CN104365587B - A kind of method making water emulsification type carboxylic acids pesticide - Google Patents
A kind of method making water emulsification type carboxylic acids pesticide Download PDFInfo
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- CN104365587B CN104365587B CN201310356590.7A CN201310356590A CN104365587B CN 104365587 B CN104365587 B CN 104365587B CN 201310356590 A CN201310356590 A CN 201310356590A CN 104365587 B CN104365587 B CN 104365587B
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Abstract
A kind of method that the invention discloses carboxylic acids pesticide water emulsifying, including two parts: 1) long-chain is secondary, tertiary amine is mixed homogeneously under stirring in water with carboxylic acids pesticide；2) or long-chain is secondary, tertiary amine is dispersed in water respectively with carboxylic acids pesticide, the two is mixed to prepare aqueous emulsion mutually.5% 35% are reached according to carboxylic acids pesticide concentration in the carboxylic acids pesticide emulsion in water prepared by this method.The emulsion that the present invention generates makes more carboxylic acids pesticide be dispersed, and makes the dissolubility increase in water of the carboxylic acids pesticide, stability increase under conditions of not carrying out complex operations.
Description
Technical field
The present invention relates to carboxylic acids pesticide, a kind of method making water emulsification type carboxylic acids pesticide.
Background technology
Carboxylic acids pesticide, because water solublity or water dispersible are the best, often adds amine such as during former medicine post-production
Ammonia, triethylamine etc. are prepared as salt form pesticide to be prepared as water preparation and using, but this dissolubility that can not solve pesticide limits
Problem, to the processing of pesticide, transports, uses and make troubles.Therefore, find a kind of method solve this kind of pesticide water dispersible and
In water the stability problem of dispersion obviously to carboxylic acids pesticidal preparations produce and use all have suitable.
Summary of the invention
It is an object of the invention to provide a kind of simple to operate, it is easy to prepare carboxylic acids pesticide high-concentration aqueous emulsion or be prone to
The method making water emulsification type carboxylic acids pesticide of water emulsification.
For achieving the above object, the technical solution used in the present invention is:
A kind of method making water emulsification type carboxylic acids pesticide:
1. long-chain is secondary, tertiary amine in synthesis: utilize long-chain halogenated hydrocarbons or long-chain alcohol ester and primary amine or secondary amine in toluene equal solvent
React (list of references: Org.Synth., 1973, Coll.Vol5,124.), or long-chain aldehyde mixes with primary amine or secondary amine, in reduction
Agent or the lower hydrogenation of metallic catalyst catalysis obtain that long-chain is secondary, tertiary amine (list of references: Org.Synth., 1988, Coll.Vol6,
499；Org.Synth., 1963, Coll.Vol4,603.), long-chain is secondary, tertiary amine formula is:
In formula: R1 is C8-18Alkyl, R2, R3 are hydrogen or C1-5Alkyl, R2, R3 can be the same or different, but can not be with
Time be hydrogen.
2. the method making water emulsification type carboxylic acids pesticide:
Long-chain is secondary, tertiary amine is mixed homogeneously under stirring in water with carboxylic acids pesticide and prepared aqueous emulsion,
Or long-chain is secondary, tertiary amine is dispersed in water respectively with carboxylic acids pesticide, and the latter two phases are mixed to prepare aqueous emulsion；
Or long-chain is secondary, tertiary amine is mixed homogeneously under ultrasonic assistant in water with carboxylic acids pesticide and prepared aqueous emulsion.
Described carboxylic acids pesticide is the pesticide at least containing a carboxyl.
Further, described long-chain is secondary, tertiary amine is at least to contain a C8-18Amine.
In described water emulsification type carboxylic acids pesticide, the weight/mass percentage composition of carboxylic acids pesticide is 5%-35%.
Further, in described water emulsification type carboxylic acids pesticide, long-chain weight/mass percentage composition secondary, tertiary amine is 5%-35%.
In described water emulsification type carboxylic acids pesticide, carboxylic acids pesticide and long-chain mol ratio secondary, tertiary amine are 3/1-1/1.
The representative example of the present invention is for utilizing N, and N-diethyl-cetylamine is mixed with mutually with imazapic
The method of aqueous emulsion.
The concrete operations of the present invention are as follows: with imazapic and N, as a example by N-diethyl-cetylamine.
Imazapic etc., N, N-diethyl-cetylamine etc. are joined in deionized water, is stirred at room temperature 1 hour
Or ultrasonic wave concussion 20 minutes；Or imazapic etc. and N, N-diethyl-cetylamine etc. are scattered in deionization respectively
In water, mixed at room temperature also stirs 1 hour or ultrasonic wave concussion 20 minutes；It is prepared as water emulsifier, the aqueous emulsion thus prepared
Can the most instant join, it is also possible to place three months after preparation and have no significant change.
