The method of obtaining inhibitor deposits of mineral salts

 

(57) Abstract:

Usage: in the chemical industry. The inventive carry out the hydrolysis of phosphorus trichloride by treatment with water or 5 - 35% hydrochloric acid in the environment of 75 - 95% of phosphorous acid at 25 - 75oC at a molar ratio of phosphorus trichloride and water, equal to 1 : (3 - 4). 3 table.

The invention relates to a method for inhibiting the deposition of mineral salts that can be used in chemical, metallurgical and other industries.

Known methods for producing inhibitors deposition of mineral salts aminomethylphosphonate type interaction of formaldehyde, derivatives of ammonia and phosphorus trichloride.

The disadvantages of the known methods are technical difficulties associated with the diversion of a large amount of heat from the reaction mass by interaction of the components, a large amount of liquid waste hydrochloric acid concentration of 20-22%, contaminated with formaldehyde and phosphorous-containing compounds.

A method of obtaining inhibitors deposition of mineral salts by the interaction of formaldehyde and nitrogen compounds with phosphorous CISL">

Closest to the proposed method is a method for inhibiting the deposition of mineral salts, which lies in the interaction of phosphorous acid, formaldehyde and ammonium chloride - waste production, and phosphorous acid is obtained by hydrolysis of phosphorus trichloride or VAT residue production dimethylphosphite.

The disadvantages of this method are.

the duration of the hydrolysis of phosphorus trichloride, due to the exothermic heat effect of the reaction of hydrolysis of phosphorus trichloride and hydration of the resulting hydrogen chloride with excess of water present in the reaction mixture;

the necessity of removing the hydrochloric acid to produce phosphoric acid concentration of 75-85%, used for synthesis inhibitor, which requires additional energy costs;

low concentration of hydrochloric acid (20-22%), warded off from the reaction mass, which finds no outlet.

It should be noted that the methods of obtaining phosphorous acid hydrolysis of phosphorus trichloride described in the literature, based on the process in organic solvents, in water or in steam Chesto solvents, phosphorous acid and the released hydrogen chloride contaminated with organic solvents and cleaning it is necessary to use special methods.

The aim of the invention is to reduce the duration of the process, simplifying and disposal of waste.

The objective is achieved by carrying out the hydrolysis of phosphorus trichloride in obtaining inhibitor deposition of mineral salts in aqueous phosphoric acid concentration 75-95% at a temperature of 25-75% and used as hydralicious agent water or hydrochloric acid concentration of up to 35%.

For the process to 75-95% phosphoric acid simultaneously poured phosphorus trichloride and water or hydrochloric acid at a molar ratio of PCl3:H2O = 1:(3-4) at 25-75oC. Then, to the resulting reaction mass is added formaldehyde and ammonium chloride, heating the mixture to 100-105oC, aged for 2-3 h and neutralized with caustic soda to pH 5-7. Hydrogen chloride in an amount up to 10% contained in the phosphoric acid, is a catalyst for condensation and prevents oxidation of phosphorous acid.

As formaldehydefree raw materials use formalin (37% aqueous who, formed in the production of polyethylenepolyamine (TU 6-05-211-1357-8). For hydrolysis of phosphorus trichloride use water, hydrochloric acid concentration of up to 35% or hydrochloric acid, the waste generated during the purification of hydrogen chloride and containing up to 7% phosphorous acid.

Example 1. Into a flask equipped with a stirrer, thermometer and reflux condenser, a load of 50 g of 75% phosphoric acid. With stirring, poured into the flask for 3 h 412 g (3 mol) of phosphorus trichloride and 162 g (9 mol) of water. The temperature of the reaction mass during high tide components 25-35oC. At the end of the tide phosphorus trichloride and water to the reaction mass, containing 83% phosphoric acid and 10% hydrogen chloride, add 278 g (3,45 mol) of formalin and 62,0 g (1.15 mol) of ammonium chloride. The mixture is kept for 3 hours at 100-105oC and get 675 g of product containing 51.2% of nitrilotriethanol acid. The yield of 99.5%. After neutralization of the reaction mass 42% sodium hydroxide solution to pH 6 receive 1325 g of 31% aqueous solution of sodium soda inhibitor. Output to 97.1%.

Hydrogen chloride released during hydrolysis, dirty pairs trichloride phosphorus in the ash. For cleaning charitychoice phosphorus, and the purified hydrogen chloride is used to produce hydrochloric acid.

Example 2. The experience carried out as described in example 1 with the difference that the temperature of the reaction mixture during the hydrolysis of phosphorus trichloride 50-55oC. eventually get 1307 g of an aqueous solution of sodium salt of the inhibitor concentration of 31.1%. Output 96,1%.

