CN1515151A - Special-purpose adjuvant for pesticide suspension agent and its preparation method - Google Patents
Special-purpose adjuvant for pesticide suspension agent and its preparation method Download PDFInfo
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- CN1515151A CN1515151A CNA031528333A CN03152833A CN1515151A CN 1515151 A CN1515151 A CN 1515151A CN A031528333 A CNA031528333 A CN A031528333A CN 03152833 A CN03152833 A CN 03152833A CN 1515151 A CN1515151 A CN 1515151A
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Abstract
The present invention relates to a special-purpose adjuvant for pesticide suspension agent and its preparation method. The special-purpose adjuvant is made up by using dispersing agent and moistening agent according to the ratio of 1:10-10:1 through the process of compounding them. Its preparation method includes the following steps: (1), adding phenethyl phenol formaldehyde resin into polymerization still, adding catalyst, introducing nitrogen gas and vacuum dewatering; (2) continuously introducing epoxy ethane at 140-170 deg.C, then ageing, pressure-reducing and removing small molecule and volatile matter, cooling to below 100 deg.c and making neutralization to obtain phenethyl phenol formaldehyde resin polyoxyethylene other; (3) making the above-mentioned product and esterifying agent implement esterification reaction; (4). after the esterification reaction is completed, using organic alkali to make neutralization, after the pH value is reached to 6-8, removing water and filtering to obtain dispersing agent; and (5). mixing the dispersing agent with moistening agent according to a certain ratio.
Description
Background technology
Insecticides adjuvant is the general name of other adminiclies except that pesticide active ingredient of use in pesticide processing preparation and the application, is indispensable important component in the pesticidal preparations processing.Along with the development of pesticides new formulation efficiently of safety and environmental protection low toxicity, more requirement has corresponding novelty, auxiliary agent is supporting with it efficiently in recent years.
At present, the auxiliary agent of domestic pesticidal preparations is based on traditional non-ionic surface active agent basically, because electrostatic repulsion forces can not be provided simultaneously, the preparation physical stability that is made into is undesirable, the products solidifying that vast scale often occurs has had a strong impact on the use of Pesticidal products.
The auxiliary agent of external pesticidal preparations generally is made up of dispersant and wetting agent, based on dispersant.Especially wherein the anionic dispersing agents that has nonionic character, not only has good wetability, can be by the orientation absorption of surfactant, reduce the surface tension between solid, liquid, being convenient to solids can be wetting fully by water, also help particle cluster dispersion or spallation and become tiny particle, increased the energy barrier that prevents that the medicine grain from reassembling, thereby can stop the coalescent again of medicine grain preferably.Be applied in the pesticidal preparations, the product physicochemical property is good, stores after 2 years, except slight bleed layer is arranged, does not solidify phenomenon.Through rocking, still can recover even attitude, but the cost of external auxiliary agent is higher.
Summary of the invention
The technical problem to be solved in the present invention is the undesirable or problem that cost is too high of existing auxiliary agent physical stability, for people provide a kind of physical property ideal, and the special assistant of lower-cost agricultural chemicals suspension agent and preparation method thereof.
For solving the problems of the technologies described above, the present invention is the novel anionic dispersant that has nonionic character concurrently of our exploitation at first, with formaldehyde phenethyl phenol chain is coupled together, make the lipophilic group part itself possess the branching type structure, oxirane with suitable mol ratio carries out polymerisation again, and with its esterification, in become novel dispersant with modification, then with aforementioned dispersant and wetting agent in 1: 10-10: 1 ratio is composite, promptly obtains the present invention.Its preparation technology comprises the steps:
(1) the phenethyl phenol formaldehyde resin is added in the polymeric kettle, add the alkali metal potassium hydroxide catalyst again, the vacuum dehydration of drum nitrogen;
(2) carry out polymerisation at 140～170 ℃ of oxirane that feed continuously, reaction finishes after aging decompression removes little molecule and volatile matter, is cooled to neutralization below 100 ℃ again, generates phenethyl phenol formaldehyde resin APEO;
(3) phenethyl phenol formaldehyde resin APEO and esterifying agent are carried out esterification;
(4) after esterification is finished,, after the pH value reaches 6～8, deviate from moisture content, get dispersant after handling after filtration with the organic base neutralization.