It has been found that carboxylic acids pesticide and long-chain is secondary, tertiary amine formed aqueous emulsion, wherein the percent mass of carboxylic acids pesticide contains
Amount is 5%-35%, and long-chain is secondary, the weight/mass percentage composition of tertiary amine is 5%-35%；Carboxylic acids pesticide is secondary with long-chain, the ratio of tertiary amine is
3/1-1/1(mol/mol).
Advantage for present invention:
The present invention by using long chain tertiary amine, and by the length changing two other carbochain of secondary, tertiary amine make tertiary amine with
Carboxylic acids pesticide becomes the intensity of salt to change, and makes the intrinsic water-soluble of carboxylic acids pesticide reduce further, so that secondary, uncle
The salt that amine and carboxylic acids pesticide generate has more surface activity and generates emulsion in water, and the emulsion of generation makes more carboxylic acid
Class pesticide is dispersed, and makes carboxylic acids pesticide dissolubility in water increase, stablize under conditions of not carrying out complex operations
Property increase.
Accompanying drawing explanation
The Imazethapyr aqueous emulsion picture that Fig. 1 provides for the embodiment of the present invention；
The imazapic aqueous emulsion picture that Fig. 2 provides for the embodiment of the present invention；
The Imazethapyr aqueous emulsion picture that Fig. 3 provides for the embodiment of the present invention；
The Imazethapyr aqueous emulsion picture that Fig. 4 provides for the embodiment of the present invention；
The glyphosate aqueous emulsion picture that Fig. 5 provides for the embodiment of the present invention；
The glyphosate aqueous emulsion picture that Fig. 6 provides for the embodiment of the present invention；
The glyphosate aqueous emulsion picture that Fig. 7 provides for the embodiment of the present invention；
The glyphosate aqueous emulsion picture that Fig. 8 provides for the embodiment of the present invention；
The glyphosate aqueous emulsion picture that Fig. 9 provides for the embodiment of the present invention.
Detailed description of the invention
Embodiment described below carboxylic acids pesticide is used for further describing the present invention, it is not limited to these are implemented
Example carboxylic acids pesticide.In these embodiments, unless specifically stated otherwise, carboxylic acids pesticide used, long-chain be secondary, tertiary amine, water with gram
G () measures.
Embodiment 1
1.45g Imazethapyr is scattered in 10g distilled water, adds 1.35g N, N-dimethyl-cetylamine, be stirred at room temperature
1 hour.Or 1.45g Imazethapyr is scattered in 10g distilled water, add 1.35gN, N-dimethyl-cetylamine, ultrasonic vibration
20 minutes, stand.See Fig. 1 after gained aqueous emulsion sample is placed February, have no sample emulsion significant change.
Embodiment 2
1.38g imazapic is scattered in 10g distilled water, adds 1.49g N, N-diethyl-cetylamine, room temperature
Stir 1 hour.Or 1.45g Imazethapyr is scattered in 10g distilled water, add 1.49g N, N-diethyl-cetylamine, ultrasonic
Shake 20 minutes, stand.Seeing Fig. 2 after gained aqueous emulsion sample is placed March, emulsion is still obvious, has no sample breast
Change phenomenon significant change.
Embodiment 3
1.45g Imazethapyr is scattered in 10g distilled water, 1.49g N, N-diethyl-cetylamine, it is stirred at room temperature 1 little
Time.Or 1.45g Imazethapyr is scattered in 10g distilled water, 1.49g N, N-diethyl-cetylamine, ultrasonic vibration 20 minutes,
Stand.Emulsion is obvious, sees Fig. 3.
Embodiment 4
1.45g Imazethapyr is scattered in 10g distilled water, adds 1.07g N, N-dimethyl-dodecylamine amine, be stirred at room temperature
1 hour.Or 1.45g Imazethapyr is scattered in 10g distilled water, add 1.07gN, N-dimethyl-dodecylamine amine, ultrasonic vibration
15 minutes, stand.Emulsion is obvious, sees Fig. 4.
Embodiment 5
0.85g glyphosate is scattered in 10g distilled water, adds 1.77g N, N-dibutyl-cetylamine, be stirred at room temperature
0.5 hour.Or 0.85g glyphosate is scattered in 10g distilled water, add 1.77g N, N-dibutyl-cetylamine, ultrasonic shake
Swing 15 minutes, stand.Emulsion is obvious, sees Fig. 5.
