SU1308556A1 - Method of producing concentrated titanium and magnesium phosphate - Google Patents

Abstract

This invention relates to a process for the preparation of catalysts, in particular a double phosphorus salt of titanium and magnesium of composition 0.5 k. The purpose of the invention is to increase the specific surface of the catalyst and accelerate the process of its production. The method is carried out by the interaction of a hydrochloric solution of titanium tetrachloride with monosodium phosphate at a molar ratio of 1: (7–10), with heating to 30-70 ° C in the presence of 30-45% vol. Ethyl or propyl alcohol. The product isolated by filtration is washed, dried and calcined at 400-500 s. The specific surface of the obtained catalyst reaches 200, the synthesis time is 3-4 hours. f-ly. with OS) ate JV C5

Description

1130855

This invention relates to a process for the preparation of catalysts, catalyst carriers, fillers, in particular titanium phosphorus double salt.

and magnesium of the composition 0,5MgO-TiOg PjOj X 6H (, 0.

The purpose of the invention is to increase the specific surface area of titanium double phosphate, and magnesium and accelerate the process of its production.

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EXAMPLE 3. The method is carried out as in example 1, only 58 g of monosubstituted magnesium phosphate (the ratio (H2O) 2 1:10) is added to a solution of titanium tetrachloride, then 90 ml (45 ml) are added. .%) ethyl alcohol. The suspension is stirred at 70 ° C. The synthesis time is 4 hours. The yield of the target product is 6.6 g, the specific surface of the catalyst is 195. .

EXAMPLE 4. The method is carried out by reacting a hydrochloric acid solution of titanium tetrachloride with monosubstituted phos-, 5 py 3, only propylene alcohol Ti HgCHjPOy) 2 equal to 1; (7-10), when the amount of 40 vol.% (80 ml). Heating time 30-70

and in the presence of alkanols (ethyl or pro-alcohol) in an amount of 30-45% by volume. The target product isolated by filtration is washed, rectified and calcined at 400-500 C. According to chemical analysis, the composition of the obtained product is 0.5MgO-TiO -P205--6H20. Its specific surface area is measured in a known manner. The activity of the catalyst obtained is determined by the reaction of dehydrating cyclohexanol to cyclohexene.

Example 1. To 200 ml (0.96 g of Ti) hydrochloric acid (0.1 M HC1) 0.1 M solution of titanium tetrachloride, 41 g of monosodium phosphate in the form of a solid salt are added. The molar ratio of Ti () 2 is 1: 7 (Ti). The mixture is stirred until complete dissolution of the magnesium phosphate, then 60 ml of ethyl alcohol (30% by volume) are introduced and heated to 70 ° C. The resulting suspension is stirred for 3 hours. The precipitate is filtered, drained under pressure, dried in air and calcined at 400 ° C .

precipitation 4.ch. The output of titanium double phosphate and magnesium is 6.5 g, specific

20

the surface of the resulting phosphate.

Carrying out the precipitation process in the presence of alcohols accelerates the formation of double phosphates due to the salting out effect. is he

25 due to the fact that polar alcohol molecules block excess phosphate ions by ion-dipole interaction, as a result of which the solubility of double phosphate decreases. At the same time in everything

30 of the volume of the initial spread. A precipitate of homogeneous phase composition is formed. The high uniformity and dispersion of the granulometric composition is also explained by the superficially active properties of the spiote, which prevents the aggregation of the precipitated

particles.

With the introduction of less than 30% by volume of alcohol into the reaction mixture, the quality indicators of the product deteriorate and the synthesis time increases. An increase in the amount of alcohol in the 45 vol.% Mixture is impractical because it does not affect the quality and speed of the synthesis of double 40

With the introduction of less than 30% by volume of alcohol into the reaction mixture, the quality indicators of the product deteriorate and the synthesis time increases. An increase in the amount of alcohol in a mixture of 45 vol.% Is impractical because it does not affect the quality and speed of the synthesis of double-output double phosphate 6.9 g, the specific surface of the obtained phosphate j phosphate. Replacing alcohol with carboxy-185. Ammonium in the reaction mixture when used — at 200 ml (0.96 g leads to the formation of titanium phosphate Ti) hydrochloric acid (0.1 M HC1) 0.1 M non permanent composition. When a titanium tetrachloride solution ratio is added (H2P04.) 2, 52 g of phosphate monosubstituted is not appropriate, the reduction in the form of a solid salt is also observed (: ROI of the yield and quality of the target pro 1:18). The ratio of () 2 1: 9. The mixture is stirred until the phosphate is completely dissolved and 80 ml are introduced.

duct.

