RU2410121C2 - Chloro-active agent and preparation method thereof based on n,n-dichloroaryl sulphamides - Google Patents

Abstract

FIELD: chemistry.

SUBSTANCE: agent is based on N,N-dichloroarylsulphamides, specifically dichloramines B, T and XB. The agent has the following components, given in wt %: trialkylaryl ammoniuim chloride - up to 3, N,N-dichloroarylsulphamides 10.0-15.0, hydroxide of an alkali metal 5.0-10.0, water - the rest. The agent also contains up to 1 ml/l indicator of the class of sulphophthaleins. The method of preparing the agent involves reaction of a hydroxide of an alkali metal and chlorides of quaternary trialkylaryl ammonium compounds in an aqueous solution with solid-phase N,N-dichlorosulphamides in autothermal conditions. The disinfecting and degassing agent has high antimicrobial activity when used to treat laboratory equipment and production wastes, as well as degassing and bleaching activity. The agent can also serve as a base for disinfecting and other formulations.

EFFECT: method of preparing the agent is simple, cheap and easy to reproduce in laboratory and field conditions.

3 cl, 5 ex

Description

The invention relates to the field of chloroactive preparations suitable for use as sources of active chlorine in degassing, disinfecting, bleaching, sterilizing, and cleaning products, using N, N-dichloroaryl sulfamides. Chlorative preparations are traditional disinfectants [Vashkov V.I. Means and methods of sterilization used in medicine. - M .: Medicine, 1973, p.176-179].

Known chlorine-containing preparation obtained from N, N-dichloroaryl sulfamides and sodium or potassium hydroxide, where dichloramines B, T and CB are used as N, N-dichloroaryl sulfamides [Russia, patent No. 2117491 C1, 19980820, published on 02.21.1996, publ. . 08/20/98].

The proposed composition, despite a number of advantages (low cost and availability of raw materials), has some disadvantages that are identified in the process of obtaining disinfectant formulations:

- the duration of the process of obtaining, requiring their production using special equipment and in technological installations;

- decanting and / or filtering of working solutions;

- the resulting working solutions require certain storage and transportation conditions at temperatures below 10 ° C, which complicates their application and use in emergency and emergency situations due to salting out processes occurring in these temperature conditions;

- to control the quality of the disinfectant, it is necessary to use chemical methods of analysis;

- the alkaline buffer capacity determined by the composition limits the bifunctional use of working solutions.

The objective of the invention is the creation of a chloroactive drug with the aim of further using it as a main component for the preparation of degassing, disinfecting and other formulations applicable in the aftermath of accidents at chemically and biologically hazardous facilities, in emergency situations, for the degassing of fume hoods, laboratory glassware, tools, equipment, work sites for temporary storage of industrial waste, personal protective equipment, solutions and reaction masses, with toxic chemicals.

The problem is achieved by creating a formulation based on N, N-dichloroaryl sulfamides (dichloramines B, T, CB), increasing the content of alkali metal hydroxides and introducing chemical compounds into the composition that ensure the occurrence of interfacial catalysis mechanisms both at the preparation stage and at the preparation stage use. The proposed ratio of components in an aqueous solution is, wt.%: Chloramines - from 10 to 15; alkalis - from 5 to 10; Quaternary trialkylarylammonium compounds or Quaternary phosphonium salts - up to 3.

To ensure the quality control of the drug during its storage and the direction of use of its working solutions, the use of sulfophthalein class indicators is proposed, which provide visual control both when the pH of the medium changes, and during redox processes. These indicators provide reversibility and have self-healing properties.

The proposed composition of the chloroactive drug can significantly simplify the method of its production, which makes it possible to carry out the process of obtaining both the drug itself and formulations based on it in the field.

The use of the proposed composition and the implementation of the production method leads to:

- to simplify the technology for producing a chloroactive drug (it is possible to obtain the drug both in the laboratory and in the field);

- to the process of obtaining the recipe in an autothermal mode;

- allows the use of dichloramines with expired shelf life;

- makes it possible to obtain a chloroactive agent of simple composition and no less effective (the active chlorine content is 20% higher) than the proposed products closest in their technical essence to the claimed method [Russia, patent No. 2117491 C1, 19980820, claimed 02.21.1996 ., publ. 08/20/98].

The essence of the method for producing a chlorrative preparation consists in the interaction of a liquid-phase component in the form of an aqueous solution of alkali metal hydroxides and chlorides of quaternary trialkylarylammonium compounds or quaternary phosphonium salts with solid-phase dichloroaryl sulfamide. The use of quaternary trialkylarylammonium compounds or quaternary phosphonium salts ensures the mechanisms of interphase catalysis both at the preparation stage and at the stage of use, interferes with the salting out of alkaline components and therefore no decanting and filtration operations are required. An increase in alkaline capacity, along with the presence of quaternary trialkylarylammonium compounds or quaternary phosphonium salts in working solutions, expands their bifunctional capabilities. The use of sulfophthalein class indicators provides visual control during storage and the choice of application of working solutions. The necessary stability of chloroactive solutions during storage and use is achieved by the proposed ratio of alkalinity to other components included in the proposed composition. To implement the proposed method for the preparation of the drug using the proposed composition does not require thorough mixing of the components. The reaction proceeds in an autothermal mode. The method is implemented in the field. It does not require preliminary preparation and storage of ready-made working solutions during degassing and disinfection operations.

Example 1. In a glass with a capacity of 250 ml pour 100 ml of water and dissolve 0.1 mol of alkali and 0.005 mol of triethylbenzylammonium chloride. 0.03 mol of N, N-dichloro-n-toluylsulfamide was charged into a solution heated to 45 ° C, and held for 5 minutes. The working solution is analyzed for the content of active chlorine. 0.1 ml of a 0.1% alcohol solution of tetrabromophenoltetraiodophthalein is added.

