Sulfitonetaine sterilizing agent and synthetic method thereof

A sulfite and fungicide technology, applied in the directions of fungicides, biocides, biocides, etc., can solve the problem of less research on bactericidal performance, and achieve broad market application prospects, good bactericidal treatment, and improved bactericidal activity. Effect

Inactive Publication Date: 2015-06-24
SOUTHWEST PETROLEUM UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are few reports on this kind of sulfite betaine fungicides, and there are few studies on their fungicidal properties.

Method used

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  • Sulfitonetaine sterilizing agent and synthetic method thereof
  • Sulfitonetaine sterilizing agent and synthetic method thereof
  • Sulfitonetaine sterilizing agent and synthetic method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1: Synthesis of intermediate vinyl sulfite

[0025] The synthesis method of the intermediate vinyl sulfite is as follows:

[0026] (1) Add 62.1g (1.0mol) of ethylene glycol into a 250mL three-necked flask, and add 88mL (1.2mol) of thionyl chloride under constant stirring;

[0027] (2) The constant temperature water bath is heated to 35~40℃, and the irritating gas escapes, and the escaped gas is absorbed with lye;

[0028] (3) After the addition of thionyl chloride is completed, raise the reaction temperature to 70°C and react for 2h;

[0029] (4) After the reaction is completed, vacuum distillation is carried out to recover 60-70℃ / 3.3×10 3 Pa.

Embodiment 2

[0030] Example 2 Synthesis of Fungicide

[0031] Experiment 1 Synthesis of bactericide 2-(1-methylimidazole) ethyl sulfite salt IAES:

[0032] (1) Add 8.2 g (100 mmol) of 1-methylimidazole and 20 mL of 1,4-dioxane to a 250 mL three-necked flask;

[0033] (2) Heat to reflux temperature, slowly add 13.0g (120mmol) vinyl sulfite dropwise under constant stirring, after the dropwise addition, react for 2-5h;

[0034] (3) After the reaction is completed, the solvent is removed by rotary evaporation, recrystallization is carried out 2-3 times with acetonitrile, and after vacuum drying, a pale yellow granular solid 2-(1-methylimidazole) ethyl sulfite salt is obtained.

[0035] Test 2 Synthesis of the fungicide 2-(4-methylmorpholine) ethyl sulfite salt MLES:

[0036] (1) Add 10.1 g (100 mmol) of 4-methylmorpholine and 20 mL of 1,4-dioxane into a 250 mL three-necked flask;

[0037] (2) Heat to reflux temperature, slowly add 13.0g (120mmol) vinyl sulfite dropwise under constant stirring, after the d...

Embodiment 3

[0047] Example 3 Structural Characterization of Fungicide

[0048] The structure of the samples prepared in Experiment 1, Experiment 2, Experiment 3, and Experiment 4 in Example 2 was analyzed by infrared spectrogram. Using KBr tableting method, the structure of the fungicide was characterized by WQF-520A Fourier transform infrared spectrometer. The infrared spectrum is as follows figure 1 , figure 2 , image 3 with Figure 4 Shown. From figure 1 It can be seen from figure 1 It can be seen that 3095cm -1 Is the stretching vibration of hydrogen on unsaturated carbon, 2095, 2877cm -1 Where is the methyl stretching vibration peak, 1648cm -1 C=C stretching vibration on the imidazole ring, 1115cm -1 Is the stretching vibration peak of S=O; from figure 2 It can be seen that 2956, 2881cm -1 Is the methyl stretching vibration peak, 1123, 1031cm -1 Is the vibration absorption peak of S=O and S—O; from image 3 It can be seen that 3030cm -1 Is the stretching vibration of hydrogen on unsa...

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Abstract

The invention discloses four zwitterionic sterilizing agents containing a sulfitonetaine structure and a synthetic method thereof. The synthetic method is characterized by comprising the following steps: (1) adding 1-methylimidazole (or 4-methylmorpholine, or N, N-dimethyl benzylamine, or 3-dimethylamino methylindole) in a three-necked flask and fully dissolving by 1, 4-dioxane; (2) heating till refluxing, slowly dropwise a certain amount of ethylene sulfite while stirring, and reacting for 2-5h after the dropwise adding step is finished; (3) removing the solvent, recrystallizing by using acetonitrile and performing vacuum drying to obtain the white powdered solid sterilizing agent. The sterilizing agent has the characteristics of good water solubility, good killing effect on sulfate reducting bacteria (SRB) and saprophytic bacteria (TGB) and long-lasting sterilizing effect. The oil field injected water and the oil field sewage can be well sterilized by the sterilizing agent; therefore, the sterilizing agent has a wide market application prospect.

Description

Technical field [0001] The invention relates to four kinds of water treatment fungicides and their synthesis methods, in particular to a fungicide for oil industry oil field injection water and oil field sewage and a synthesis method thereof. Background technique [0002] With the development of social economy and the improvement of technological level, people's awareness of environmental protection is constantly increasing, and higher requirements are put forward for the quality of living environment. Therefore, chemical agents with killing function have attracted people's attention and have been widely used in many fields such as energy extraction, medical and health, and daily life. At this stage, oil is still the pillar energy that promotes the operation of society. In oil exploration, water injection and polymer solution injection are used to increase oil recovery. However, there are many kinds of microorganisms in oilfield water injection, mainly sulfate reducing bacteria ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/60C07D295/088C07D209/14C07C301/00A01N43/50C07C41/02A01N43/38A01P1/00A01P3/00C02F1/50
CPCC07D233/60A01N43/38A01N43/50A01N43/84C02F1/50C07C41/02C07C301/00C07D209/14C07D295/088
Inventor 苟绍华何杨周利华罗珊张勤赵鹏敬东
Owner SOUTHWEST PETROLEUM UNIV
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