CN107759782A - A kind of preparation method of pesticide emulsion in water auxiliary agent - Google Patents

A kind of preparation method of pesticide emulsion in water auxiliary agent Download PDF

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Publication number
CN107759782A
CN107759782A CN201711056100.6A CN201711056100A CN107759782A CN 107759782 A CN107759782 A CN 107759782A CN 201711056100 A CN201711056100 A CN 201711056100A CN 107759782 A CN107759782 A CN 107759782A
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CN
China
Prior art keywords
rilanit special
auxiliary agent
preparation
water auxiliary
pesticide emulsion
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Pending
Application number
CN201711056100.6A
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Chinese (zh)
Inventor
吴进
王先彬
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NANJING YANGZI HONGLIYUAN CHEMICALS CO Ltd
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NANJING YANGZI HONGLIYUAN CHEMICALS CO Ltd
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Priority to CN201711056100.6A priority Critical patent/CN107759782A/en
Publication of CN107759782A publication Critical patent/CN107759782A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G65/00Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
    • C08G65/02Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
    • C08G65/26Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
    • C08G65/2603Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen
    • C08G65/2615Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen the other compounds containing carboxylic acid, ester or anhydride groups
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/02Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
    • A01N25/04Dispersions, emulsions, suspoemulsions, suspension concentrates or gels

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Pest Control & Pesticides (AREA)
  • Plant Pathology (AREA)
  • Dispersion Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Agronomy & Crop Science (AREA)
  • Medicinal Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Toxicology (AREA)
  • Engineering & Computer Science (AREA)
  • Dentistry (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Colloid Chemistry (AREA)

Abstract

The invention discloses a kind of preparation method of pesticide emulsion in water auxiliary agent, comprise the following steps:Rilanit special is added in polymerization reaction kettle, add base metal catalysts, the epoxide reaction with short-chain branch is added into ether, etherificate polymerisation obtains rilanit special polyethers A, rilanit special polyethers A will be obtained, after neutralized processing, after adding base metal catalysts nitrogen displacement, then oxirane is added, etherificate polymerisation obtains rilanit special polyethers B, after neutralized processing, obtains pesticide emulsion in water auxiliary agent, wherein, the amount ratio of the material of the epoxides with short-chain branch and rilanit special is 90~100:1;The amount ratio of the material of oxirane and rilanit special is 30~40:1.The pesticide emulsion in water auxiliary agent that the present invention obtains, it is applied in pesticide emulsion in water, the physical stability of aqueous emulsion can be significantly improved, and there is extensive adaptability, can applied in Multiple Pesticides.