(5) the dispersion powder that above-mentioned steps is made and wetting agent mix in proportion.
In above-mentioned processing step (1), phenethyl phenol formaldehyde resin and oxirane mol ratio are 1: 10-1: 50, and optimum mole ratio is 1: 15-1: 30; The time of drum nitrogen vacuum dehydration is 30 minutes, and catalyst amount is the 0.1%-0.7% of phenethyl phenol formaldehyde resin and oxirane gross weight.
Time aging in above-mentioned processing step (2) is 20～60 minutes.
The mol ratio of phenethyl phenol formaldehyde resin APEO and esterifying agent is 2.3 in above-mentioned processing step (3): 1-4: 1, and esterifying agent can be P
2O
5, PCl
3, POCl
3In any one, esterification temperature is 50-100 ℃, esterification time is 2-8 hour.
Organic base in above-mentioned processing step (4) can be any one in ammoniacal liquor, diethanol amine, triethanolamine, diethylenetriamine, the triethylene tetramine.
Intermediate product dispersant of the present invention is a phenethyl phenol formaldehyde resin polyoxyethylene ether phosphate salt, and it has following structural formula:
The preferred proportion of dispersant of the present invention and wetting agent is: 1: 5-5: 1.
The present invention has adopted the novel anionic dispersant that has nonionic character concurrently, thisly phenethyl phenol chain is coupled together with formaldehyde, make the lipophilic group part itself possess the branching type structure and make that like this molecular structure of this product is better, the physical stability of water-based property preparation is better.Design of the present invention has broken through domestic general traditional idea (nonionic and calcium salt are composite), but presses general in the world being made up of novel dispersant and wetting agent, and both bring into play synergistic effect, can further improve the physicochemical property of preparation.Solved and perplexed domestic suspending agent layering, problem of solidification for a long time, filled up the blank of domestic water base property preparation special assistant, its cost also more abroad significantly reduces with analog assistant simultaneously.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1:
(1) the phenethyl phenol formaldehyde resin is metered in the polymeric kettle, adds 0.1% alkali metal potassium hydroxide catalyst, drum nitrogen vacuum dehydration 30 minutes;
(2) be that 1: 10 ratio feeds continuously oxirane at 140 ℃ and carries out polymerisation in phenethyl phenol formaldehyde resin and oxirane mol ratio, reaction finished the back aging 20 minutes, and decompression removes little molecule and volatile matter then; Be cooled to neutralization below 100 ℃, generate phenethyl phenol formaldehyde resin APEO, detection PH, cloud point, moisture are respectively 76 ℃ of cloud points, moisture 0.35%, PH6.12;
(3) with phenethyl phenol formaldehyde resin APEO and esterifying agent P
2O
5Be 2.3: 1 ratio esterification 2 hours under 50 ℃ temperature in molar ratio;
(4) after esterification is finished, neutralize, after the pH value reaches 6～8, deviate from moisture content, get dispersant after handling after filtration with ammoniacal liquor.
Actual measurement dispersant quality index data: working substance content 97.1%, moisture 1.05%, PH6.56
(5) dispersant that above-mentioned steps is made and wetting agent fatty alcohol-polyoxyethylene ether are composite in 4: 1 ratio.
Embodiment 2:
Processing step and the embodiment of embodiment 2 are identical, and no is
Catalyst amount is 0.3% in the step (1);
Phenethyl phenol formaldehyde resin and oxirane mol ratio are 1: 20 in the step (2), polymerization temperature is 150 ℃, ageing time is 40 minutes, and the quality index data that polymerisation finishes back actual measurement phenethyl phenol formaldehyde resin APEO is: 97 ℃ of cloud points, moisture 0.21%, PH5.96;
The mol ratio of phenethyl phenol formaldehyde resin APEO and esterifying agent is 3: 1 in the step (3), and esterifying agent is PCl
3, esterification temperature is 80 ℃, esterification time is 5 hours;
Organic base is a diethanol amine in the step (4), and actual measurement dispersant quality index data is: working substance content 97.8%, moisture 0.94%, PH6.88
The dispersant and the wetting agent oleyl alcohol amine APEO that make is promptly composite in 1: 1 ratio.
