CN104402739B - The method of cationic sterilant is prepared in a kind of sewer oil modification - Google Patents
The method of cationic sterilant is prepared in a kind of sewer oil modification Download PDFInfo
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- CN104402739B CN104402739B CN201410553808.2A CN201410553808A CN104402739B CN 104402739 B CN104402739 B CN 104402739B CN 201410553808 A CN201410553808 A CN 201410553808A CN 104402739 B CN104402739 B CN 104402739B
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Abstract
The method of cationic sterilant is prepared in a kind of sewer oil modification, by sewer oil filtered while hot, remove wherein insolubles, filtrate is joined in reaction vessel, add isopyknic aqueous sulfuric acid, stirring reaction, after reaction system is down to room temperature, leave standstill separatory, oil phase to use after isopyknic washing three times to obtain acidifying sewer oil, again acidifying sewer oil is joined in reaction vessel, add 1 of equimolar ratio example successively, 2-glycidyl trimethyl ammonium chloride and reaction solvent, stirring reaction, after having reacted, remove reaction solvent, namely solid residue obtains the cationic sterilant based on sewer oil modification after using acetone recrystallization, containing ester group in this cationic biocide molecules structure, degrade under can realizing natural condition, for environmental friendliness shaped material, present invention achieves the comprehensive utilization of sewer oil, the raw material sources adopted are extensive, synthesis technique is simple, reaction process low emission, reaction conditions is gentle, meet the requirement of chemicals production " greenization ".
Description
Technical field
The present invention relates to sewer oil technical field of comprehensive utilization, be specifically related to a kind of method that cationic sterilant is prepared in sewer oil modification.
Background technology
In cats product, be used as the mainly quaternary ammonium salt of sterilant, cationic sterilant has following features: 1) broad-spectrum sterilization; 2) product toxicity is little, biological degradability good, do not have detrimentally affect to environment; 3) in water, solvability is good, applied widely, storage-stable; 4) corrosion-free to being applied thing; 5) infiltration, perviousness by force, and have and certain soil removability; 6) stable performance, 5 joining property are good.Cationic sterilant has been widely used as the sterilization and disinfection of surgical operation and medicine equipment, the sterilization algae removal of industrial circulation water treatment, the treatment agent of oil field wastewater re-injection, the sanitas of forestry and building trade, sericulture disinfectant, the cleaning disinfectant of household person, public health and crust, the sterilization detergent of domestic animal, the clean sterilant of meat, eggs and other food processing plants, some kind also can be used as insect-proof agent.
Sewer oil, makes a general reference all kinds of poor quality oils existed in life, and its largest source is the oil trap of large-scale restaurant, city water drain, if edible very harmful to human body.Sewer oil can be divided three classes: one is the sewer oil of narrow sense, by the greasy floating matter in water drain or by the leftovers of hotel, restaurant, leftovers (common name swill) oil through simply processing, extracting; Two is pork inferior, haslet, pigskin processing and the oil of output after refining; Three is after exceeding certain number of times for the oily access times of fried food product, then is reused or toward the oil reused after wherein adding some fresh oils.Sewer oil backflow dining table is a thing of making us beating one's brains, and best terms of settlement carries out recycle exactly, turns waste into wealth.At present, sewer oil usually after deep processing for biofuel, beneficiation reagent, production ethanol and biogas and aviation wet goods, but these processing technology programs are loaded down with trivial details, make sewer oil fully cannot obtain recycle.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, a kind of sewer oil modification is the object of the present invention is to provide to prepare the method for cationic sterilant, the cationic biocide molecules of preparation introduces acidifying sewer oil component by esterification, and the methyl of the substituting group of positively charged ion end simultaneously containing three small volumes, this structural molecule cationic head base can be adsorbed in phage surface closely, destroy the cytolemma of thalline, thalline self-dissolving can be caused dead, and long-chain ester based structure can penetrate into thalline inside further, make tropina sex change, thus effectively play germicidal action.
