CN1130176A - Alkyl-dimethyl-2-(sulfurous acid) ethyl ammonium and its preparing method - Google Patents
Alkyl-dimethyl-2-(sulfurous acid) ethyl ammonium and its preparing method Download PDFInfo
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- CN1130176A CN1130176A CN 95112809 CN95112809A CN1130176A CN 1130176 A CN1130176 A CN 1130176A CN 95112809 CN95112809 CN 95112809 CN 95112809 A CN95112809 A CN 95112809A CN 1130176 A CN1130176 A CN 1130176A
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- sulfurous acid
- ethyl ammonium
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Abstract
The present invention relates to a kind of bactericide for treatment of the industrial circulation water and the preparation thereof. It is composed of ethylene sulfite and 10-20 carbon nitrile base in the molar ratio of 1:0.8-1.2.
Description
The present invention relates to a kind of water treatment biocide and preparation method thereof, particularly water treatment biocide in the industrial circulating water and preparation method thereof.
In underground water, rivers and lakes water and soil, all contain a kind of sulphate reducing bacteria (Sulfate reducing bacteria is called for short SRB).This is a kind of anerobe, and is higher with content in underground water and the soil especially.SRB can become hydrosulphuric acid (H2S) to sulfate reduction, and the hydrosulphuric acid of generation is a kind of weak acid, and iron and steel is had the oil production of intensive corrosive nature, majority is a secondary oil recovery, that have or even tertiary oil recovery wants to inject earlier a large amount of water in well during oil recovery, oil and water are released simultaneously again.This water filling, in northern China or the Northwest, most use underground water, and also after the profit extraction, behind the branch oil-yielding stratum, water will continue to recycle.Contain a large amount of SRB in such water filling and the cycling use of water.In aboveground down-hole, on the ground and the pipeline of subterranean equipment and conveying very strong corrosive nature is arranged.SRB is the formidable enemy of oil exploration industry.Equally, petrochemical plant, fertilizer plant, the unit of a large amount of use recirculated water such as heat power plant also is subjected to the harm of SRB deeply, and these used water all will pass through germicidal treatment earlier.The general the easiest method of sterilization is to feed chlorine to water or the chlorination goods, and SRB has the intensive reductibility, and chlorine and chlorine goods are oxygenant, so SRB can make chlorine lose efficacy, and self survival is fine.For this reason, China at present the most frequently used medicament of killing SRB is dodecyl benzyl dimethyl ammonium chloride (industrial be called 1227 or geramine), because 1227 use for many years, SRB has produced resistance.Have only 1227 using dosages of increasing, just produce effect.Be (being ten thousand heavy/above consumption of water) more than the 100ppm as 1227 pharmaceutical quantities of adding in China's domestic oil field water.Use cost is increased, and economic benefit is low.Purpose of the present invention is exactly in order to address the above problem, and proposes high alkyl dimethyl-2-(sulfurous acid) ethyl ammonium of the good economic benefit of a kind of sterilization effect and preparation method thereof.
Technical solution of the present invention:
A kind of alkyl dimethyl-2-(sulfurous acid) ethyl ammonium is characterized in that it is made through mixing, reacting by heating by the tertiary amine of sulfurous acid ethylene ester and 10-20 carbon, and the mol ratio of its two kinds of compositions is:
The tertiary amine of 10-20 carbon: sulfurous acid ethylene ester is 1: 0.8-1.2.
The general formula of molecular structure of its product is:
R=8-18 wherein.
The preparation method of a kind of alkyl dimethyl-2-(sulfurous acid) ethyl ammonium is characterized in that first tertiary amine with 10-20 carbon mixes in reactor with sulfurous acid ethylene ester, and reacting by heating promptly obtains product of the present invention under 50-120 ℃ temperature condition again.
