DE2939525A1 - Calcium phosphate catalyst prodn. for decomposition of 1,3-dioxane(s) - by pptn. of calcium phosphate in presence of ammonia,then steaming in presence of conditioning agent - Google Patents

Abstract

Ca phosphate catalyst is prepd. by reacting a water soluble Ca salt with a water-soluble phosphate in NH4OH; recovering the ppt., shaping and drying; and firing at 450-600 deg.C in steam contg. H3PO4 or an org. cpd. (I) or H3PO4 and air or (I) and an inert gas. (I) is an aldehyde, an alcohol, a diene or an O-contg. heterocyclic. The reaction between the Ca salt and phosphate is NH4OH is carried out at a mole ratio of 1.5:1 if no H2PO4 treatment is used; or 1.5-5:1 if the reaction mixt. is treated with an H3PO4 soln. to pH 5.0-7.0, pref. 5.5-6.0. Used esp. for conversion of 4,4-dimethyl-1,3-dioxane into isoprene. It can also be used for dehydration of alcohols. Catalyst has high activity and high selectivity; it also has a long service life and low coking tendency.

Description

description

The invention relates to the production of catalysts, for example are used in the isoprene production from isobutylene and formaldehyde, in particular a process for producing a calcium phosphate catalyst for decomposing the 1,3-Dioxanes, in particular 4,4-dimethyl-1,3-dioxane (also called DMD) Isoprene and for the dehydration of alcohols A process for the production is known of phosphates of croup II, which are used as catalysts for the selective cleavage of the - C - O bonds in the organic compounds, including the cleavage of 4,4-dimethyldioxane-I, 3 to isoprene as well as for the dehydration of alcohols can be used by precipitation of neutral metal phosphates of group II from aqueous solutions of the salts the same and water-soluble salts of phosphoric acid and subsequent separation of the rebound Washing and shaping of the catalyst granulate from the paste obtained (US-PS 3872216).

The catalysts prepared by the above process have a low selectivity (78-82 mol%) and a low activity, the one low volume velocity of the DMD throughput (0.7 h-1) and a high operating temperature (approx. 375 ° C) conditional.

Selectivity is expressed as the amount of that formed, expressed in moles Isoprene is defined as the amount of D2D converted, expressed in moles.

The selectivity quantity is determined by the composition and the structure of the catalyst as well as the conditions of its operating process.

When the selectivity increases, the gain in one Unit of the finished product, for example 1 t of isoprene, required amount of raw material away. The insufficient selectivity of the produced by the known process Catalyst causes the large consumption of raw materials, which is about 2.10-2.25 kg DMD 1 kg isoprene.

The activity of calcium phosphate catalysts depends on their acidity which is determined by the number and strength of the active centers, and stands with the degree of DMD conversion.

The DMD conversion rate is a ratio of the amount of DMD converted to the total amount conveyed (expressed as a percentage).

At the moment it is known to keep Xin in which the calcium phosphate catalysts by converting calcium and phosphoric acid salts in aqueous ammoniacal is Chen medium, washing, drying and thermal treatment of the precipitate in the superheated steam or steam / air mixture produced at elevated temperatures (U.S. Patent 3,846,338). The catalysts produced by the known process show low activity.

In addition, the calcium phosphate catalysts obtained in the manner described have low effectiveness (0.3-0.4 t isoprene per 1 m³ of the catalyst per hour) on.

The effectiveness of a catalyst depends on its activity, selectivity and {volume velocity of the starting components throughput.

In the known method, the thermal treatment takes place at increased temperatures, which leads to overheating of the heat carrier up to 650-8000C and thereby the increased energy expenditure and the use of the special thermostable Requires materials of the reaction apparatus suitable for the production of catalysts.

Another disadvantage of that produced by the known process Catalyst consists in its relatively short life (250 h).

The life of a catalytic converter depends on many parameters, in particular on its composition and structure, activity, operating temperature and coke deposition. The coke deposit is understood to be the formation of coke on the Catalyst surface area in DGD implementation, expressed as the percentage relationship the amount of coke deposited (in moles) versus the amount of DMD reacted (in moles) is.

Apart from the advantages of the known method of manufacture a calcium phosphate catalyst has not yet been an industrial production process developed, as there is no catalyst with the selectivity required for production and stability is invented.

