SU1212939A1 - Method of producing mixed phosphate of alkali metal and stannum - Google Patents

Description

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The invention relates to a method for producing an alkali metal and tin mixed phosphate of composition (P04), where M is Li, Na, K, Rb

Cyi (HOCTb of the proposed method consists in TOMs that prepare a mixture of acid phosphate of tin and alkali metal chloride in a ratio of 1: (2-A) molars. The mixture is heated to 600-800 ° C and held in a predetermined mode for 1-3 hours, Cooled. Then mixture washed from soluble products by reaction with water. According to chemical X-ray and thermographic analysis methods, the undissolved precipitates are compounds of the general composition Jl Sn (P04) 3 where and are Li, Na, K, Rb

Example. A mixture of 6 g of Sn (HPO) 2 and 1.64 g of LiCE, at a molar ratio of 1; 2, is heated at 600 ° C for 2 hours. The cooled mixture is washed from the soluble portion with water. The residue is analyzed by chemical methods 5 x-ray and thermographic analyzes of the resulting compound corresponds to the formula LiSnjCPO).

The yield of the product is 97% or 4.96 g.

P li m e p 2. A mixture of 6 g of FIRDS); and 3.28 g Lice (1: 4 mol) is heated at 800 ° C for 1.5 hours. 0: The precipitated mixture is washed from the soluble portion with water. The residue is analyzed by chemical X-ray and thermographic analyzes. The compound obtained corresponds to the formula LiSnj (Р04)

The yield of the product is 97% or 4.95. Example 3. A mixture of 6 g of Sn (HPO) 2 and 3.38 g of MaSe (1: 3 mol) is heated at 600 ° C for 3 hours. The mixture is washed from the soluble part with water. The residue is analyzed by chemical, radiographic and thermographic anahgis. The compound obtained corresponds to the formula

NaSn, (P0 ,,) h

The yield is 98% or 5.16 g. Example 4. A mixture of 6 g of Sni (HP04) 2 and 2.26 g of NaCS (1: 2 mol) is heated for 1 hour. The cooled mixture is removed from the soluble portion with water. The residue is anapicated by chemical, chemical x-ray and thermographic X-rays

392

go analyzes. The compound obtained corresponds to the formula Na5p2 (PO) h.

The yield of the product is 97% or 5.11 g.

PRI me R 5. See e 6 g

Sn (HPO) 2 and 4.32 g KSE (1: 3 mol) are heated at 700 ° C for 2 h. The cooled mixture is washed from the soluble part with water. The residue is analyzed by chemical, radiographic and thermographic analyzes. The resulting compound corresponds to the formula KSn (Р04).

You product progress 97% or 5.25 g „

Example 6. A mixture of 6 g of Sn (HPOp2 and 5.76 KCE (1: 4 mol)) is heated at 800 ° C for 1 hour. The cooled mixture is washed from the soluble part with water. The residue is analyzed by chemical, X-ray and thermographic analysis. The resulting compound Corresponds to the formula KZPZ (RO),

The yield of the product is 97% or 5.25 g.

Example 7. A mixture of 6 g of Sn (HP04) 2 and 7.0 g of RbCE (1: 3 mol). Heat at 700 ° C for 3 hours. Cool the adenoia mixture from the soluble part with water. The residue is analyzed by chemical, radiographic and thermographic analyzes. The compound obtained corresponds to the formula RbSn (.RO), the yield of the product is 98% or 5.75 g.

Example 8. A mixture of 6 g

Sn (HPO,), and 9.34 RbC (1: 4 mol)

about heated at 800 ° C for

2 hours Oz collapsible mixture washed

from the soluble part of the water. The residue is analyzed by chemical, radiographic and thermographic analyzes. The compound obtained corresponds to the formula

RbSn (Р04) h.

The yield of the product is 97% or 5.69 g. EXAMPLE 8 (known). 2 g of Sn (НРО ,,) 2 Н ,, О are titrated with 0.1 But LiOH solution (NaOH, KOH) in the presence of О51 and. an aqueous solution of LiCg chloride (NaCe 5 KCE). The amount of Li (K) is equal to the exchange capacity of Sn (). J, i.e., 6 meq-eq per 1 g of Sn (HPO) J HjО. The system is kept

) achieve equilibrium within 12 days. In less time, equilibrium is not reached. The solid phase is separated from the solution, washed and exhausted.

air dry to constant weight. The obtained samples are dried in air and examined by chemical, X-ray and thermographic analyzes. The compound obtained corresponds to the formula Zp (m PO). nHjO, where M - Li, Na, K. Sn (M PO) is subjected to heating, during which, starting with and above, are formed, according to X-ray diffraction, mixed phosphates of alkali metal and tin of composition m 3n, (PO.), blends with

IzR04, where M is Li, Na, K.

M SnjCPO) washed from monovalent metal orthophosphates with water.

The yield of the product is 60%, with all stages of the preparation of the compounds being carried out for 14 days.

Table 1 presents the dependence of the product yield on the process temperature.

From Table 1 it follows that carrying out the process at a temperature below 600 ° C does not ensure the completeness of the process. Increasing the temperature above 800 ° C is impractical because it leads to an increase in energy consumption without reducing the process time and increasing the product yield. The choice of heating time is carried out according to the yield of the product — optimal results with a process time of 1-3 hours,

Table 2 shows the dependence of the time taken to obtain the process on temperature with a product yield of 90%.

Output%: LiSnj (Р04) e

NaSn (Р04) s KSn (Р04) s RbSnj (Р04) s

In Table 3, the dependence of the yield of L Sn (P04) on the heating time at is given;

In tab. presented exit

M Sn (PO) s at a ratio of 1 M CE:: Sn (HPO), a process time of 1 hour and at 800 ° C.

The choice of the molar ratios of the initial reactants of the mixture is due to the stoichiometry of the chemical reaction. As can be seen from Table 4, the yield of the mixed alkali metal phosphate and tin remains almost constant, starting with the ratio of alkali metal chloride to monosodium tin phosphate, equal to m of CisNCHCHO 2: 1 mol.

Increasing the amount of tin acid phosphate above stoichiometric

leads to an increase in the yield of impurities in the form of tin pyrophosphate. Increasing the amount of alkali metal chloride above 4: 1 mole is impractical because it leads to overrun

one of the reagents, without reducing the process time and increasing the yield of the product.

Table 3 shows the dependence of the yield of М Snj (Р04) 3 on the ratio

M СЬ: Sn (HP04) 2 with a process time of 1 hour and a temperature of 800 ° C.

As can be seen from the above examples, the process time for the proposed method is 1-3 hours,

those. reduced by more than 100 times, in addition, the product yield increased to 97% compared to 60% by a known method.

Table 1

Time h

Does not provide complete reaction

709797969797

659897989898

609797989898

709898979898

Output,% M Snj (PO),

97

716/31

Circulation 452 Subscription

VNIIPI USSR State Committee

on inventions and discoveries 113035, Moscow, Zh-35, Raushsk nab., 4/5

Branch PPP Patent, Uzhgorod, st. Project, 4

table 2

Table 3

Table4

97

97

97

Claims (2)

1. METHOD FOR PRODUCING MIXED ALKALINE METAL PHOSPHATE AND TIN by reacting monosubstituted tin phosphate and alkali metal chloride, and so on, 4ψο, in order to reduce the process time while increasing the product yield and preserving its quality, alkali metal chloride taken in solid form and the interaction is carried out at 600-800 ° C for 1-3 hours 2. The method according to claim 1, characterized in that the alkali metal chloride and tin orthophosphate are taken in an amount of (2-4): 1 mol, respectively. SU „„ 1212939 1 12