The present invention is a raw material with the tertiary amine and the sulfurous acid ethylene ester of 10-20 carbon, makes the sterilant of brand new, and the usage quantity of killing SRB significantly reduces, and only is 1/10th to 1/5th of 1227 medicaments, and economic benefit improves greatly.
Product of the present invention also has following advantage:
1, germ-killing efficiency height, production technique is also simple.
2, corrosion inhibition is preferably arranged, the consumption of inhibition water conditioner in the time that water treatment can being reduced.
When 3, being used, can not produce precipitation with other water conditioner (inhibiter, Scale inhibitors) etc.Thereby compatibility is good.
4, it is a kind of wide-spectrum bactericide, if usage quantity is 0.5-1ppm, can kill intestinal bacteria etc. immediately, and other anerobe is killed.This product self toxicity is minimum.1227 LD
50Be 50 milligrams/kilogram (big white mouse), this product LD
50Be 2500 milligrams/kilogram (big white mouse), harmless substantially to people and domestic animal etc.
5, solve old product 1227 and be insoluble in water, earlier water-soluble 1227 in advance, be made into 50% aqueous solution packed and transported again, the problem that transportation is easily leaked and traffic capacity increases.It can solid-stately be transported to uses on-the-spot interim preparation, easy to use, has also reduced traffic capacity.
Technological process of the present invention is:
1, prepares intermediate---sulfurous acid ethylene ester earlier
Raw material: ethylene glycol, sulfur oxychloride (thionyl chloride)
Promptly obtain intermediate sulfurous acid ethylene ester.
Concrete grammar is elder generation's adding ethylene glycol, drips the sulfur oxychloride of equimolar amount, and dropping under insulation earlier has a large amount of hydrogenchloride during dropping, and water secondary or three absorptions are in case a large amount of polluted air.Be warming up to 80 ℃ after dropwising gradually, treat that hydrogenchloride is no longer emitted after, the underpressure distillation that heats up again, colourless liquid be intermediate sulfurous acid ethylene ester.Residue has strong tearing property to discard.
2, the tertiary amine of 10-20 carbon generates this product and homologue with the intermediate reaction again.These homologues, the same with this product all have an identical sterilizing ability.Be example with 16 tertiary amines, 12 tertiary amines, 14 tertiary amines below, its chemical equation is respectively:
Obtain hexadecyldimethyl benzyl ammonium-2-(sulfurous acid) ethyl ammonium.
Obtain dodecyl dimethyl-2-(sulfurous acid) ethyl ammonium.
Obtain tetradecyl dimethyl-2-(sulfurous acid) ethyl ammonium.
Concrete grammar is to add tertiary amine earlier, adds intermediate sulfurous acid ethylene ester more gradually, after the agitation and dropping intermediate finishes, is warming up to 97 ℃, gets the higher magma of viscosity.Be cooled to about 70 ℃, can emit this product and homologue.Be the very big decorating film of viscosity after the cooling.
Among the present invention, the best proportioning of the tertiary amine of 10-20 carbon and sulfurous acid ethylene ester is 1: 1.The number of alkyl R the best is 12-16 in the general formula of molecular structure of its product.In the preparation method, the temperature of its reacting by heating the best is 90-100 ℃.
Embodiment:
1, preparation intermediate sulfurous acid ethylene ester (is example with the 1mol intermediate):
Get 75 gram ethylene glycol (1mol), place three-necked bottle, from dropping funnel, drip 140 gram (1mol) sulfur oxychlorides, derive the hydrogenchloride of emitting in the reaction with conduit.After dropwising under the room temperature, warming-in-water, when treating that hydrogenchloride is no longer emitted, reheat and underpressure distillation.Obtain the sulfurous acid ethylene ester colourless transparent liquid of about 108 gram 1mol.