The SrfinduBg is based on the task, through the changes in the process engineering manufacturing conditions an increase in activity, Effectiveness and selectivity and lifetime of the catalyst together with the To achieve a reduction in coke deposits in the DMD implementation.

The given task becomes by developing a method Production of a calcium phosphate catalyst by converting calcium salts and phosphoric acid salts in the aqueous ammonia medium, separation from the reaction mixture of the precipitate formed, its shaping, drying and thermal treatment dissolved in a water vapor atmosphere at elevated temperatures at which according to the invention the thermal treatment at temperatures from 450 to 600 ° C in the presence of Water vapor with phosphoric acid or aldehyde or with an oxygen-containing heterocyclic compound, or mixed with alcohol, or with diolefin, or in the presence of water vapor mixed with inert gas or air and phosphoric acid is, or in the presence of water vapor, which with inert gas and aldehyde or

with an oxygen-containing heterocyclic compound, or

Alcohol or diolefin has been mixed *.

It is recommended to use formaldehyde or acetaldehyde as the aldehyde.

It is useful as the oxygen-containing heterocyclic compound To use methylhydropyrene or methylenetetrahydropyran.

It is also advisable to use trimethylcarbinol (2-methyl - 2-propanol) as the alcohol or isopropenyl ethyl alcohol to be used.

It is advisable to use isoprene or piperylene (1,3 - pentadiene) as the diolefin to use.

It is recommended to implement calcium salts and phosphoric acid salts to be carried out in an aqueous-ammoniacal medium at a molar ratio of 1.5: 1.

It is preferable to implement calcium salts and phosphoric acid salts in an aqueous-ammoniacal medium with a molar ratio of the starting components 1.5-5.0: 1 and the reaction mixture formed with the phosphoric acid solution to be treated up to the pH value 5.0-7.0.

It is useful to mix the reaction mixture with the phosphoric acid solution to be treated up to the pH value 5.5-6.0.

Carrying out the process for the preparation of calcium phosphate catalyst under the conditions mentioned above, a catalyst with high selectivity (86.0-87.5 Moles of high activity (96-97%) and low coke deposition (less than 1 mole%) were obtained.

The method for making the calcium phosphate catalyst is carried out as follows.

As starting reagents, the solutions of calcium salts, for. B. of calcium chloride, and the solutions of phosphoric acid salts, e.g. B. of diammonium phosphate, Disodium phosphate et al.

taken. The solution of phosphoric acid salt is made before the implementation an ammonia solution with the calcium salt solution for the purpose of setting the pH value admitted.

The solutions of calcium and phosphoric acid salts gradually become into a stirred tank with continuous stirring of the resulting suspension poured together. The molar ratio of the calcium salts and the phosphoric acid salts is 1, i5: 1. The implementation is also at the molar ratio of the starting component where 1.5-5.0: 1 (preferably 2.5: 1) is possible. In this case, the reaction mixture formed will with the solution of phosphoric acid up to the pH value 5.0-7.0 (preferably 5.5-6.0) treated.

The above-mentioned range of the proportions of the calcium and phosphoric acid salts and the pH of the reaction mixture is guaranteed the required structure and composition of the resulting catalyst.

The precipitate formed is filtered or any other known method separated from the calcium salt anion with distilled water Washed free by the known method and granulated at one temperature dried from 110 - 1400C, whereby the starting calcium phosphate is obtained, which it is then introduced into a reaction apparatus.

The reactor is a quartz tube with a diameter of 20-26 mm. It's put in an electric furnace, and the one in his Interior The catalyst located is at 400-600 ° C with steam with the addition of phosphoric acid or an organic compound is thermally treated.

As an organic compound that is added to the water vapor, Formaldehyde, acetaldehyde, methyldihydropyran $ (MDHP), methyllenetetrahydropyran (MTIIP), Trimethylcarbinol (TMK), isopropenyl ethyl alcohol (IPÄA), isoprene or piperylene be used.

When making a calcium phosphate catalyst without machining of the reaction mixture with phosphoric acid solution, the thermal treatment is preferred made at 450 ° C.

