CN1229020C - Suspension emulsion of nicotine microcapsule, and its prepn. method - Google Patents

Suspension emulsion of nicotine microcapsule, and its prepn. method Download PDF

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Publication number
CN1229020C
CN1229020C CN 03139131 CN03139131A CN1229020C CN 1229020 C CN1229020 C CN 1229020C CN 03139131 CN03139131 CN 03139131 CN 03139131 A CN03139131 A CN 03139131A CN 1229020 C CN1229020 C CN 1229020C
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China
Prior art keywords
glue
nicotine
suspension emulsion
oil
vegetable oil
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Expired - Fee Related
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CN 03139131
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Chinese (zh)
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CN1513311A (en
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张天良
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Zhong Weide
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Individual
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  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

The present invention discloses a nicotine microcapsule suspension emulsion and a preparation method thereof. The nicotine microcapsule suspension emulsion contains nicotine as effective components, surface active agent, vegetable oil, auxiliary agent, solvent, water and composition of two and more than two hydrolysates of animal glue, vegetable glue and sea product glue. The preparation method comprises the steps that the auxiliary agents, the vegetable oil and the surface active agents are added into the oily nicotine liquor; the mixed liquor is diluted by the solvents, heated to 50 to 80 DEG C and continuously stirred and a certain amount of water is added; then, two or more than two kinds of glues from the animal glues, the vegetable glues and the sea product glues are respectively hydrolyzed, heated to 50 to 80 DEG C and filtered; the filtrates are mixed, uniformly stirred and added into the preparation liquor; the mixed liquor is mixed and stirred at the rotary speed of 200 to 600 rotations per minute and is simultaneously and naturally cooled for 2 hours. The nicotine microcapsule suspension emulsion has the advantages of slow light degradation and long effect and can be widely used on green economic crops without nuisance.