Embodiment 6
0.85g glyphosate is scattered in 10g distilled water, adds 1.49g N, N-dibutyl-dodecyl amine, be stirred at room temperature
0.5 hour.Or 0.85g glyphosate is scattered in 10g distilled water, add 1.49g N, N-dibutyl-dodecyl amine, ultrasonic shake
Swing 15 minutes, stand.See Fig. 6.Seeing Fig. 6 after gained aqueous emulsion sample is placed February, emulsion is the most obvious.
Embodiment 7
0.85g glyphosate is scattered in 10g distilled water, adds 1.49g N, N-diethyl-cetylamine, be stirred at room temperature
0.5 hour.Or 0.85g glyphosate is scattered in 10g distilled water, add 1.49g N, N-diethyl-cetylamine, ultrasonic shake
Swing 15 minutes, stand.Emulsion is obvious, sees Fig. 7.
Embodiment 8
0.85g glyphosate is scattered in 10g distilled water, adds 1.34g N-ethyl-cetylamine, be stirred at room temperature 0.5
Hour.Or 0.85g glyphosate is scattered in 10g distilled water, add 1.34gN-ethyl-cetylamine, ultrasonic vibration 15 points
Clock, stands.Emulsion is obvious, sees Fig. 8.
Embodiment 9
4.04g glyphosate is scattered in 10g distilled water, adds 4.05g N, N-dimethyl-cetylamine, be stirred at room temperature
0.5 hour.Or 4.04g glyphosate is scattered in 10g distilled water, add 4.05g N, N-dimethyl-cetylamine, ultrasonic shake
Swing 10 minutes, stand.See Fig. 9.See Fig. 9 after gained aqueous emulsion sample is placed January, have no sample significant change.
Claims (4)
1. the method making water emulsification type carboxylic acids pesticide, it is characterised in that:
Long-chain is secondary, tertiary amine is mixed homogeneously under stirring in water with carboxylic acids pesticide and prepared aqueous emulsion；
Or long-chain is secondary, tertiary amine is dispersed in water respectively with carboxylic acids pesticide, and the latter two phases are mixed to prepare aqueous emulsion；
Or long-chain is secondary, tertiary amine is mixed homogeneously under ultrasonic assistant in water with carboxylic acids pesticide and prepared aqueous emulsion；
Described long-chain is secondary, tertiary amine is combined as with carboxylic acids pesticide: Imazethapyr and N, N-dimethyl-cetylamine, methyl miaow grass
Cigarette and N, N-diethyl-cetylamine, Imazethapyr and N, N-diethyl-cetylamine, Imazethapyr and N, N-dimethyl-dodecylamine
Amine, glyphosate and N, N-dibutyl-cetylamine, glyphosate and N, N-dibutyl-dodecyl amine, glyphosate and N, N-diethyl
Base-cetylamine, glyphosate and N-ethyl-cetylamine, glyphosate and N, N-dimethyl-cetylamine.
2. according to the method making water emulsification type carboxylic acids pesticide described in claim 1, it is characterised in that: described water emulsification type
In carboxylic acids pesticide, the weight/mass percentage composition of carboxylic acids pesticide is 5%-35%.
3. according to the method making water emulsification type carboxylic acids pesticide described in claim 1, it is characterised in that: described water emulsification type
In carboxylic acids pesticide, long-chain weight/mass percentage composition secondary, tertiary amine is 5%-35%.
4. according to the method making water emulsification type carboxylic acids pesticide described in claim 1, it is characterised in that: described water emulsification type
In carboxylic acids pesticide, carboxylic acids pesticide and long-chain mol ratio secondary, tertiary amine are 3/1-1/1.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0074329A3 (en) * | 1981-09-09 | 1984-03-28 | Ciba-Geigy Ag | Aqueous concentrates of pesticides |
| CN102805101A (en) * | 2012-09-06 | 2012-12-05 | 江苏龙灯化学有限公司 | Weeding combination containing glyphosate, fomesafen and pyraflufen-ethyl and application thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0733618A (en) * | 1993-07-22 | 1995-02-03 | Kubota Corp | Nematicide preparation and method for using the same |
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2013
- 2013-08-15 CN CN201310356590.7A patent/CN104365587B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0074329A3 (en) * | 1981-09-09 | 1984-03-28 | Ciba-Geigy Ag | Aqueous concentrates of pesticides |
| CN102805101A (en) * | 2012-09-06 | 2012-12-05 | 江苏龙灯化学有限公司 | Weeding combination containing glyphosate, fomesafen and pyraflufen-ethyl and application thereof |
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| CN104365587A (en) | 2015-02-25 |
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