If the manufacture involves a stage of treatment of the suspension with Including phosphoric acid to a pH of 5.0-7.0, the thermal treatment takes place preferably at 500 ° C.

The thermal treatment can also be done with water vapor with the addition inert gas, in particular nitrogen, argon and others. as well as air (if the water vapor the phosphoric acid is added).

The .Wasserdampf is with the volume velocity of 1.0-2.0 h-1 supplied.

The amount of phosphoric acid present in the catalyst at thermal Treatment is fed is 0.05-0.25 g ae 1 kg of the catalyst per hour.

The treatment lasts 2-50 hours, preferably 20-30 hours.

The volume rate of the organic compound addition is 0.7-1.5 h-1, preferably 1.0 h-1.

After treating the catalyst with the steam, mixed with any of the organic compounds mentioned gen or the water vapor mixed with the inert gas and any of the compounds mentioned the catalyst is with the steam / air mixture at 450-600 ° C, preferably 500-550 ° C regenerated to burn off the coke deposited on the catalyst surface. The air is at the volume velocity of 300-700 h, the water vapor - 1.0-2.0 h-1 supplied.

The calcium phosphate catalyst produced has the following Properties: DMD conversion - 96-97%, selectivity -86.0-87.5 mol%, coke deposition - less than 1%.

Below are typical examples that address certain aspects illustrate the invention and its features and advantages to the clearest Express.

Example 1 As starting components for the preparation of the catalyst if you take 1.78 1 calcium chloride solution (calcium chloride content 101.892 g per 1 liter) and 1.608 1 diammonium phosphate solution (diammonium phosphate content 51.02 g per 1 liter), with the last immediately before the reaction an ammonia solution (152.15 g per 1 liter) based on the ratio of 2.33 mol of ammonia per 1 mol of diammonium phosphate is admitted. The calcium chloride solution and the diammonium phosphate solution are placed in a stirred tank gradually poured. The solutions are poured together within 2 hours while continuously stirring the resulting suspension. The implementation is progressing with the practically constant volume ratio of the solutions, the necessary molar ratio the calcium and phosphoric acid salts in the amount of 2.5: 1 guaranteed the pH of the suspension is in the range 9.0 + 0.05. The resulting suspension treated with 150 ml of phosphoric acid at a concentration of 281.26 g per 1 liter to reduce> <the pH value to 5.75. The precipitate obtained is separated from the solution by filtering, from the chlorine ion with the distilled Washed free of water, granulated and dried at a temperature of 120 ° C. That by it Calcium phosphate produced in an amount of 24 cm is poured into one from a quartz tube entered with the diameter 20-26 mm existing reaction apparatus. The reaction apparatus is placed in an electric furnace. The catalyst creates water vapor 4000C with the addition of phosphoric acid, based on the ratio 0.2 g of phosphoric acid passed per 1 kg of the catalyst within 30 hours.

The catalyst produced in this way is used in the LMD cleavage tested in the steam atmosphere. The DMD gap o process is at the average Temperature of 320 C and the atmospheric pressure carried out within 2 hours.

DMD is used in an amount of 24 cm³ / h and water in an amount of 48 cm³ / h conveyed, which is the volume speed of the DMD throughput of 1.0 h-1 and corresponds to the DMD dilution with steam in a ratio of 1: 2.

The conversion cycle is followed by a regeneration cycle, which consists of that the deposited coke is burned off every 2 hours of catalyst operation.

The regeneration cycle is carried out at 425 ° C with the addition of 48 cm³ water and 16800 cc of air. The catalyst is then by means of gas-liquid chromatography analyzed.

The amount of coke deposited is determined according to the known method. The test results of the catalyst are shown in Table 1 below.

Example 2 The calcium phosphate catalyst is based on that in example 1 described manner.

The thermal treatment of the starting calcium phosphate is based on the carried out at 50000 as described in Example 1.

The test of the catalyst produced runs on that in the example 1 described way.

The test results of the catalytic converter are shown below Table 1 listed.

Example 3.

The calcium phosphate catalyst is based on that described in Example 1 Way made.

The thermal treatment of the starting calcium phosphate is based on the carried out in the manner described in Example 1 at 6000C.

The test of the catalyst produced runs on that in the example 1 described way.