Example 3. Into a flask equipped with a stirrer, thermometer and reflux condenser, load 75 g 95% phosphorous acid and poured with stirring for 3 h 700 g (5.0 mol) of phosphorus trichloride and 365 g(20.0 mol) of water. The process temperature of 70-75oC. To the resulting reaction mass, containing 85% phosphoric acid and 9% hydrogen chloride, add 470 g of 37% formalin and 110 g of ammonium chloride. The mixture was incubated 2 h at 105oC, neutralize 43% sodium hydroxide solution to pH 6. Get 2200 g 31,5%-aqueous solution of sodium salt of the inhibitor. The yield of 98.2%.

Example 4. In a reactor equipped with a stirrer, thermometer and reflux condenser, load 80% phosphorous acid and stirring at a temperature of 30-40oC poured 700 g of phosphorus trichloride and 300 g of water. Evolved hydrogen chloride passes siritho hydrogen, add 490 g of 37% formalin and 153 g of ammonium chloride, stirred for 2 h at 103-105oC, neutralize 43% sodium hydroxide to pH 5 and receive 2290 g of 31.4% of the inhibitor. The yield of 98.3%.

Example 5. In a reactor as described in example 1, load 70 g 90% of phosphorous acid and poured with stirring for 2 h 300 g (2,18 mol) of phosphorus trichloride and 120 g (6,66 mol) of water. The process temperature is 65-75oC. To the resulting reaction mass containing 94% of phosphorous acid and 4% hydrogen chloride, add 235 g of 37% formalin and 53 g of ammonium chloride, the mixture was incubated 2 h at 105oC and neutralized with caustic soda to pH 7, receive 1170 g of inhibitor, the concentration of 29%. Output to 96.9%.

Example 6. In a reactor as described in example 1 was charged 150 g of 75% phosphoric acid and poured for 3 h 412 g of phosphorus trichloride and 205 g of 20% hydrochloric acid. Process temperature 25-35oC. hydrogen Chloride produced during the reaction, enters the wash bottle filled with concentrated hydrochloric acid (1,175 g/cm3), where the absorption of phosphorus trichloride, carried away from the reaction mixture. Purified hydrogen chloride absorb water and get a hydrochloric acid concentration of 35-36%.

P is the acid and 7% hydrogen chloride, add 235 g of 37% formalin and 53 g of ammonium chloride. The mixture is kept for 3 hours at 100-105oC and after neutralization 42% sodium hydroxide solution to pH 5 get the 1020 g of a 34% aqueous solution of sodium salt of the inhibitor. The yield of 98.3%.

In table. 1 shows the receipt of the inhibitor using as gidrolizuemye agent hydrochloric acid of different concentrations and hydrochloric acid formed during the purification of hydrogen chloride.

In table. 2 shows data on the duration of the stages of the synthesis process of obtaining inhibitor of the prototype and the proposed method.

Thus, the above examples show the following advantages of the proposed method:

reduced process time by eliminating the stage of Stripping hydrochloric acid, as produced phosphoric acid has a concentration of 82-94% and without additional concentration is used to obtain inhibitor;

excluding energy costs for cooling of the reaction mixture during the hydrolysis, as the exothermic heat effect hydrolysis does not occur and to maintain the required temperature of heat addition or rejection is not required;

the exception is I temperature limitations (not exceeding 40oC prototype);

recycling waste production of hydrochloric acid used for the purification of hydrogen chloride vapors from phosphorus trichloride is carried away from the reaction zone;

obtaining hydrogen chloride, which can be used to obtain concentrated hydrochloric acid, THE corresponding 6-01-193-80.

The concentration of the inhibitor in the resulting solutions was determined by titration of copper sulfate in the presence of the indicator-murexide.

The effectiveness of inhibitors obtained using ammonium chloride - waste production polyethylenepolyamines (TU 6-05-211-1357-84), salts of calcium are shown in table.3.

As can be seen from the table. 2, the efficiency of the inhibitors obtained by the proposed method is not inferior to the effectiveness of the inhibitor obtained in the prototype. The output of the inhibitors is 96-100%, the output of the inhibitor in the prototype 93-99%.

The method of obtaining inhibitor deposits of mineral salts by hydrolysis of phosphorus trichloride and interaction obtained phosphorous acid with formaldehyde and ammonium chloride, characterized in that, to simplify the method and time of its holding, the hydrolysis trichloride phospho what>With a molar ratio of phosphorus trichloride and water, equal to 1 : 3 - 4.

 

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