Description

A kind of preparation method of pesticide emulsion in water auxiliary agent
Technical field
The present invention relates to a kind of preparation method of pesticide emulsion in water auxiliary agent.
Background technology
With the fast development of modern preparation, pesticidal preparations just develop towards the direction of environment-friendly type, and aqueous emulsion is exactly One of which, domestic insecticides adjuvant is not also very flourishing at present, and also no small gap, use are existing compared with developed countries The aqueous emulsion that auxiliary agent is made into mainly is passed through on ageing stability presence more or less in terms of physical stability is certain the problem of Often there is serious lamination, greatly limit the application of water-emulsion preparation.Therefore it is necessary on the basis of existing technology Research hair outputs that a kind of scope of application is wider, can be effectively by the uniform and stable scattered water with aqueous phase of a variety of oiliness pesticide original medicines Emulsion adjunct.
The content of the invention
The invention provides a kind of preparation method of pesticide emulsion in water auxiliary agent.
In order to solve the above problems, the technical solution adopted in the present invention be it is such, a kind of pesticide emulsion in water auxiliary agent Preparation method, it is characterised in that comprise the following steps:
1) rilanit special is added in polymerization reaction kettle, addition base metal catalysts, after nitrogen displacement, addition has For the epoxide reaction of short-chain branch into ether, it is standby that etherificate polymerisation obtains rilanit special polyethers A;Wherein, it is described to have The epoxides of short-chain branch is selected from the mixing of 1,2- epoxy butanes, one kind in 2,3- epoxy butanes or two or more any proportion Thing, it is 90~100 to have the amount ratio of the epoxides of short-chain branch and the material of rilanit special:1;
2) step 1) is obtained into rilanit special polyethers A, after neutralized processing, added into base metal catalysts nitrogen displacement Afterwards, oxirane is then added, etherificate polymerisation obtains rilanit special polyethers B, after neutralized processing, obtains pesticide water The amount ratio of the material of emulsion adjunct, oxirane and rilanit special is 30~40:1.
Preferably, described base metal catalysts are sodium methoxide, potassium methoxide, Sodium Allylate, allyl potassium alcoholate, methallyl alcohol The mixture of one or both of sodium, methallyl potassium alcoholate, iso-amylene sodium alkoxide, iso-amylene potassium alcoholate any of the above ratio.
Preferably, the quality of the base metal catalysts described in step 1) be hydrogenated castor oil quality 1-3%, step 2) In used base metal catalysts quality be rilanit special polyethers A mass 2-5%.
Preferably, step 1) reaction pressure is 0.1~1.0MPa;Reaction temperature is 110~160 DEG C.
Preferably, step 2) reaction pressure is 0.1~1.0MPa;Reaction temperature is 110~160 DEG C.
Preferably, the one kind or two or more any ratio of neutralization reagent in formic acid, acetic acid, propionic acid, lactic acid, citric acid The mixing of example.
Beneficial effect:The present invention is by rilanit special with having epoxides (1,2- epoxy butane, 2, the 3- rings of short-chain branch The mixture of one kind or two or more any proportion in oxygen butane) and unbranched epoxides (oxirane) addition polymerization Copolyether is formed, a certain amount of short-chain branch ethyl is introduced in polyether backbone so that the hydrophilic and hydrophobic grouping in molecular structure Reach a relatively good scope, so as to which stability is high, have it is good emulsify, disperse, soaking, the performance such as solubilising.
Embodiment
In order to deepen the understanding of the present invention, below in conjunction with embodiment, the invention will be further described, the embodiment It is only used for explaining the present invention, is not intended to limit the scope of the present invention..
Embodiment 1
Rilanit special 1mol, catalyst sodium methoxide 15g are put into 1L reactors, nitrogen displacement 2 times, is warming up to 110 ~120 DEG C, 1,2- epoxy butane 90mol are passed through, it is 0.1-0.5MPa, slaking reaction aging 1.5hr to control reaction pressure, is taken off Gas, after pressure is reduced into 0, obtain rilanit special polyethers A;Acetic acid will be added in obtained rilanit special polyethers A so that pH value Between 5-7, catalyst sodium methoxide 40g is added, nitrogen displacement 2 times, 105~135 DEG C is warming up to, is continuously added to oxirane, It is 0.10~0.40MPa to control reaction pressure, adds oxirane 30mol, curing and degassing, after pressure is reduced into 0, obtains hydrogen Change castor oil polyethers B;Rilanit special polyethers B material temperatures are down to 90~100 DEG C, add acetic acid into polyethers B so that pH value exists Between 5-7, discharge to obtain pesticide emulsion in water auxiliary agent 1.
Embodiment 2
Rilanit special 1mol, catalyst sodium methoxide 30g are put into 1L reactors, nitrogen displacement 2 times, is warming up to 110 ~120 DEG C, 1,2- epoxy butane 100mol are passed through, it is 0.1-0.5MPa, slaking reaction aging 1.5hr to control reaction pressure, is taken off Gas, after pressure is reduced into 0, obtain rilanit special polyethers A;Formic acid will be added in obtained rilanit special polyethers A so that pH value Between 5-7, catalyst sodium methoxide 40g is added, nitrogen displacement 2 times, 105~135 DEG C is warming up to, is continuously added to oxirane, It is 0.10~0.40MPa to control reaction pressure, adds oxirane 40mol, curing and degassing, after pressure is reduced into 0, obtains hydrogen Change castor oil polyethers B;Rilanit special polyethers B material temperatures are down to 90~100 DEG C, add formic acid into polyethers B so that pH value exists Between 5-7, discharge to obtain pesticide emulsion in water auxiliary agent 2.
Embodiment 3
Rilanit special 1mol, catalyst sodium methoxide 25g are put into 1L reactors, nitrogen displacement 2 times, is warming up to 110 ~120 DEG C, 1,2- epoxy butane 95mol are passed through, it is 0.1-0.5MPa, slaking reaction aging 1.5hr to control reaction pressure, is taken off Gas, after pressure is reduced into 0, obtain rilanit special polyethers A;Formic acid will be added in obtained rilanit special polyethers A so that pH value Between 5-7, catalyst sodium methoxide 40g is added, nitrogen displacement 2 times, 105~135 DEG C is warming up to, is continuously added to oxirane, It is 0.10~0.40MPa to control reaction pressure, adds oxirane 35mol, curing and degassing, after pressure is reduced into 0, obtains hydrogen Change castor oil polyethers B;Rilanit special polyethers B material temperatures are down to 90~100 DEG C, add formic acid into polyethers B so that pH value exists Between 5-7, discharge to obtain pesticide emulsion in water auxiliary agent 3.
Using the pesticide emulsion in water auxiliary agent 1-3 that embodiment 1-3 is prepared as auxiliary agent be applied to 2.5% time, In 40% chlopyrifos, 6.9% galloping horse water emulsion formula, its capability and performance is then tested respectively.Specific experiment result such as table 1 is to table Shown in 3:
Pesticide emulsion in water auxiliary agent 1-3, which is applied to correspond to respectively in 2.5% time aqueous emulsion, obtains 2.5% time aqueous emulsion 1- 3, its determination of quality index result is as shown in table 1:
Table 1
Pesticide emulsion in water auxiliary agent 1-3, which is applied to correspond to respectively in 40% chlorpyrifos aqueous emulsion, obtains 40% chlorpyrifos aqueous emulsion 1-3, its determination of quality index result are as shown in table 2:
Table 2
Pesticide emulsion in water auxiliary agent 1-3 is corresponded to and is obtained 6.9% galloping horse aqueous emulsion 1-3, its matter respectively applied to 6.9% galloping Malaysia and China Figureofmerit measurement result is as shown in table 3:
Table 3
The pesticide emulsion in water auxiliary agent that the present invention obtains, it is applied in pesticide emulsion in water, aqueous emulsion can be significantly improved Physical stability, and there is extensive adaptability, it can be applied in Multiple Pesticides.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention God any modification, equivalent substitution and improvements made etc., should be included in the scope of the protection with principle.