In order to achieve the above object, the technical solution used in the present invention is:
A method for cationic sterilant is prepared in sewer oil modification, comprises the following steps:
The first step: sewer oil is heated to 50-70 DEG C, filtered while hot, remove wherein insolubles, filtrate is joined in the first reaction vessel, add isopyknic mass concentration 3-5% aqueous sulfuric acid, heat up stirring reaction 5-8h under the condition of 85 DEG C, after reaction system is down to room temperature, leave standstill separatory, oil phase to use after isopyknic washing three times to obtain acidifying sewer oil;
Second step: acidifying sewer oil is joined in the second reaction vessel, add 1 of equimolar ratio example successively, 2-glycidyl trimethyl ammonium chloride and reaction solvent, stirring reaction 8-15h under the condition of 40-60 DEG C, after having reacted, remove reaction solvent, namely solid residue obtains the cationic sterilant based on sewer oil modification after using acetone recrystallization, described reaction solvent is tetrahydrofuran (THF) or dioxane, and both mixed solvents.
Tool of the present invention has the following advantages:
1, have effectively achieved the comprehensive utilization of sewer oil, and this method production cost is low.
2, by cationic sterilant prepared by sewer oil modification, owing to containing ester group in molecular structure, degrade under can realizing natural condition, this cationic sterilant is environmental friendliness shaped material.
3, simple, the reaction process low emission of extensive, the synthesis technique of raw material sources that adopts of the present invention, reaction conditions are gentle, meet the requirement of chemicals production " greenization ".
Embodiment
Below by embodiment, the present invention is specifically described.
Embodiment 1
A method for cationic sterilant is prepared in sewer oil modification, comprises the following steps:
The first step: sewer oil is heated to 50 DEG C, filtered while hot, remove wherein insolubles, filtrate is joined in the first reaction vessel, add isopyknic mass concentration 4% aqueous sulfuric acid, heat up stirring reaction 6h under the condition of 85 DEG C, after reaction system is down to room temperature, leave standstill separatory, oil phase to use after isopyknic washing three times to obtain acidifying sewer oil;
Second step: acidifying sewer oil is joined in the second reaction vessel, add 1 of equimolar ratio example successively, 2-glycidyl trimethyl ammonium chloride and dioxane, with stirring reaction 12h under the condition of 50 DEG C, after having reacted, remove dioxane, namely solid residue obtains the cationic sterilant based on sewer oil modification after using acetone recrystallization.
Embodiment 2
A method for cationic sterilant is prepared in sewer oil modification, comprises the following steps:
The first step: sewer oil is heated to 60 DEG C, filtered while hot, remove wherein insolubles, filtrate is joined in the first reaction vessel, add isopyknic mass concentration 4% aqueous sulfuric acid, heat up stirring reaction 7h under the condition of 85 DEG C, after reaction system is down to room temperature, leave standstill separatory, oil phase to use after isopyknic washing three times to obtain acidifying sewer oil;
Second step: acidifying sewer oil is joined in the second reaction vessel, add 1 of equimolar ratio example successively, 2-glycidyl trimethyl ammonium chloride and tetrahydrofuran (THF), stirring reaction 10h under the condition of 60 DEG C, after having reacted, remove tetrahydrofuran (THF), namely solid residue obtains the cationic sterilant based on sewer oil modification after using acetone recrystallization.
Embodiment 3
A method for cationic sterilant is prepared in sewer oil modification, comprises the following steps:
The first step: sewer oil is heated to 50 DEG C, filtered while hot, remove wherein insolubles, filtrate is joined in the first reaction vessel, add isopyknic mass concentration 3% aqueous sulfuric acid, heat up stirring reaction 8h under the condition of 85 DEG C, after reaction system is down to room temperature, leave standstill separatory, oil phase to use after isopyknic washing three times to obtain acidifying sewer oil;
Second step: acidifying sewer oil is joined in the second reaction vessel, add 1 of equimolar ratio example successively, 2-glycidyl trimethyl ammonium chloride and dioxane, stirring reaction 15h under the condition of 40 DEG C, after having reacted, remove dioxane, namely solid residue obtains the cationic sterilant based on sewer oil modification after using acetone recrystallization.
The present embodiment, only for being further detailed the present invention, can not be interpreted as the restriction of protection domain, and the person skilled in the art of this area makes some nonessential improvement according to content of the present invention and adjustment also belongs to protection scope of the present invention.