2, system hexadecyldimethyl benzyl ammonium-2-(sulfurous acid) ethyl ammonium: in three-necked bottle, add 269 gram (1mol) hexadecyldimethyl benzyl ammonium amine (industrial abbreviation 16 tertiary amines) earlier, by adding 108 gram (1mol) sulfurous acid ethylene esters in the dropping funnel, heating in water bath to 97 ℃ stirring, pour out after becoming viscous fluid, be product of the present invention.
3, system dodecyl dimethyl-2-(sulfurous acid) ethyl ammonium:
Elder generation adds 213 gram (1mol) dodecyl dimethyl amine (industrial abbreviation 12 tertiary amines) in three-necked bottle, and by adding 108 gram (1mol) sulfurous acid ethylene esters in the dropping funnel, heating in water bath to 97 ℃ stirring is poured out after the one-tenth viscous fluid, is product of the present invention.
4, system tetradecyl dimethyl-2-(sulfurous acid) ethyl ammonium:
Elder generation adds 241 gram (1mol) tetradecyl dimethyl amines (industrial abbreviation 14 tertiary amines) in three-necked bottle, and by adding 108 gram (1mol) sulfurous acid ethylene esters in the dropping funnel, heating in water bath to 97 ℃ stirring is poured out after the one-tenth viscous fluid, is product of the present invention.
The present invention also can add an amount of solvent in reaction process, make reaction more all even thoroughly.
Claims (6)
1, a kind of alkyl dimethyl-2-(sulfurous acid) ethyl ammonium is characterized in that it is made through mixing, reacting by heating by the tertiary amine of sulfurous acid ethylene ester and 10-20 carbon, and the mol ratio of its two kinds of compositions is:
The tertiary amine of 10-20 carbon: sulfurous acid ethylene ester is 1: 0.8--1.2.
The general formula of molecular structure of its product is:
R=8-18 wherein.
2, by the described alkyl dimethyl-2-of claim 1 (sulfurous acid) ethyl ammonium, it is characterized in that the tertiary amine of 10-20 carbon and the best proportioning of sulfurous acid ethylene ester are 1: 1.
3,, it is characterized in that the number of the alkyl R in its general formula of molecular structure is best and be 12-16 by the described alkyl dimethyl-2-of claim 1 (sulfurous acid) ethyl ammonium.
4, the preparation method of a kind of alkyl dimethyl-2-(sulfurous acid) ethyl ammonium is characterized in that first tertiary amine with 10-20 carbon mixes in reactor with sulfurous acid ethylene ester, and reacting by heating promptly obtains product of the present invention under 50-120 ℃ temperature condition again.
5,, it is characterized in that the temperature of its reacting by heating is best for 90-100 ℃ by the preparation method of the described alkyl dimethyl-2-of claim 4 (sulfurous acid) ethyl ammonium
6, by the preparation method of the described alkyl dimethyl-2-of claim 4 (sulfurous acid) ethyl ammonium, it is characterized in that and in reaction process, to add an amount of solvent, make reaction more all even thoroughly.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 95112809 CN1130176A (en) | 1995-12-15 | 1995-12-15 | Alkyl-dimethyl-2-(sulfurous acid) ethyl ammonium and its preparing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 95112809 CN1130176A (en) | 1995-12-15 | 1995-12-15 | Alkyl-dimethyl-2-(sulfurous acid) ethyl ammonium and its preparing method |
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| Publication Number | Publication Date |
|---|---|
| CN1130176A true CN1130176A (en) | 1996-09-04 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 95112809 Pending CN1130176A (en) | 1995-12-15 | 1995-12-15 | Alkyl-dimethyl-2-(sulfurous acid) ethyl ammonium and its preparing method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104725320A (en) * | 2015-01-05 | 2015-06-24 | 西南石油大学 | Sulfitonetaine sterilizing agent and synthetic method thereof |
-
1995
- 1995-12-15 CN CN 95112809 patent/CN1130176A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104725320A (en) * | 2015-01-05 | 2015-06-24 | 西南石油大学 | Sulfitonetaine sterilizing agent and synthetic method thereof |
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