SU1139733A1 - Method of obtaining 3-amino-1,2,4-dithiazolidinethion-5 - Google Patents

Abstract

1. METHOD OF OBTAINING 3-AMINO1, 2,4-DITIAZOLIDONIONA-5 using amidane rodanide in the presence of water when heated, so that, in order to increase the yield of the target product and simplify the process technology, ammonium rodanide interacts With an acidic se.1 sodium sulfate or ammonium salt, water is taken in a mass ratio to ammonium rodanide 0.4-0.5: 1, respectively, the process is carried out in a heterogeneous phase. 2. A pop method, 1, characterized in that the process is carried out at a mass ratio of ammonium rhodium and sodium or ammonium sulphate, 1: 1.75-2.1, respectively. S 3. Method. But nn. 1 and 2, which is based on the fact that the process is carried out for 50-60 minutes. ,

Description

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This invention relates to an improved process for the preparation of 3-amino-1,2,4-dithiazolidin-5-ion (xanthan hydrogen), which is used as a rubber vulcanization accelerator and in the synthesis of corrosion inhibitors to protect ferrous and non-ferrous metals.

The closest to the proposed is the method of obtaining 3-amino1, 2,4-dithiazolidin-5-5, which is that ammonium or sodium rodanide is reacted with concentrated sulfuric acid in water at 70-75 ° C, respecting the weight ratio of rohanide and sulfuric acid, equal to 1: 2.3-2.4, respectively. The yield of the target product is 40% l2.

The disadvantages of this method are the low yield of the target product, the use of hydrogen sulfide, carbon dioxide and carbon dioxide in the process of reacting the reactants using scarce concentrated sulfuric acid.

The purpose of the invention is to increase the yield of the target product, as well as simplify the process technology,

The goal is achieved by the fact that according to the method of producing 3-amino-1,2,4 dithiazol yridinone-5 ammonium rohanide is reacted with an acidic sulphate of sodium, or ammonium, water is taken in mass ratio of ammonium to robanide of 0.4-0.5: 1 accordingly, the process is conducted in a heterogeneous phase.

The process is carried out at a mass ratio of ammonium ammonium and sodium or ammonium acid sulfate 1, 1.75-2.1, respectively.

The process is carried out for 50-60 minutes

The proposed method allows a 2-fold increase in the yield of the target product,

And p and meer. 1, To 180 g of ammonium rhodanide (NHjSCN), 316 g of sodium sulphate (NaHSO j) is added, which corresponds to a ratio of 1; 1.76, and, after thorough mixing, another 80 g of water. The mixture is heated to 75 ° C for 90 minutes and then kept at this temperature for 60 minutes. Then, 1500 ml of water was added to the reaction mixture to dissolve unreacted salts, and then 3-amino 1,254-dithiazolidin-5-5 was removed from the solution by filtration.

A total of 101.5 g of product is obtained, which corresponds to a yield of 85.7% (in terms of rodanide),

The content of the main substance in it is 96.5%. h The elemental composition of the obtained product is presented in table. one,

The effect of temperature on the output of xanthan hydrogen at a constant (Ratio III SCN: NaHS04 1 s 1.75 and a dwell time of 60 minutes is given in Table 2,

As can be seen from this table, 2, the temperature rise positively affects only up to 75s. Above this temperature, the yield of the product begins to decrease. This is due to the volatilization of hydro genic acid as the temperature rises. Therefore, it is desirable to conduct the process within the temperature range of 60 - 80 C,

At the exit of the product, as follows from the table. 2, the ratio between ammonium rhodanide and sodium hydrochloride is affected,

 The effect of ammonium rohanide ratio; sodium sulphate on the output of xanthan hydrogen with a constant temperature and a holding time of 60 minutes is given in Table 3,

The highest yield is achieved at a ratio of 1: 1.75. The decrease in yield at a ratio of 1: 1.5 can be explained by the lack of hydrogen ions necessary to complete the reaction. The effect of a large excess of acid salt on the product yield can be explained by the fact that per unit volume of the reacting mass there is a large acidity, which in all likelihood leads to the possibility of side processes, reducing 1X, ultimately, the yield of the target product.

The effect of the exposure time on the yield of xanthan hydrogen with the ratio NH4SCN: NaHS04 1: 1.75 and 60 ° С is given in table 4,

A low yield at a shutter speed of 15 min can be explained by the incompleteness of the reaction in a given period of time,

The lack of time after 60 minutes of exposure indicates that the reaction is completely complete and further maintaining the reaction mass does not give an increment of output.

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The effect of the NH SCNtH O ratio on the product yield at constant ratios NH4SCN: NaHS04 1: 1.75, 60 ° C and a holding time of 60 minutes is given in Table. five.

When considering the data given in table. 5, it should be assumed that the amount of water added by the ia reaction system is not enough to completely dissolve the salts. The low yield of the target product in the absence of water can be explained by the fact that the dissociation of an acid salt with formation of hydrosulfate ion (HSOij) takes place to a small extent and therefore the development of other reactions leading to the production of xanthan hydrogen is difficult. Increasing the amount of water leads to a decrease in the concentration of HSO due to dilution and, therefore, reduces the activity of hydrogen ions, which catalyze the process of polymerization of hydrogen hydroxide.

397334

: In tab. 6 shows comparative indicators of the process for the preparation of 3-amino-1,2,4-dithioazolidin-5-5 by known and proposed methods. 5 From the comparative data in Table. 6, it is clear that the prototype method is inferior to the expected production of xanthan hydrogen as per you. In addition, the proposed method for producing xanthan hydrogen eliminates the use of deficient and aggressive sulfuric acid, improves the yield and quality of the chain 5 product, creates more comfortable and safer working conditions, and lengthens the service life of the equipment. The cost of a ton of xanthan hydrogen in the proposed method at 826.5 p .; 20 less than the basic version. | With an annual need for xanthan hydrogen for a rvzino-technical, hardware, and radio engineering capacity in the amount of 1000 tons, the economic effect will be 826500 r. Table

Content of the main substance,% Indicators 1gL16 Yield,% 59.5 Content of the main substance,%

Temperature, C

96.5

94

93

T tb l and c a 3 Ratio NH SCNtNaHSO 1: 2, t 1: .75 J 1,1,5 66,167,271,856,8 Indicators 15 I 20 Yield,% 58.8 64.4 Content of the main substance,% 89.0 90.0 26.4 61.6 Yield,% Content of the main substance,%

Table4 85 Exposure time, min I 40 I 50 I 60 66.8 69.0 71.8 71.9 91.0 92.0 93.0 93.5 67.6 71.8 63.4 90

Claims (3)

1. METHOD FOR PRODUCING 3-AMINO,2,4-DITIAZOLIDINTHION-5 using ammonium thiocyanate in the presence of water when heated, characterized in that, in order to increase the yield of the target product and simplify the process technology, ammonium thiocyanate is reacted with an acidic sulfate salt sodium or ammonium, water is taken in a mass ratio to ammonium thiocyanate of 0.4-0.5: 1, respectively, the process is carried out in a heterogeneous phase. 2. The method of pop. 1, characterized in that the process is carried out with a mass ratio * of ammonium thiocyanate and sodium or ammonium acid sulfate, 1: 1.75-2.1, respectively. 3. Method According to paragraphs. 1 and 2, which entails that the process is conducted for 50-60 minutes. 1139733 2