Embodiment 3:
The processing step of embodiment 3 and embodiment 1 are also identical, and different is:
Catalyst amount is 0.7% in the step (1);
Phenethyl phenol formaldehyde resin and oxirane mol ratio are 1: 50 in the step (2), polymerization temperature is that 170 ℃ of ageing times are 60 minutes, and polymerisation finishes back actual measurement phenethyl phenol formaldehyde resin APEO quality index data: cloud point＞100 ℃, moisture 0.24%, PH5.72;
The mol ratio of phenethyl phenol formaldehyde resin APEO and esterifying agent is 4: 1 in the step (3), and esterifying agent is POCl
3, esterification temperature is 100 ℃, esterification time is 8 hours
Organic base is a diethylenetriamine in the step (4), actual measurement dispersant quality index data: working substance content 97.3%, moisture 1.13%, PH7.02
The dispersant and the wetting agent empgen BB that make is promptly composite in 2.5: 1 ratio.
Wetting agent of the present invention also can adopt fatty acid amide N methyl taurine sodium, polyoxyethylene nonylphenol ether etc. except that above-mentioned three three all materials that embodiment adopted.
Following table has been listed the present invention and the comparison of the special assistant application performance of typical agricultural chemicals suspension agent both at home and abroad:
| Domestic conventional auxiliary agent | The present invention | External same analog assistant | |||
| Form | Triphen ethyl-phenol APEO, dodecyl benzene sulfonate | Phenethyl phenol formaldehyde resin polyoxyethylene ether phosphate salt, wetting agent | Phenethyl phenol polyoxyethylene ether phosphate salt, wetting agent | ||
| Consumption (%) | 5-6 | 3 | 4 | ||
| Application performance | Particle diameter (μ m) | 3.8 | 2.54 | 2.49 | |
| Particle size distribution range (μ m) | 0.68-15.56 | 0.1-6.63 | 0.1-6.78 | ||
| Dispersed | Difference | Very | Very | ||
| Viscosity | 450 | 570 | ?560 | ||
| Bin stability | Refrigeration (0 ℃, seven days) | Be clamminess in the bottom | Homogeneous phase, no bleed | Homogeneous phase, no bleed | |
| Heat is hidden | The heat storage is tied solid after 6 days | Bleed 4% | Bleed 5% | ||
Claims (14)
1, a kind of special assistant of agricultural chemicals suspension agent, it is characterized in that it by dispersant and wetting agent in 1: 10-10: 1 ratio is composite to form.
2, the special assistant of agricultural chemicals suspension agent as claimed in claim 1, it is characterized in that dispersant and wetting agent preferred proportion be 1: 5-5: 1.
3, the special assistant of agricultural chemicals suspension agent as claimed in claim 1 is characterized in that described dispersant is a phenethyl phenol formaldehyde resin polyoxyethylene ether phosphate salt, and it has following structural formula:
4, the preparation method of the special assistant of claim 1 or 2 or 3 described agricultural chemicals suspension agents is characterized in that comprising the steps:
(1) the phenethyl phenol formaldehyde resin is added in the polymeric kettle, add the alkali metal potassium hydroxide catalyst again, the vacuum dehydration of drum nitrogen;
(2) feed oxirane continuously at 140～170 ℃, finish to be cooled to neutralization below 100 ℃ again, generate phenethyl phenol formaldehyde resin APEO after aging decompression removes little molecule and volatile matter;
(3) phenethyl phenol formaldehyde resin APEO and esterifying agent are carried out esterification;
(4) after esterification is finished,, after the pH value reaches 6～8, deviate from moisture content, get dispersant after handling after filtration with the organic base neutralization.
(5) dispersant that above-mentioned steps is made and wetting agent mix in proportion.
5, the preparation method of the special assistant of agricultural chemicals suspension agent as claimed in claim 4 is characterized in that middle phenethyl phenol formaldehyde resin of step (1) and oxirane mol ratio are 1: 10-1: 50;
6, the preparation method of the special assistant of agricultural chemicals suspension agent as claimed in claim 5 is characterized in that the optimum mole ratio of middle phenethyl phenol formaldehyde resin of step (1) and oxirane is 1: 15-1: 30.