Description

Nicotinic Microcapsule Suspending Agent And Its Preparation Method
(1) technical field:
The present invention relates to the formulation technical field of agricultural chemicals, is a kind of Nicotinic Microcapsule Suspending Agent And Its Preparation Method specifically.
(2) background technology:
As everyone knows, nicotine directly proposes from tobacco, has the characteristics of efficient, low toxicity, noresidue, and suitable pollution-free green food is used, but nicotine itself is seen photolysis, is evaporated completely in half an hour in the sun.
(3) summary of the invention:
Purpose of the present invention is intended to overcome the deficiency of above-mentioned prior art, and a kind of nicotine microcapsules suspension emulsion is provided.
Another object of the present invention provides the preparation method of nicotine microcapsules suspension emulsion.
The present invention has mainly solved nicotine and has seen the problem that photolysis is fast.
Nicotine microcapsules suspension emulsion of the present invention since its capsule skin forms by natural high molecular polymer fully, can be in air cracking fully, to plant itself and environmental nonpollution, can large tracts of land use on economic crops such as vegetables, melon and fruit.
In order to achieve the above object, the present invention is achieved in that nicotine microcapsules suspension emulsion, it is characterized in that it is is effective ingredient with nicotine, and contain surfactant, vegetable oil, auxiliary agent, solvent, water, also contain one or both the composition of hydrolysate in marine product glue and animal glue and the natural plant gum simultaneously; Surfactant is triphen ethyl phenol APEO, dibenzyl xenol APEO, vegetable oil is cottonseed oil, rapeseed oil, castor oil acid, auxiliary agent is calcium dodecyl benzene sulfonate, phenethyl phenol polyethenoxy polyethenoxy ether, castor oil ethylene oxide adduct, solvent is a dimethylbenzene, animal glue is gelatin, natural plant gum is an amylan, and marine product glue is fish glue, sodium alginate.
The preparation method of nicotine microcapsules suspension emulsion of the present invention comprises following processing step:
A, the making of capsule nuclear in oily liquid nicotine, adds auxiliary agent, vegetable oil, surfactant, adds solvent again and dilutes, and is heated to 60-80 ℃, constantly stirs simultaneously, adds a certain amount of water again; Auxiliary agent is calcium dodecyl benzene sulfonate, phenethyl phenol polyethenoxy polyethenoxy ether, castor oil ethylene oxide adduct, vegetable oil is cottonseed oil, rapeseed oil, castor oil acid, surfactant is triphen ethyl phenol APEO, dibenzyl xenol APEO, and solvent is a dimethylbenzene;
B, the making of capsule skin is carried out the hydrolysis of all kinds of glue respectively earlier with one or both glue in marine product glue and animal glue and the natural plant gum, is heated to 60-80 ℃ respectively, filters the back and mixes, and stirring gets final product; Marine product glue is fish glue, sodium alginate, and animal glue is gelatin, and natural plant gum is an amylan;
C, microcapsule formulation is poured the capsule skin raw material of step b in the reactor of capsule nuclear of step a, mixes under 200-600 rev/min rotating speed and stirs, and after lowering the temperature 2 hours naturally simultaneously, packs.
The preparation method of nicotine microcapsules suspension emulsion of the present invention, when its described capsule skin adopted animal glue and natural plant gum, its capsule hole skin was little and inhomogeneous, did not reach the release time of regulation on request, therefore also need add blowing agent.
Nicotine microcapsules suspension emulsion of the present invention is with organic macromolecule the effective body of agricultural chemicals to be wrapped from the outside, the lattice voids of handy big minute ascus wall discharges slowly, avoid its photodissociation, thereby reduce the consumption of former medicine greatly, prolong the lasting period, can control its lasting period and rate of release artificially; Because of nicotine sees that photolysis is fast, thereby be its effective drug duration of control, the particle diameter of its microcapsules is bigger, generally is controlled at the 10-50 micron.
A kind of Nicotinic Microcapsule Suspending Agent And Its Preparation Method of the present invention compared with the prior art, have substantive distinguishing features and marked improvement: 1, nicotine microcapsules suspension emulsion sees that photolysis is slow, thereby improve its drug effect, prolong effective drug duration simultaneously, learn through test, its former medicine reduces 30-50%, and control efficiency improves 10-20%, and the lasting period prolongs 3-10 doubly; 2, its capsule skin of nicotine microcapsules suspension emulsion is made up of natural polymer fully, and fully biodegradable, thereby noresidue can be extensive use of on the nuisanceless green economic crops.
(4) embodiment:
In order to understand better and to implement, describe a kind of Nicotinic Microcapsule Suspending Agent And Its Preparation Method of the present invention in detail below in conjunction with embodiment.
Embodiment 1, with 2.8g oily liquid nicotine, adding 0.5g calcium dodecyl benzene sulfonate, 0.5g phenethyl phenol polyethenoxy polyethenoxy ether, 3g castor oil, 4g triphen ethyl phenol APEO, 6g dimethylbenzene, be heated to 70 ℃, constantly stir simultaneously, add 16g water again, standby; 8g gelatin, 8g sodium alginate are added 92g water respectively to be hydrolyzed, be heated to 70 ℃ respectively, each 25g of glue that gets after the said hydrolyzed filters, filtering the back mixes, and stir, the glue that stirs is added in the reserve liquid of making previously, under 400 rev/mins rotating speed, mix and stir, naturally cooling promptly got nicotine microcapsules suspension emulsion after 2 hours simultaneously.
Nicotine microcapsules suspension emulsion of the foregoing description and 5% nicotine cream are at blue or green worm drug effect lasting period contrast table of control Lay such as table 1.
Table 1
The test sample Extension rate Borer population is counted head/strain before the medicine Preceding 1 day of medicine Behind the medicine 3 days Behind the medicine 5 days
Head/strain Proofread and correct preventive effect % Head/strain Proofread and correct preventive effect % Head/strain Proofread and correct preventive effect %
Nicotine microcapsules suspension emulsion 1000 8 1 87.5 1.2 80 2.5 68.75
5% nicotine cream 1000 6 2 66.7 7 0 7 0
Control group Not dispenser 5 5 / 6 / 8 /
Embodiment 2, with 5g oily liquid nicotine, adding 0.6g calcium dodecyl benzene sulfonate, 0.6g castor oil ethylene oxide adduct, 4g cottonseed oil, 4.5g dibenzyl xenol APEO, 7g dimethylbenzene, be heated to 60 ℃, constantly stir simultaneously, add 18g water again, standby; 8g amylan, 8g sodium alginate are added 92g water respectively to be hydrolyzed, be heated to 60 ℃ respectively, each 28g of glue that gets after the said hydrolyzed filters, filtering the back mixes, and stir, the glue that stirs is added in the reserve liquid of making previously, under 500 rev/mins rotating speed, mix and stir, naturally cooling promptly got nicotine microcapsules suspension emulsion after 2 hours simultaneously.
Embodiment 3, with 2g oily liquid nicotine, adding 0.2g calcium dodecyl benzene sulfonate, 0.2g phenethyl phenol polyethenoxy polyethenoxy ether, 2g rapeseed oil, 3g triphen ethyl phenol APEO, 5g dimethylbenzene, be heated to 50 ℃, constantly stir simultaneously, add 14g water again, standby; 7.5g gelatin, 7.5g amylan are added 92g water respectively to be hydrolyzed, be heated to 50 ℃ respectively, each 15g of glue that gets after the said hydrolyzed filters, filter the back and mix, and stir, add the 1g blowing agent, the glue that stirs is added in the reserve liquid of making previously, mix under 200 rev/mins rotating speed and stir, cooling promptly got nicotine microcapsules suspension emulsion after 2 hours naturally simultaneously.
Embodiment 4, with 10g oily liquid nicotine, adding 1g calcium dodecyl benzene sulfonate, 1g phenethyl phenol polyethenoxy polyethenoxy ether, 5g castor oil, 5g triphen ethyl phenol APEO, 10g dimethylbenzene, be heated to 80 ℃, constantly stir simultaneously, add 20g water again, standby; 8g gelatin, 8g sodium alginate are added 92g water respectively to be hydrolyzed, be heated to 60 ℃ respectively, each 30g of glue that gets after the said hydrolyzed filters, filter the back and mix, and stir, the glue that stirs is added in the reserve liquid of making previously, under 600 rev/mins rotating speed, mix and stir, naturally cooling was packed behind adding anti-icing fluid, the dyestuff after 2 hours simultaneously, promptly got nicotine microcapsules suspension emulsion.