The test results of the catalytic converter are shown below Table 1 listed.

Example 4 The calcium phosphate catalyst is based on that in example 1 described manner.

The thermal treatment of the starting calcium phosphate takes place at 5000C with steam with the addition of phosphoric acid based on the ratio 0.2 g of phosphoric acid per 1 kg of catalyst 3 per hour and of nitrogen in the amount of 4800 cm, which corresponds to a gas volume velocity of 200 h-1.

The test of the catalyst produced runs on that in the example 1 described way.

The test results of the catalytic converter are shown below Table 1 listed.

Example 5 The calcium phosphate catalyst is based on that in example 1 described manner.

The thermal treatment of the starting calcium phosphate takes place at 5000C with steam with the addition of phosphoric acid based on the ratio 0.2 g of phosphoric acid per 1 kg of catalyst per hour and the amount of air of 4800 cm3, which corresponds to the gas volume velocity of 200 h ~ 1.

The test of the catalyst produced runs on that in the example 1 described way.

The test results of the catalytic converter are shown below Table 1 listed.

Example 6 The calcium phosphate catalyst is based on that in example 1 described manner.

The thermal treatment of the starting calcium phosphate takes place at 450 ° C with steam with the addition of formaldehyde (7% by weight) within 4 hours.

The steam volume velocity is (taking into account the 7 ew.en aqueous formaldehyde solution) 2.0 h 1.

The prepared catalyst is tested before the combustion of the coke deposited on its surface at 500 ° C with the addition of 48 cm³ / h of water and 16800 cc / h of air.

The test of the catalyst produced runs on that in the example 1 described way.

The results of the testing of the catalyst are shown below Table 1 listed.

Example 7 The calcium phosphate catalyst is based on that in example 1 described manner manufactured.

The thermal treatment of the starting calcium phosphate is 0 to the manner described in Example 6 was carried out at 500.degree.

The prepared catalyst is tested prior to combustion of the coke deposited on its surface to that described in Example 6 Way subjected.

The exam; of the catalyst produced runs on that in the example 1 described way.

The test results of the catalytic converter are shown below Table 1 listed.

Example 8 The calcium phosphate catalyst is based on that in example 1 described manner produced.

The thermal treatment of the starting calcium phosphate @ is based on the in the manner described in Example 6 carried out at 6000C.

The prepared catalyst is tested prior to combustion of the coke deposited on its surface to that described in Example 6 Way subjected.

The test of the catalyst produced runs on that in the example 1 described way.

The test results are shown in Table 1 below.

Example 9 The calcium phosphate catalyst is based on that in example 1 described manner produced.

The essential treatment of the outgangacalcium phosphate takes place at 5000C with steam with the addition of 5 wt. Acetaldehyde in the steam.

The prepared catalyst is tested prior to combustion of the coke deposited on its surface to that described in Example 6 Way subjected.

The test of the catalyst produced runs on that in the example 1 described way.

The test results are given in Table 1 below.

Example 10 The calcium phosphate catalyst is based on the example 1 described manner produced.

The thermal treatment of the starting calcium phosphate takes place at 40,000 with steam with the addition of 7% by weight formaldehyde and nitrogen in the Amount of 4800 cm3 in the water vapor what the gas volume velocity of 200 hours within 4 hours.

The prepared catalyst is tested prior to combustion of the coke deposited on its surface to that described in Example 6 Way subjected.

The test of the catalyst produced runs on that in the example 1 described way.

The test results are shown in Table 1 below.

Example 11 The calcium phosphate catalyst is based on that in Example 1 described manner produced.

The thermal treatment of the starting calcium phosphate takes place at 5000C with steam with the addition of 31.4% by weight MDHP within 2 hours. The volume rate of the MnRP feed is 1.0 h-1, that of the water vapor or 2.0 h 1.

The prepared catalyst is tested before the combustion of the coke deposited on its surface to that described in Example 6 Way subjected.

The test of the catalyst produced runs on that in the example 1 described way.

The test results are listed in Table 1 below.

Example 12 The calcium phosphate catalyst is based on that in Example 1 described manner produced.