111 g (98.1%) are obtained. Found: Cl (act.) 36.09 mg · ml ^-1 ; 35.91 mg · ml ^-1 . Calculated Cl (act.) 37.29 mg · ml ^-1 . The yield of active chlorine is 96.5%.

Example 2. In a glass with a capacity of 250 ml pour 100 ml of water and dissolve 0.1 mol of alkali and 0.005 mol of a mixture of alkyldimethylbenzylammonium chlorides (catamine B). 0.03 moles of N, N-dichlorobenzenesulfamide are charged into a solution heated to 30 ° C and incubated for 15 minutes without stirring. The working solution is analyzed for the content of active chlorine. Add 0.1 ml of a 0.1% alcohol solution of tetrabromophenoltetraiodophthalein.

108.5 g (95.8%) are obtained. Found: Cl (act.) 35.29 mg · ml ^-1 ; 35.40 mg ml ^-1 . Calculated Cl (act.) 37.29 mg · ml ^-1 . Yield 94.78%.

Example 3. In a glass with a capacity of 250 ml pour 100 ml of water and dissolve the previously prepared mixture: 0.1 mol of alkali and 0.005 mol of triethylbenzylammonium chloride. 0.03 moles of N, N-dichlorobenzenesulfamide are charged into a solution heated to 50 ° C and held for 15 minutes. The working solution is analyzed for the content of active chlorine. Add 0.1 ml of a 0.1% alcohol solution of tetraiodophenol tetraiodophthalein.

107.5 g (94.5%) are obtained. Found: Cl (act.) 37.29 mg · ml ^-1 ; 36.40 mg ml ^-1 . Calculated Cl (act.) 37.29 mg · ml ^-1 . The yield of active chlorine is 98.80%.

Example 4. In a glass with a capacity of 250 ml pour 100 ml of water and dissolve 0.1 mol of alkali. 0.03 mol of N, N-dichloro-n-toluylsulfamide was charged into a solution heated to 75 ° C, and kept for 5 hours. The reaction mass is decanted for about a day. The working solution is analyzed for the content of active chlorine. 0.1 ml of a 0.1% alcohol solution of α-naphtholphthalein is added.

75 g (70.0%) are obtained. Found: Cl (act.) 28.09 mg · ml ^-1 ; 27.91 mg ml ^-1 . Calculated Cl (act.) 37.29 mg · ml ^-1 . The yield of active chlorine is 70.5%.

Example 5. In a polymer barrel with a capacity of 200 l, 100 l of water is poured and a previously prepared mixture of 5 kg of sodium hydroxide and 0.5 kg of triethylbenzylammonium chloride is dissolved. 3.6 kg of N, N-dichlorobenzenesulfamide are loaded into the solution, and aging is carried out for 5 minutes. The working solution is analyzed for the content of active chlorine. 20 ml of a 0.1% alcohol solution of tetrabromophenoltetraiodophthalein are added.

100.5 kg (88.8%) are obtained. Found: Cl (act.) 32.77 mg ml ^-1 , 31.40 mg ml ^-1 . Calculated Cl (act.) 37.29 mg · ml ^-1 . The yield of active chlorine is 86.0%.

Thus, the proposed composition and method for producing a chloroactive drug from N, N-dichloroaryl sulfamides (dichloramines B, T, HB) using chlorides of quaternary alkylarylammonium compounds that provide mechanisms for interphase catalysis, in comparison with its prototype [Russia, patent No. 2117491 C1, 19980820, claimed 02.21.1996, publ. 08/20/98,], has several advantages:

- It makes it possible to obtain a chloroactive agent simple in composition and no less effective than existing products (the content of active chlorine is 20% higher);

- increases the yield of active chlorine by 20% compared with the closest prototype [Russia, patent No. 2117491 C1, 19980820, claimed 02.21.1996, publ. 08.20.98 g.];

- simplifies the technology of obtaining the drug;

- allows you to carry out the process of obtaining recipes in autothermal mode;

- we realize in the field;

- expands the possibility of using the drug as a bifunctional agent (disinfectant, degassing), in emergency situations and during the liquidation of accidents, as well as for the degassing of laboratory glassware, instruments, equipment, fume hoods, work sites for temporary storage of industrial waste, personal protective equipment, solutions and reaction masses contaminated with toxic chemicals and other forms of microorganisms;

- allows the use of dichloramines with expired shelf life;

- reduces the amount of liquid waste when using the proposed tool, since it does not require additional processing and washing surfaces to remove salts of alkaline earth metals (in the form of white plaque), formed during degassing and disinfection of existing chloroactive agents;

- the possibility of processing infected, oily surfaces (degassing, disinfection of weapons and military equipment) without their preliminary preparation (cleaning) using organic solvents is expanding.

Claims (3)

1. Chlorative agent based on N, N-dichloroaryl sulfamides and alkali metal hydroxide, characterized in that it additionally contains trialkylarylammonium chloride or Quaternary phosphonium salts in the following ratios of components, wt.%:
trialkylarylammonium chloride up to 3.0
N, N-dichloroaryl sulfamides 10.0-15.0
alkali metal hydroxide 5.0-10.0
water - the rest 2. The chloroactive agent according to claim 1, characterized in that it contains an indicator of the class of sulfophthaleins up to 1 ml / L. 3. The method of producing the chloroactive agent according to claim 1, characterized in that the liquid-phase component is reacted in the form of an aqueous solution of alkali metal hydroxides and chlorides of quaternary trialkylarylammonium compounds or quaternary phosphonium salts with solid phase dichloroaryl sulfamide in an autothermal mode.