Claims (6)

1. a kind of preparation method of pesticide emulsion in water auxiliary agent, it is characterised in that comprise the following steps:
1) rilanit special is added in polymerization reaction kettle, addition base metal catalysts, after nitrogen displacement, added with short For the epoxide reaction of side chain into ether, it is standby that etherificate polymerisation obtains rilanit special polyethers A;Wherein, it is described have it is short The epoxides of side chain is selected from the mixture of 1,2- epoxy butanes, one kind in 2,3- epoxy butanes or two or more any proportion, The amount ratio of the material of epoxides and rilanit special with short-chain branch is 90~100:1;
2) by step 1)Rilanit special polyethers A is obtained, after neutralized processing, after adding base metal catalysts nitrogen displacement, Then oxirane is added, etherificate polymerisation obtains rilanit special polyethers B, after neutralized processing, obtains agricultural chemicals water and milk The amount ratio of the material of agent aid, oxirane and rilanit special is 30~40:1.
A kind of 2. preparation method of pesticide emulsion in water auxiliary agent according to claim 1, it is characterised in that described alkali metal Catalyst be sodium methoxide, potassium methoxide, Sodium Allylate, allyl potassium alcoholate, methallyl sodium alkoxide, methallyl potassium alcoholate, iso-amylene sodium alkoxide, The mixture of one or both of iso-amylene potassium alcoholate any of the above ratio.
A kind of 3. preparation method of pesticide emulsion in water auxiliary agent according to claim 1, it is characterised in that step 1)Described in Base metal catalysts quality be hydrogenated castor oil quality 1-3%, step 2)In the quality of used base metal catalysts be The 2-5% of rilanit special polyethers A mass.
A kind of 4. preparation method of pesticide emulsion in water auxiliary agent according to claim 1, it is characterised in that step 1)Reaction pressure Power is 0.1~1.0MPa;Reaction temperature is 110~160 DEG C.
A kind of 5. preparation method of pesticide emulsion in water auxiliary agent according to claim 1, it is characterised in that step 2)Reaction pressure Power is 0.1~1.0MPa;Reaction temperature is 110~160 DEG C.
6. the preparation method of a kind of pesticide emulsion in water auxiliary agent according to claim 1, it is characterised in that neutralization reagent is selected from The mixture of one kind or two or more any proportion in formic acid, acetic acid, propionic acid, lactic acid, citric acid.
CN201711056100.6A 2017-10-31 2017-10-31 A kind of preparation method of pesticide emulsion in water auxiliary agent Pending CN107759782A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101790553A (en) * 2007-07-26 2010-07-28 株式会社资生堂 Alkylene oxide derivative and skin external preparation containing the same
CN102030897A (en) * 2010-11-17 2011-04-27 南京扬子鸿利源化学品有限责任公司 Hydrogenated castor oil block polyether as well as preparation method and application thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101790553A (en) * 2007-07-26 2010-07-28 株式会社资生堂 Alkylene oxide derivative and skin external preparation containing the same
CN102030897A (en) * 2010-11-17 2011-04-27 南京扬子鸿利源化学品有限责任公司 Hydrogenated castor oil block polyether as well as preparation method and application thereof

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Application publication date: 20180306

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