The thermal treatment of the calcium phosphate takes place within 0 ton 2 hours at 500 C with steam with the addition of 31.6 wt.% MTHP. The volume velocity the M2MP feed is 1.0-1, that of the steam 2.0. The catalyst produced is used prior to testing the combustion of the coke deposited on its surface in the manner described in Example 6.

The test of the catalyst produced runs on that in the example 1 described way.

The test results are shown in Table 1 below.

Example 13 The calcium phosphate catalyst is based on that in Example 1 described manner produced.

The thermal treatment of the busang calcium phosphate with subsequent The deposited coke is burned off at 0 400 C in the manner described in Example 11 Way.

The catalyst obtained is tested as in Example 1.

The test results are shown in Table 1 below.

Example 14 The caltium phosphate catalyst is based on that in Example 1 described manner produced.

The thermal treatment of the starting calcium phosphate with subsequent The deposited coke is burned off at 600 ° C to the im Example 11 described manner.

The catalyst obtained is tested as in Example 1.

The test results are shown in Table 1 below.

Example 15 The calcium phosphate catalyst is based on that in Example 1 described manner produced.

The thermal treatment of the initial calcium phosphate takes place within 2 hours at 500 ° C with steam with the addition of 31.4 wt.% MDHP and nitrogen in the amount of 4800 cm³, which is the gas volume velocity of Corresponds to 200 h.

The catalyst obtained is prior to testing the combustion of the coke deposited on its surface in the manner described in Example 6 subjected.

The test of the catalyst produced runs as in the example 1 from.

The test results are shown in Table 1 below.

Example 16 The calcium phosphate catalyst is based on that in Example 1 described manner.

The thermal treatment of the starting calcium phosphate takes place within of 6 hours at 5000C with steam with the addition of 28.3% by weight, TMK. The volume velocity the TMK supply is 1.0 h-1, that of the water vapor or 2.0 h-1 (on PlUssiOigkeit based).

The prepared catalyst is tested prior to combustion of coke deposited on its surface in the manner described in Example 6 The test of the catalyst produced is carried out as in Example 1.

The test results are listed in Table 1 below.

Example 17 The calcium phosphate catalyst is written on @ e @ B @@ 1b Way made.

The thermal treatment of the output sphates takes place within b 6 hours at 5000C with the addition of 30.9% by weight of isopropenyl ethyl alcohol (IPÄA). @@@ Volume velocity of the IPÄA feed is 1.0 h-1, the @ water vapor corresponds to 2.0 h-1 (based on liquid).

The prepared catalyst is tested before the combustion of the coke deposited on its surface to that described in Example 6 Way subjected.

The test of the catalyst produced runs as in the example 1 from.

The test results are shown in Table 1 below.

Example 18 The calcium phosphate catalyst is based on that in Example 1 described manner.

The thermal treatment of the starting calcium phosphate with subsequent Burning of the deposited coke is successful those in example 16 described way at 4000C.

The test of the catalyst produced runs as in the example 1 from.

The test results are shown in Table 1 below.

Example 19 The calcium phosphate catalyst is based on that in Example 1 type described and tracks are established.

The thermal treatment of the; tusGang calcium phosphate with subsequent The deposited coke is burned off in the manner described in Example 16 at 600 ° C.

The test of the catalyst produced runs as in the example 1 from.

The test results are shown in Table 1 below.

Example 20 The calcium phosphate catalyst is based on that in Example 1 prepared manner described, bie thermal treatment of the starting calcium phosphate takes place within 6 hours at 5000C with steam with the addition of 28.3 Weight% TMK and nitrogen in the amount of 48CO cm3, which is the gas volume velocity of 200 h-1.

The prepared catalyst is tested prior to combustion of the coke deposited on its surface to that described in Example 6 Way subjected.

The test of the catalyst produced runs on that in the example 1 described way.

The test results are shown in Table 1 below.

Example 21 The calcium phosphate catalyst is based on that in the example 1 described manner.

The thermal treatment of the starting calcium phosphate takes place within of 9 hours at 450 ° C. with steam with the addition of 25.4% by weight isoprene. the The volume speed of the isoprene feed is 1.0 hl, that of the water vapor 2.0 h-1 (based on liquid).

The prepared catalyst is tested prior to combustion of the coke deposited on its surface to that described in Example 6 Way subjected.

