SU1572993A1 - Method of producing ammonium tripolyphosphate - Google Patents

Abstract

The invention relates to the technology of polyphosphate production, in particular ammonium tripolyphosphate, which can be used as a concentrated fertilizer, fertilizer additive for leveling the composition, additives to synthetic detergents, as a catalyst for cracking oil products, the active component of fire extinguishing agents, the original product of the synthesis of polyphosphates. The purpose of the invention is to simplify and speed up the process. The essence of the invention is that the precipitation is carried out from a solution of potassium tripolyphosphate with a saturated solution of ammonium acetate at 15 - 25 ° C and a molar ratio of 1: (66 - 154), 1: (17.6 - 35.4), 1 :( 26.4 - 35.2) for 0.2, 1 and 2M solutions of potassium tripolyphosphate, respectively. The obtained crystals are separated from the solution in a day, washed with ethanol and dried. 1 hp f-ly, 3 tab.

Description

This invention relates to a process for the production of polyphosphates, in particular ammonium tripolyphosphate of the formula (NH4) 5P30, which can be used as a concentrated fertilizer, fertilizer additive for leveling out additives, additives to synthetic detergents, as a catalyst for the cracking of petroleum products, the active component of fire extinguishing agents, the original product of the synthesis of polyphosphates.

The aim of the invention is to simplify the method and reduce its implementation time.

Example. To 50 ml of a filtered solution of potassium tripolyphosphate containing 4.8 g of anhydrous potassium tripolyphosphate (0.2 M solution), at 20 ° C, 100 ml of ammonium hydrochloric acid ammonium solution (d 1.099 g / cm 8.8 M solution) are poured, mixed and after a day the formed crystals are separated on a Buchner funnel, washed with ethanol, dried in air for a day, weighed, analyzed. The yield is 3.55 g, which is 98.3.

According to the results of chemical, chromatographic and X-ray phase analyzes, the composition of the product corresponds to the formula (NH4) 5P30.0 H20.

The experiments were carried out as described in the example, only the ratios of the initial reagents were changed.

The results are shown in Table. one.

SL

N

N9

WITH qD 00

From the data in Table 1, it can be seen that for a 0.2 M solution of K5P, 010 with a molar ratio of less than 66, the yield of the finished product is lower (only k2%, i.e., it is impractical to precipitate under such conditions). I5 - the yield of the finished product does not increase, so there is no point in increasing the number of jAc added.

For a 1 M K5P 010 solution, the ratio is less than 17.6, the product is isolated with an admixture of the ammonium potassium double salt. With a ratio of more than 35.2-5, the product yield does not increase, so there is no point in increasing the amount of added precipitant. .

For a 2 M solution with a ratio less than 26, and the product precipitates - 20 s with an admixture of the ammonium potassium double salt. With a ratio of more than 35.2, the product yield does not increase, so it makes no sense to increase the amount of precipitating reagent. 25

Thus, the optimal molar ratios of the starting reagents are the intervals for 0.2 M K5P30, CH3COONIU 1: (66-151); for 1 M K5P; o10 KVR, 3Q: CH, COONH4 1: (17.6-35.2); for 2 M K5PiiO, 0 KSPS0№: CH3COONH4 1: (26.4-35.2).

The results of experiments to obtain the target product - (Ш4) 5Р 010-Н20 in the temperature range (15-25) ° С are given in table. 2

From tab. 2 that at a temperature of less than T5 ° C, (NtI4) eF, Q k2H20 is co-precipitated with the target product, and at a temperature of more than 25 ° C, according to chromatographic analysis, the target product is clogged with tripolyphosphate degradation products — ammonium ortho- and pyrophosphates.

In tab. 3 shows the comparative characteristics of the target products obtained by the proposed and known methods.

35

45

five

Q

Q

five

five

Thus, the advantages of the proposed method are that, using a solution of potassium tripolyphosphate instead of sodium tripolyphosphate, it is possible to minimize the amount of water needed to dissolve the starting material, reduce the filtering process of this solution by 60 minutes.

In addition, the proposed method allows synthesis without resorting to the use of ion exchange columns. In this case, the process is carried out in 6 stages, while, in a known method, the process of producing ammonium tripolyphosphate proceeds in 8 stages, this ensures a reduction in the number of service personnel, makes it possible to free up space for other industries, and greatly simplifies and accelerates the process of obtaining ammonium tripolyphosphate more than 30 hours

Claims (2)

1. A method of producing ammonium tripolyphosphate, including the interaction of an alkali metal tripolyphosphate with ammonium acetate, filtering the precipitate of the desired product, washing it with ethanol, and drying, in order to simplify and speed up the process, the alkali metal tripolyphosphate is used as tripolyphosphate potassium, the interaction is carried out at 15-25 ° C. 2. A method according to claim 1, characterized in that potassium tripolyphosphate is used with a concentration of 0.2-2 M, and the reaction is carried out at a molar ratio of tripolyphosphate: ammonium acetate, equal to 1: (66-, for a 0.2 M solution of tripolyphosphate , 1: (17.6-35,) for 1 Mi 1:: (2bL 35.2) for 2 M solutions, respectively. Table 1 Taken ratio of initial components K5P5010 and UCA volume I molar 1 M solution of potassium tripolyphosphate 1: 0.5 1: 1 1: 4.4 1: 8.8 1: 1.5 1: 13.2 1: 2 1: 17.6 2 M solution of potassium tripolyphosphate 1: 5 1:22 1: 5.5 1: 24.2 1: 6 1: 26.4 Product yield,% of theoretically expected Impurity of ammonium double salt - potassium 103 Impurity of ammonium double salt -cali 88 100% of the target product 97 100 100 100 96 97 Impurity double salts of ammonium -cali 96 Impurity of ammonium potassium double salt 100 100% of the target product 1: 21: 8812 (NHjjP O ,,, H70 + (No.),), P, 0CHO g 2H20 Chromatographic tripolyphosphate 1: 31: 26, t13 On the radiograph of the product 1: 71: 30,812 diffraction is present maximum at 26 9 °, characteristic of the phase (NH,) ,; P, 010 Table 3 The test results by the method Ate food operations the famous 16 g of sodium tripolyphosphate are dissolved in 4 ml of water and filtered for 75 minutes. 27 h 3 h Get 240 ml of solution 480 ml of ammonium acetate are added to 240 ml of solution for 1 day. table 2 proposed , 3 g of potassium tripolyphosphate are dissolved in 30 ml of water and flooded for 15 minutes. 64 ml of ammonium acetate are added to 32 ml of solution for 1 day.