Claims (2)

1, nicotine microcapsules suspension emulsion is characterized in that it is is effective ingredient with nicotine, and contains surfactant, vegetable oil, auxiliary agent, solvent, water, also contains one or both the composition of hydrolysate in marine product glue and animal glue and the natural plant gum simultaneously; Surfactant is triphen ethyl phenol APEO, dibenzyl xenol APEO, vegetable oil is cottonseed oil, rapeseed oil, castor oil acid, auxiliary agent is calcium dodecyl benzene sulfonate, phenethyl phenol polyethenoxy polyethenoxy ether, castor oil ethylene oxide adduct, solvent is a dimethylbenzene, animal glue is gelatin, natural plant gum is an amylan, and marine product glue is fish glue, sodium alginate.
2, the preparation method of the described nicotine microcapsules of claim 1 suspension emulsion comprises following processing step:
A, the making of capsule nuclear in oily liquid nicotine, adds auxiliary agent, vegetable oil, surfactant, adds solvent again and dilutes, and is heated to 60-80 ℃, constantly stirs simultaneously, adds a certain amount of water again; Auxiliary agent is calcium dodecyl benzene sulfonate, phenethyl phenol polyethenoxy polyethenoxy ether, castor oil ethylene oxide adduct, vegetable oil is cottonseed oil, rapeseed oil, castor oil acid, surfactant is triphen ethyl phenol APEO, dibenzyl xenol APEO, and solvent is a dimethylbenzene;
B, the making of capsule skin is carried out the hydrolysis of all kinds of glue respectively earlier with one or both glue in marine product glue and animal glue and the natural plant gum, is heated to 60-80 ℃ respectively, filters the back and mixes, and stirring gets final product; Marine product glue is fish glue, sodium alginate, and animal glue is gelatin, and natural plant gum is an amylan;
C, microcapsule formulation is poured the capsule skin raw material of step b in the reactor of capsule nuclear of step a, mixes under 300-600 rev/min rotating speed and stirs, and after lowering the temperature 2 hours naturally simultaneously, packs.
CN 03139131 2003-08-16 2003-08-16 Suspension emulsion of nicotine microcapsule, and its prepn. method Expired - Fee Related CN1229020C (en)

Priority Applications (1)

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CN 03139131 CN1229020C (en) 2003-08-16 2003-08-16 Suspension emulsion of nicotine microcapsule, and its prepn. method

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Application Number Priority Date Filing Date Title
CN 03139131 CN1229020C (en) 2003-08-16 2003-08-16 Suspension emulsion of nicotine microcapsule, and its prepn. method

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BRPI0619826B1 (en) * 2005-12-14 2016-02-10 Sumitomo Chemical Co pesticide microcapsule and method for producing said microcapsule.
CN103651588B (en) * 2013-09-10 2015-11-11 北京联合大学生物化学工程学院 A kind of preparation method of the encapsulate pesticides for killing aphid
CN110250174B (en) * 2018-03-12 2022-08-19 侨昌现代农业有限公司 Oil-containing dry suspending agent formulation and processing technology thereof
CN109757475A (en) * 2019-03-01 2019-05-17 杨卫东 A kind of microcapsule formulation and preparation method thereof coating solid pesticide raw medicine

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Owner name: ZHONG WEIDE

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Address after: 100071, Fengtai District Science City, Beijing, No. 10 Spark Road B-107 Beijing Tianshan dark horse Biotechnology Co., Ltd.

Patentee after: Zhong Weide

Address before: 265601 north ditch, Shandong, Penglai, Beijing, Shandong, Beijing biological pharmaceutical, Limited by Share Ltd

Patentee before: Zhang Tianliang

EE01 Entry into force of recordation of patent licensing contract

Assignee: Beijing Tianshan dark horse Biotechnology Co., Ltd.

Assignor: Zhong Weide

Contract fulfillment period: 2007.6.6 to 2012.6.5 contract change

Contract record no.: 2009990000430

Denomination of invention: Suspension emulsion of nicotine microcapsule, and its prepn. method

Granted publication date: 20051130

License type: Exclusive license

Record date: 2009.5.6

LIC Patent licence contract for exploitation submitted for record

Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2007.6.6 TO 2012.6.5; CHANGE OF CONTRACT

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Effective date: 20090506

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CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20051130

Termination date: 20120816