Claims (4)
1. a method for cationic sterilant is prepared in sewer oil modification, it is characterized in that, comprises the following steps:
The first step: sewer oil is heated to 50-70 DEG C, filtered while hot, remove wherein insolubles, filtrate is joined in the first reaction vessel, add isopyknic mass concentration 3-5% aqueous sulfuric acid, heat up stirring reaction 5-8h under the condition of 85 DEG C, after reaction system is down to room temperature, leave standstill separatory, oil phase to use after isopyknic washing three times to obtain acidifying sewer oil;
Second step: acidifying sewer oil is joined in the second reaction vessel, add 1 of equimolar ratio example successively, 2-glycidyl trimethyl ammonium chloride and reaction solvent, stirring reaction 8-15h under the condition of 40-60 DEG C, after having reacted, remove reaction solvent, namely solid residue obtains the cationic sterilant based on sewer oil modification after using acetone recrystallization, described reaction solvent is tetrahydrofuran (THF) or dioxane, and both mixed solvents.
2. the method for cationic sterilant is prepared in a kind of sewer oil modification according to claim 1, it is characterized in that, comprises the following steps:
The first step: sewer oil is heated to 50 DEG C, filtered while hot, remove wherein insolubles, filtrate is joined in the first reaction vessel, add isopyknic mass concentration 4% aqueous sulfuric acid, heat up stirring reaction 6h under the condition of 85 DEG C, after reaction system is down to room temperature, leave standstill separatory, oil phase to use after isopyknic washing three times to obtain acidifying sewer oil;
Second step: acidifying sewer oil is joined in the second reaction vessel, add 1 of equimolar ratio example successively, 2-glycidyl trimethyl ammonium chloride and dioxane, stirring reaction 12h under the condition of 50 DEG C, after having reacted, remove dioxane, namely solid residue obtains the cationic sterilant based on sewer oil modification after using acetone recrystallization.
3. the method for cationic sterilant is prepared in a kind of sewer oil modification according to claim 1, it is characterized in that, comprises the following steps:
The first step: sewer oil is heated to 60 DEG C, filtered while hot, remove wherein insolubles, filtrate is joined in the first reaction vessel, add isopyknic mass concentration 4% aqueous sulfuric acid, heat up stirring reaction 7h under the condition of 85 DEG C, after reaction system is down to room temperature, leave standstill separatory, oil phase to use after isopyknic washing three times to obtain acidifying sewer oil;
Second step: acidifying sewer oil is joined in the second reaction vessel, add 1 of equimolar ratio example successively, 2-glycidyl trimethyl ammonium chloride and tetrahydrofuran (THF), stirring reaction 10h under the condition of 60 DEG C, after having reacted, remove tetrahydrofuran (THF), namely solid residue obtains the cationic sterilant based on sewer oil modification after using acetone recrystallization.
4. the method for cationic sterilant is prepared in a kind of sewer oil modification according to claim 1, it is characterized in that, comprises the following steps:
The first step: sewer oil is heated to 50 DEG C, filtered while hot, remove wherein insolubles, filtrate is joined in the first reaction vessel, add isopyknic mass concentration 3% aqueous sulfuric acid, heat up stirring reaction 8h under the condition of 85 DEG C, after reaction system is down to room temperature, leave standstill separatory, oil phase to use after isopyknic washing three times to obtain acidifying sewer oil;
Second step: acidifying sewer oil is joined in the second reaction vessel, add 1 of equimolar ratio example successively, 2-glycidyl trimethyl ammonium chloride and dioxane, stirring reaction 15h under the condition of 40 DEG C, after having reacted, remove dioxane, namely solid residue obtains the cationic sterilant based on sewer oil modification after using acetone recrystallization.
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| CN105176693B (en) * | 2015-09-23 | 2019-03-26 | 西京学院 | A kind of preparation method of the antistatic agent based on polyhydroxy gutter oil quaternary ammonium salt |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102586029A (en) * | 2012-01-05 | 2012-07-18 | 上虞市精细化工厂 | Preparation method of easily-degraded esterquat softening agent |
| CN103828814A (en) * | 2014-03-05 | 2014-06-04 | 陕西省蒲城美尔果农化有限责任公司 | Fruit tree sterilization coating agent prepared from swill-cooked dirty oil and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102586029A (en) * | 2012-01-05 | 2012-07-18 | 上虞市精细化工厂 | Preparation method of easily-degraded esterquat softening agent |
| CN103828814A (en) * | 2014-03-05 | 2014-06-04 | 陕西省蒲城美尔果农化有限责任公司 | Fruit tree sterilization coating agent prepared from swill-cooked dirty oil and preparation method thereof |
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