wt.%

33 3 2

34

four

ten

14

table 2

Reaction products

2-Ethylhexanol 2-Ethylhexanal Aldehyde Oil Butyl Alcohol Butyl Butyrate Water Condensate Vat residue

Claims (2)

Formula of Invention What | With a simplified process, the method of producing 2-ethylhexanopa - weight%: tapitic condensation and hydrogenating oil aldehyde with elevated titanium dioxide O-60 temperature, characterized by that. CopperO4O-50, T a b l and c a 3 Composition, wt.% 32 2 1 39 4 8 13 55 catalyst is of the following composition, 7 7494178 The process is conducted at a temperature. USSR author's certificate 250C and supply of aldehyde oil or № 18888, cl. C O7 C 31 / OZ, 1957. butyl alcohol 0,7-O, 8 li hydrogen 360-420 liters per 1 liter of catalyst per hour. 2. USSR author's certificate Sources of information fo 478830, cl. C 07 S 29/16 1972 taken into account in the examination (prototype).