CN102630668B - Environment-friendly slow-release micro-capsule suspension agent and preparation method thereof - Google Patents

Environment-friendly slow-release micro-capsule suspension agent and preparation method thereof Download PDF

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Publication number
CN102630668B
CN102630668B CN 201210110465 CN201210110465A CN102630668B CN 102630668 B CN102630668 B CN 102630668B CN 201210110465 CN201210110465 CN 201210110465 CN 201210110465 A CN201210110465 A CN 201210110465A CN 102630668 B CN102630668 B CN 102630668B
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capsule
agent
finished product
core
reactor
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CN102630668A (en
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苏庆申
王才库
张祥栋
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SHANDONG DONGXIN BIOLOGICAL PESTICIDES CO Ltd
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SHANDONG DONGXIN BIOLOGICAL PESTICIDES CO Ltd
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Abstract

The invention relates to an environment-friendly slow-release micro-capsule suspension agent and a preparation method thereof. The environment-friendly slow-release micro-capsule suspension agent is prepared from 25-28% of capsule core material (1), 8-12% of floating catalyst (2), 1-2% of dispersing agent (3), 45-50% of thinning agent (4), 5-8% of capsule skin material (5), 0.2-0.4% of thickeningagent (6), 0.05-0.15% of sourness conditioning agent (7), 0.2-0.5% of anti-coagulating agent (8), 0.05-0.15% of regulation additive (9), 0.05-0.15% of defoaming agent (10) and 4-7% of anti-freezing agent (11) according to a proportion. Automatic production is carried out on a special production line under the operation of an intelligent control system. According to the invention, the environment-friendly slow-release micro-capsule suspension agent does not contain organic solvent components, such as dimethylbenzene and the like, so that chemical injury caused by pesticide volatilization can be avoided, and the environmental pollution can be reduced; because the efficacy duration is increased, the dosage is reduced by half, the efficacy is doubled, and weed damage can be controlled for a long time; the concentration of pesticides contacted by crops is reduced, so that the safety is increased; and in addition, the environment-friendly slow-release micro-capsule suspension agent has the advantages of being automatic for production in the preparation process, time-saving, labour-saving, good in quality, low in cost, high in production efficiency and good in economical benefit.

