A method of obtaining a solid disodium salt of nitrilotriethanol acid

 

(57) Abstract:

The invention relates to a method for producing a solid disodium salt of nitrilotriethanol acid (NTF) by neutralizing the solution NTF - acid with sodium hydroxide to pH 2.5 and 3.4. The concentration of NTF - acid in the reaction mass is 30-50 wt.%. The method allows to obtain the disodium salt of NTF - acid in crystalline form with the content of the basic substance 97-99% with a yield of about 75% of theory. 2 C.p. f-crystals, 2 tab.

The invention relates to a technology for sodium salts of nitrilotriethanol (NTF) acid, used as components of detergents, inhibitors, and other industries.

Known methods for producing sodium salts NTF-acids (five - and destinationy) in aqueous solution by neutralizing with caustic soda, the reaction mass formed in obtaining NTF - acid interaction of phosphorus compounds (phosphorous acid, phosphorus trichloride or monomethylfumarate) with ammonia and formaldehyde in the aquatic environment (Ed.St. USSR N 992519, MKI C 07 F 9/38, publ. 1983 ).

However, the use of sodium salts NTF - acid in the form of water which also leads to a significant cost when transporting over long distances. Closest to the present invention is a method of obtaining trinational salt NTF - acid in solid form, whereby the product of the interaction of ammonia with formaldehyde and phosphorus trichloride is treated with caustic soda at 70-80oC to pH 3.5 to 4.5, and the target product are filtering (RF Patent N 2056428, MKI C 07 F 9/38, publ. 1986 ).

Obtained by a specified method trinacria salt NTF-acid on quality indicators corresponds to the technical product (TU 6-09-20-243-94) and cannot be used, for example, in the food industry.

The problem to which the invention is directed, is to obtain disodium salt NTF - acid in solid form.

This task is solved in that an aqueous solution NTF-acid neutralized with sodium hydroxide to pH 2.5 and 3.4, and to obtain the target product with high yield and the desired frequency concentration NTF-acid in the reaction mass (solution of the acid plus alkali or its solution) should be 30 to < = 50.%.

When carrying out the same process with prior NTF-acid, for example by interaction of ammonia, formaldehyde and compounds of trivalent phosphorus, NTF-acid extracted from reaktywacja the following examples.

Example 1. To neutralize the charge of 100 g of an aqueous solution with a mass fraction of the main substance of 45% and with continuous stirring in small portions dose of 12.3 g of solid sodium hydroxide (mass fraction NTF-acid in the reaction mass is 40%). The reaction proceeds with evolution of heat and the reaction mixture is heated to 50-80oC. the Dosage of caustic soda stop when after complete dissolution of the last portion of alkali pH of the reaction mass reaches 3.0V. The reaction mass incubated for 2 hours with continuous stirring, cooled to 15-20oC, the resulting suspension filtered. The crystalline precipitate is dried under vacuum at 40oC. Get 42,3 g of product with quality indicators: mass fraction of the main substances in terms of Na2NTF. H2O - 97,4%; mass fraction of chlorine-ion - 0,16%; acid number 448 mg KOH/g, the Obtained product composition corresponds disodium salt NTF-acid dnovotny (see tab.1 in the end of the description).

Analytical data mass fraction in it disodium salt NTF-acid dnovotny is 97,4%. Output 76,1% of theoretical.

Examples 2-6. The process is carried out analogously to example 1 with changing conditions of neutralization and the mass fraction NTF-acid in the region of the flask with a capacity of 1 DM3, equipped with a mechanical stirrer, a refrigerator connected to a absorption of hydrogen chloride, and two drip funnels, placed 108, 36% hydrochloric acid, then with vigorous stirring and at a temperature of 40oC added simultaneously dropwise 192 g of phosphorus trichloride (1.4 M PCI3) and a mixture of 144 g of 37% formalin solution(1.8 M) CH2O) and 40 g of ammonia water (0,6 M NH3), keeping the temperature rate of addition of reagents and external cooling. Upon completion of addition, the reaction mass is heated to 100oC and kept at this temperature for 1 h for complete removal of the evolved hydrogen chloride. Then the reaction mass is then cooled to 25-30oC under stirring. The resulting crystalline product (87,6 g 90,2% NTF - acid) is filtered off, dissolved in and 70.5 g of water and with vigorous stirring, added dropwise 44% solution of sodium hydroxide (calculated mass fraction of NTF-acid in the reaction mass 38%). The dosage of caustic soda stop when the pH reaches 3.0V. After the reaction mass was incubated for 2 h with continuous stirring. Then the reaction mass is then cooled to 15-20oC, the resulting suspension filter is the duty to regulate the composition of the disodium salt NTF-acid dnovotny. Output 43.1% of theoretical, calculated on PCI3.

The given examples show that increasing the concentration of NTF-acid in the reaction mass more than 50% leads to deterioration of the quality of the target product (mass fraction of the basic substance, the mass fraction of chlorine-ion). In addition, in this case, there is thickening of the suspension resulting from the crystallization of the reaction mass. The decrease in same concentration NTF-acid in the reaction mass below 30% leads to the decrease of the yield of the target product. It should be noted that the choice of the mass concentration NTF-acid in the reaction mass is possible to adjust the purity of the product.

The process of neutralization solution NTF-acid at pH below 2.5 or above 3,4 leads to lower values of "exit" of the target product and the mass fraction of the main substances in the finished product.

To neutralize NTF-acid can be used as a solid alkali, and its solution.

Thus, the proposed method allows to obtain the disodium salt of NTF-acid in crystalline form with the content of the basic substance 97-99% with a yield of about 75% of theoretical.

1. The method of obtaining TV will gorhaut neutralization with sodium hydroxide to a pH of 2.5 - 3,4.

2. The method according to p. 1, characterized in that the concentration of NTF - acid in the reaction mass is 30 to 50 wt.%.

3. The method according to PP.1 and 2, characterized in that during the process to prior NTF-acid, for example, the interaction of ammonia, formaldehyde and compounds of trivalent phosphorus before neutralization NTF - acid is recovered from the reaction medium by crystallization.

 

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