The test of the catalyst produced runs on that in the example 1 described way.

The test results are shown in Table 1 below.

Example 22 The calcium phosphate catalyst is based on that in example 1 described manner produced.

The, thermal treatment of the initial cylcium phosphate with subsequent The deposited coke is burned off in the manner described in Example 21 and way at 500 ° C.

The test of the catalyst produced runs on that in the example 1 described way.

The test results are shown in Table 1 below.

Example 23 The caldium phosphate catalyst is based on the example 1 described manner produced.

The thermal treatment of the starting calcium phosphate with subsequent The deposited coke is burned off in the manner described in Example 21 at 6000C.

The test of the catalyst produced runs as in the example 1 from.

The test results are listed in Table 1 below.

Example 24 The calcium phosphate catalyst is based on that in Example 1 described manner.

The thermal treatment of the starting calcium phosphate takes place within of 9 hours at 500 ° C with steam with addition 3 of 25.4 wt.% Isoprene and Nitrogen in the amount of 4800 cm, what what the what-folumende-speed of Corresponds to 200 h.

The catalyst obtained is prior to testing the combustion of the coke deposited on its surface in the manner described in Example 6 subjected.

The test of the catalyst produced runs on that in the example 1 described way.

The test results are shown in Table 1 below.

Example 25 The calcium phosphate catalyst is based on that in Example 1 described Way made.

The thermal treatment of the starting calcium phosphate takes place within of 9 hours at 5000C with steam with the addition of 25.3% by weight of piperylene. the The volume rate of the piperylene feed is 1.0 h 1, that of the water vapor 2.0 h-1.

The prepared catalyst is tested prior to combustion of the coke deposited on its surface to that described in Example 6 Way subjected.

The test of the catalyst produced runs on that in the example 1 described way.

The test results are shown in Table 1 below.

Example 26.

1.18 l of a calcium chloride solution are used as starting reagents C calcium chloride content 99.8 g per 1 liter) and 2.0 l of a disodium phosphate solution (Disodium phosphate content 50.21 g per 1 liter), the last being immediately before the reaction an ammonia solution (130 g per liter) based on the ratio 4.3 moles of ammonia per 1 mole of disodium phosphate is added. In a stirred tank Calcium chloride and disodium phosphate solutions become gradually within 2 hours poured together under the continuous teaching of the resulting suspension. The reaction takes place at the constant volume ratio of the solutions that the necessary Molar ratio of calcium chloride and disodium phosphate of 1.5: 1.0 guaranteed, the pH of the suspension is in the range 9.0 + 0.05. The precipitate obtained is separated from the chlorine ion by filtering washed with distilled water, granulated and at temperature 1200C dried. The thermal treatment of the phosphate takes place in the example 1 described manner at 500 ° C.

The test of the catalyst produced runs on that in the example 1 at the reaction temperature of 3750C.

The test results are shown in Table 1 below.

Example 27.

The catalyst is in the manner described in Example 26 and Way made.

The thermal treatment of the calcium phosphate takes place on the im Example 1 described manner at 400 ° C.

The test of the catalyst produced runs on that in the example 26 described.

The test results are listed in Table 1 below.

Example 28.

The catalyst is in the manner described in Example 26 and Way made.

The thermal treatment of the calcium phosphate takes place on the im Example 6 described manner. The manufactured catalyst is used prior to testing subjected to the burning off of the coke deposited on its surface according to Example 6.

The catalyst is tested as in Example 26.

The test results are given in Table 1 below.

Example 29.

The catalyst is in the manner described in Example 26 and Manufactured way, The thermal treatment of the calcium phosphate takes place on the as described in Example 13. The manufactured catalyst is used prior to testing subjected to the burning off of the coke deposited on its surface according to Example 6.

The test of the catalyst produced is as in Example 26 carried out.

The test results are given in Table 1 below.

In the description of the above examples for execution In the present invention, the specific terms have been used in their narrower sense used, it should be noted, however, that this invention is by no means on the accepted concepts are limited and that every concept covers all equivalents, fulfilling the same functions and for solving the the same tasks are needed.

Although the invention with reference to the preferred typical Embodiments is described above, the specialists must be in be clear that the execution of the procedure is subject to insignificant changes can be without departing from the essence of the invention.