Description

A kind of slowly-releasing environment-friendly type microcapsule suspending agent and preparation method thereof
Technical field
The present invention relates to the weed killer herbicide agricultural chemicals, relate in particular to water baseization preemergence herbicide and production technology thereof.
Background technology
Ministry of Industry and Information of country has announced since the production licence of emulsifiable concentrates for agricultural chemicals product off the docket, the formulation of Pesticidal products presents variation, what wherein can replace the emulsifiable concentrate pesticide product has microemulsion, aqueous emulsion and a microcapsule suspending agent, but microemulsion and aqueous emulsion are because the needs of processing technology, use toxic solvents such as toluene, dimethylbenzene to need during production, have only microcapsule suspending agent can realize water baseization production.Existing microcapsule formulations encapsulation technique has following several: (one) interfacial polymerization; be with active substance and suitable macromolecule cyst wall monomer be dissolved in the immiscible organic solvent of water in; again oil phase is joined in the aqueous phase solution that contains suitable emulsifier and protection glue at shearing condition; form oil-in-water or Water-In-Oil; control particle size as required; if it is improper that solvent is selected; during preparation high concentration microcapsule formulations crystalline polamer takes place easily, the irregular crystal that crystallization goes out can destroy cyst wall and can't bring into play drug effect.(2) home position polymerization reaction method, be that high polymer monomer and prepolymer are placed oil phase, before adding, earlier solid active agent is dissolved in the immiscible organic solvent of water in, use in-situ polymerization technology and produce asymmetric cyst wall, internal layer provides support, the outer diffusion rate that determines need heat certain hour when forming cyst wall.(3) coacervation is the severe Polymer Solution reaction of the opposite electricity with another of cation high molecular solution that contains pre-dispersed active substance, and the agglomeration step lapping must wrap up core materials fully, forms soft shell capsule, the difficult control of this technology.(4) microcapsule suspension atomized drying micro-capsule granula processed, be to contain active substance and high molecular slip carries out atomized drying, make macromolecule form cyst wall around solid capsule-core particle, encapsulated granula is distributed in the water more still can recover former state, but particle diameter is bigger.(5) molecular inclusion is to make clad material with beta-schardinger dextrin-, forms microcapsules at molecular level, and hygroscopicity is low, easily preserves, and is biodegradable, but the cost height, difficulty is big, the cycle is long.Above process is produced microcapsule suspending agent, has the following disadvantages: because active component is become the capsule material parcel, fail effectively to control the packing rate, can reduce drug effect, fall flat; Because it is microcapsules technology relates to numerous areas, relatively harsher to the physics and chemistry selection of former medicine; Production process can pollute environment; Extended storage stability is not good; The particle diameter skewness; Rate of release shakiness etc.
Summary of the invention
Purpose of the present invention is developed new microcapsule suspending agent exactly and is determined its preparation technology, makes microcapsules have core/shell structure; particle diameter is evenly distributed, and reaches rate of release and takes into account to hold and imitate and quick-acting, and effective ingredient is good; improve pharmacodynamic stability; Automation of Manufacturing Process control is totally-enclosed, realizes process " three wastes " zero-emission, the protection environment; improve production efficiency and product quality; save production cost, easy to use, safe, improve the economic and social benefits.
Task of the present invention is finished like this: study a kind of slowly-releasing environment-friendly type microcapsule suspending agent and preparation method thereof, the set of dispense of slowly-releasing environment-friendly type microcapsule suspending agent is than by quality being: core materials 25~28%, emulsifier 8~12%, dispersant 1~2%, thinner 45~50%, capsule leather material 5~8%, thickener 0.2~0.4%, regulating acid agent 0.05~0.15%, anti-agglomerating agent 0.2~0.5%, regulate auxiliary agent 0.05~0.15%, defoamer 0.05~0.15%, antifreeze 4~7%, make the microcapsule suspending agent finished product according to the proportioning combination, core materials in the set of dispense ratio is the Acetochlor of purity 96%, emulsifier is the Sodium Polyacrylate of purity 40%, dispersant is the Phosphate of Polyoxyethylene Isooctyl Ether of purity 95%, thinner is deionized water, the capsule leather material is the etherificate melamine glue of purity 50%, and thickener is the industrial goods xanthans, and regulating acid agent is the hydrochloric acid of purity 35%, anti-agglomerating agent is the industrial goods aluminium-magnesium silicate, regulating auxiliary agent is industrial goods sodium hydroxide, and defoamer is industrial silicone emulsion, and antifreeze is industrial goods ethylene glycol.The quality index of microcapsule suspending agent finished product is: core materials gross mass mark 23.5~26.5%, free core materials mass fraction≤1.5%, pH value scope 5.0~8.0, suspensibility 〉=90%, mass fraction rate of release≤90% of the outer effective ingredient of 20min capsule, topple over back residue≤5%, washing back residue≤1%, lasting foaming characteristic 〉=30ml, 75 μ m wet screenings test percent of pass 〉=98%, spontaneous dispersiveness 〉=95%, freeze/thaw cyclical stability and heat storage stability meet the relevant national standard regulation.Various elements are raw material in the set of dispense ratio, on the sealed special production line