7, the preparation method of the special assistant of agricultural chemicals suspension agent as claimed in claim 4 is characterized in that the time of drum nitrogen vacuum dehydration in the step (1) is 30 minutes.
8, the preparation method of the special assistant of agricultural chemicals suspension agent as claimed in claim 4 is characterized in that catalyst amount is the 0.1%-0.7% of phenethyl phenol formaldehyde resin and oxirane gross weight in the step (1).
9, the preparation method of the special assistant of agricultural chemicals suspension agent as claimed in claim 4 is characterized in that the time aging in the step (2) is 20～60 minutes.
10, the preparation method of the special assistant of agricultural chemicals suspension agent as claimed in claim 4 is characterized in that the mol ratio of middle phenethyl phenol formaldehyde resin APEO of step (3) and esterifying agent is 2.3: 1-4: 1.
11, the preparation method of the special assistant of agricultural chemicals suspension agent as claimed in claim 4 is characterized in that esterifying agent can be P in the step (3)
2O
5, PCl
3, POCl
3In any one.
12, the preparation method of the special assistant of agricultural chemicals suspension agent as claimed in claim 4 is characterized in that esterification temperature is 50-100 ℃ in the step (3), and esterification time is 2-8 hour.
13, the preparation method of the special assistant of agricultural chemicals suspension agent as claimed in claim 4 is characterized in that organic base in the step (4) can be any one in ammoniacal liquor, diethanol amine, triethanolamine, diethylenetriamine, the triethylene tetramine.
14, the special assistant of agricultural chemicals suspension agent as claimed in claim 1 is characterized in that wetting agent can be any one in oleyl alcohol amine APEO, fatty acid amide N methyl taurine sodium, fatty alcohol-polyoxyethylene ether, polyoxyethylene nonylphenol ether, the empgen BB.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA031528333A CN1515151A (en) | 2003-08-26 | 2003-08-26 | Special-purpose adjuvant for pesticide suspension agent and its preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA031528333A CN1515151A (en) | 2003-08-26 | 2003-08-26 | Special-purpose adjuvant for pesticide suspension agent and its preparation method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1515151A true CN1515151A (en) | 2004-07-28 |
Family
ID=34240687
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA031528333A Pending CN1515151A (en) | 2003-08-26 | 2003-08-26 | Special-purpose adjuvant for pesticide suspension agent and its preparation method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102079813A (en) * | 2010-11-18 | 2011-06-01 | 浙江皇马科技股份有限公司 | Preparation method of phenol polyoxyethylene phosphonate |
| CN103828797A (en) * | 2014-03-17 | 2014-06-04 | 长兴德源环保助剂有限公司 | Novel special auxiliary of atrazine suspension and preparation method of auxiliary |
| CN109169643A (en) * | 2018-08-23 | 2019-01-11 | 南京拓际生物科技有限公司 | Low bubble heavy duty detergent pesticidal aqueous suspension agent aid of one kind and preparation method thereof |
| CN109315391A (en) * | 2018-11-05 | 2019-02-12 | 石家庄宏科生物化工有限公司 | A kind of liquid pesticidal tackifying assistant and preparation method thereof |
-
2003
- 2003-08-26 CN CNA031528333A patent/CN1515151A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102079813A (en) * | 2010-11-18 | 2011-06-01 | 浙江皇马科技股份有限公司 | Preparation method of phenol polyoxyethylene phosphonate |
| CN102079813B (en) * | 2010-11-18 | 2012-05-30 | 浙江皇马科技股份有限公司 | Preparation method of phenol polyoxyethylene phosphonate |
| CN103828797A (en) * | 2014-03-17 | 2014-06-04 | 长兴德源环保助剂有限公司 | Novel special auxiliary of atrazine suspension and preparation method of auxiliary |
| CN109169643A (en) * | 2018-08-23 | 2019-01-11 | 南京拓际生物科技有限公司 | Low bubble heavy duty detergent pesticidal aqueous suspension agent aid of one kind and preparation method thereof |
| CN109315391A (en) * | 2018-11-05 | 2019-02-12 | 石家庄宏科生物化工有限公司 | A kind of liquid pesticidal tackifying assistant and preparation method thereof |
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