All changes and modifications do not apply to deviating and than from the nature and scope of the invention as defined in the patent claims includes.

RESULTS OF THE CATALYST TESTS IN THE DMD SPLIT PROCESS Operating temperature: 3200C Volume rate of DMD throughput 1 h l DMD dilution with H20: 1: 2 Table 1 Catalysts characteristic values according to DMD conversion selectivity coke deposition games degree,% mole% mole% 1 2 3 4 1 97.5 86.9 1.53 2 97.2 87.2 0.84 3 96.0 87.5 0.56 4 97.4 86.9 1.04 5 97.3 86.8 1.09 1 2 3 4 6 97.5 87.0 1.50 7 97.3 87.5 0.54 8 96.0 87.3 0.47 9 97.4 87.3 0.61 10 97.4 86.9 1.58 11 97.2 - 87.3 0.65 12 97.2 87.2 0.69 13 97.4 86.9 1.60 14 95.9 87.5 0.48 15 97.3 87.2 0.80 16 97.1 87.0 0.70 17 97.0 87.2 0.68 18 97.5 86.8 1.70 19 95.8 87.4 0.46 20 97.1 86.9 0.74 21 97.4 86.9 1.61 22 96.8 87.1 0.63 23 95.9 87.5 0.56 24 97.0 87.0 0.72 25 96.9 87.3 0.66 26 94.7 87.2 0.59 27 95.2 86.4 1.78 28 95.0 86.6 0.52 29 94.8 87.0 0.50 30 94.7 86.8 0.52 31 94.9 86.6 0.58

Claims (8)

Oleg Efimovich Batalin Arkadij Samuilovich Dykman Izrail Markovich BelgorodskiJ Oleg Alexeevitsch Ostrouchov Lyudmila Vasiljevna Golovko Vladimir Ivanovich Nevstruev Anatolij Ivanovich Lukaschov PROCESS FOR MANUFACTURING A CALCIUM PHOSPHATE CATALYST SATOR Claims 1. Process for the preparation of a calcium phosphate catalyst by Conversion of calcium and phosphoric acid salts in an aqueous ammaniacal medium, Separation from the reaction mixture of the precipitate formed, its forms, Drying, thermal treatment in a steam atmosphere at an elevated temperature, d a d u r c h g e -k e n n n z e i c h n e t that the thermal treatment at 400 up to 6000C in the presence of steam, which is mixed with phosphoric acid or aldehyde, or with an oxygen-containing heterocyclic compound, or with alcohol, or Diolefin is mixed, or water vapor mixed with inert gas or air and phosphoric acid is mixed, or water vapor, the one with inert gas and aldehyde, or with an oxygen-containing heterocyclic compound, or Alcohol, or diolefin mixed, takes place. 2. The method according to claim 1, d a d u r c h g e -k e n n z e i c h n e t that the aldehyde used is formaldehyde or acetaldehyde. 3. The method of claim 1, d a d u r c h g e -k e n n z e i c h n e t that the oxygen-containing heterocyclic compound methylhydropyran or Methylentetrahydropyran is used. 4. The method according to claim 1, d a d u r c h g e -k e n n z e i c h n e t that trimethylcarbinol or isopropenyläthylkarbinol used as alcohol will. 5. The method of claim 1, d a d u r c h g e -k e n n z e i c h n e t that the diolefin isoprene resp. Piperylene is used. 6. The method according to claims 1 to 5, d a d u r c h g e k e n n z e i c h n e t that the implementation of calcium salts and phosphoric acid salts in the aqueous-ammoniacal medium with a molar ratio of the starting components 1.5: 1 is carried out. 7. The method according to claims 1 to 5, d a d u r c h g e k e n n z e i c h n e t that the implementation of calcium salts and phosphoric acid salts in the aqueous-ammoniacal Medium at a molar ratio of the starting components 1.5 to 5.0: 1 carried out and the reaction mixture formed with the phosphoric acid solution is treated up to the pH value 5.0 to 7.0. 8. The method according to claim 7, d a d u r c h g e -k e n n z e i c h n e t that the reaction mixture with the phosphoric acid solution down to the pH value 5.5 to 6.0 is treated.