The interval of permissible synthesis temperatures is 30-70 ° C.

(40 bb.%) Of ethanol followed by stirring at a temperature below 30 ° C, the suspension slowly (more than 20 hours), with heating up to. Time precipitation 4h. Further operations are similar to example 1.

at temperatures higher than 70 ° C, hydrolysis of dissolved titanium with the formation of titanium dioxide is observed.

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The yield of double phosphate is 6.6 g, the specific surface area of the resulting phosphate is 200 m2 / g.

EXAMPLE 3. The method is carried out as in example 1, only 58 g of monosubstituted magnesium phosphate (the ratio (H2O) 2 1:10) is added to a solution of titanium tetrachloride, then 90 ml (45 ml) are added. .%) ethyl alcohol. The suspension is stirred at 70 ° C. The synthesis time is 4 hours. The yield of the target product is 6.6 g, the specific surface of the catalyst is 195. .

Example 4: Conducted as in Example 5, except that 40% by volume propyl alcohol (80 ml) is used as an organic reagent. Time

py 3, only as an organic reagent using propyl alcohol amount of 40 vol.% (80 ml). Time

precipitation 4.ch. The output of titanium double phosphate and magnesium is 6.5 g, specific

the surface of the resulting phosphate.

Carrying out the precipitation process in the presence of alcohols accelerates the formation of double phosphates due to the salting out effect. is he

due to the fact that the polar molecules of the alcohol block the excess phosphate ions by ion-dipole interaction, as a result of which the solubility of the double phosphate decreases. At the same time in everything

the volume of the initial rass.vore is the formation of a precipitate of a homogeneous phase composition. The high homogeneity and dispersion of the granulometric composition is also explained by the surface-active properties of the spiote, which prevents the aggregation of the precipitated

particles.

With the introduction of less than 30% by volume of alcohol into the reaction mixture, the quality indicators of the product deteriorate and the synthesis time increases. An increase in the amount of alcohol in a mixture of 45 vol.% Is impractical because it does not affect the quality and speed of the synthesis of double

phosphate. The substitution of ammonium for ammonium carbonate in the reaction mixture leads to the formation of titanium phosphate of unstable composition. At a ratio (H2P04.) 2 that does not correspond to the indicated one, a decrease in the yield and quality of the target product is also observed.

duct.

The interval of permissible temperatures for conducting the synthesis is 30-70 C.

At temperatures below 30 ° C, the process is slow (more than 20 hours), with

at temperatures higher than 70 ° C, hydrolysis of dissolved titanium with the formation of titanium dioxide is observed.

The proposed method allows to increase the deposition rate of the catalyst by 10-15 times (by a known method it takes 48 hours, and by the proposed 3-4 hours), to increase the uniformity of the final product and its specific surface area up to 200 (By the known method, the specific surface area of the catalyst is 95 ).

Conversion of cyclohexanol to cyclohexene using titanium double phosphate and magnesium as catalyst is 96% (specific surface area of catalyst 200). When using a kapapizator with a surface of 95 (by a known method) in this reaction, the degree of conversion of cyclohexanol is reduced to 51%.

The advantage of the proposed method is also the complete elimination in the synthesis of the consumption of di- cicitic orthophosphoric acid.

Editor M.Blanar

Compiled by V. Vilinska

Tehred V. Kadar Proofreader L. Pat Ai

Order 1767/18 Circulation 456 Subscription VNIIPI State Committee of the USSR

on affairs of inventions and discoveries 113035, Beskva, F-35, 4/5 Raushsk nab.

Production and printing company, Uzhgorod, st. Project, 4

Claims (2)

1. A method of producing titanium and magnesium double phosphate by reacting a hydrochloric acid solution of titanium tetrachloride with a magnesium salt — by heating, precipitating the product in the presence of a chemical reagent, followed by calcining, drying, and calcining the target product, characterized in that specific surface and acceleration of the process, monosodium phosphate is used as a magnesium salt at a ratio of: Mg (H2P04) 2 1 (7-10), and the precipitation is carried out in the presence of 30-75%, of ethyl or propyl alcohol. 2. The method according to claim 1, which is different from the fact that the interaction of the hydrochloric acid solution of titanium tetrachloride with monosodium phosphate is carried out at 30-70 s.