that some main line equipment and corollary equipment connect to form with pipeline respectively, carry out automated production by the intelligent control system manipulation, main line equipment adopts the preparation still, the capsule-core emulsion reactor, capsule skin reactor, the capsule-core homogenizer, capsule skin homogenizer, the encystation reactor, solidify condenser, the finished product condenser, device of full automatic packaging, corollary equipment is measuring tank, charge pump, the homogeneous material basin, the homogeneous material pump, discharge pump, the finished product basin, through the preparation emulsifying step, the pre-polymerization homogenizing step, solidify condensing steps, froth breaking finished product step, each processing step of automatic packaging step, under the corresponding process conditions of each step, make the microcapsule suspending agent finished product.The main line equipment of preparation emulsifying step is the preparation still, the capsule-core emulsion reactor, capsule skin reactor, corollary equipment is measuring tank, charge pump, the processing step process is: after the core materials process is melt and dissolved, with emulsifier, dispersant, thinner adds in the measuring tank according to the proportioning ratio, transport to the preparation still by charge pump by feeding pipe, again in pipeline input capsule-core emulsion reactor, with thickener, regulating acid agent adds the capsule-core emulsion reactor by proportioning, be heated to 60 ℃, stir with the 1500r/min rotating speed, be warming up to 85~90 ℃ in the 20min, make the capsule-core emulsion behind the 30min, simultaneously the capsule leather material is added in the capsule skin reactor by proportioning, be heated to 60 ℃ with 1500r/min rotating speed stirring 20min, heat again and stir 40min to 85~90 ℃ with the 800r/min rotating speed, make capsule skin material, capsule-core emulsion and capsule skin material are transported to the capsule-core homogenizer respectively by pipeline, capsule skin homogenizer enters the pre-polymerization homogenizing step.The main line equipment of pre-polymerization homogenizing step is capsule-core homogenizer and capsule skin homogenizer, corollary equipment is the homogeneous material basin, the processing step process is: the capsule-core emulsion is process 1500r/min high speed shear 30min in the capsule-core homogenizer, form emulsifying liquid, capsule skin material forms the pre-polymerization material through the 1500r/min high speed shear in capsule skin homogenizer, emulsifying liquid and pre-polymerization material form homogeneous pre-polymerization liquid by mixing in the pipeline input homogeneous material basin, prepare to enter the curing condensing steps.The main line equipment that solidifies condensing steps is the encystation reactor, solidify condenser, corollary equipment is the homogeneous material pump, the processing step process is: the homogeneous material pump is with the homogeneous pre-polymerization liquid in the homogeneous material basin, in pipeline input encystation reactor, stir, mix, be warming up to 85~90 ℃, stir 60min, simultaneously with regulating acid agent, anti-agglomerating agent adds the encystation reactor by proportioning, and it is 4.0 that preceding 20min regulates the pH value, and it is 2.5 that back 40min regulates the pH value, after the cooling, solidify in the condenser by the pipeline input, the condensation polymerization is shaped, and makes the synthetic encystation of capsule-core capsule skin, transport to the finished product condenser by pipeline then, enter froth breaking finished product step.The main line equipment of froth breaking finished product step is the finished product condenser, corollary equipment is discharge pump and finished product basin, the processing step process is: encystation adds the finished product condenser, in the finished product condenser, add adjusting auxiliary agent, defoamer, antifreeze by proportioning simultaneously, shear condensation process 30~50min through ovennodulation, stablize, froth breaking, make the microcapsule suspending agent particle, stored by pipeline input finished product basin by discharge pump, prepare to enter automatic packaging step.Automatically the main line equipment of packaging step is device of full automatic packaging, the processing step process is: the microcapsule suspending agent particle in the finished product basin is transported to device of full automatic packaging by pipeline, automatically the packing container of packing into is the microcapsule suspending agent finished product, the sampling inspection warehousing after passing.Intelligent control system comprises that calculator and system control special-purpose software, hardware, connect the sensor that is installed on the production equipment by lead, to detect data and feed back to calculator, according to preset program numerical value speed of agitator, temperature in the kettle, the capsule skin degree of polymerization and thickness, pH value, foam, the flow feeding of process be adjusted control automatically.Acetochlor chemistry in the raw material is by name: 2 '-ethyl-6 '-methyl-N-(ethoxymethyl)-2-chloro acetanilide, former medicine is faint yellow to brown liquid, molten o'clock greater than 0 ℃, boiling point is greater than 200 ℃, not volatile and photodissociation, relative density ratio with water in the time of 30 ℃ is 1.11:1, and the solvability in water is 23mg/L.According to the physicochemical property of Acetochlor and determining of controlling object, the technological principle that the present invention produces the Acetochlor microcapsule suspending agent is: after earlier former medicine, solvent, floating agent and water being mixed, become O/w emulsion with the homogenizer shearing, then water-soluble film forming agent is joined in the emulsion form agricultural chemicals, heat up, coat film forming behind the adding catalyzer.Reaction finishes, and adds the auxiliary agent modulation again, namely makes final products---microcapsule suspending agent.Melamine resin is as in-situ polymerization capsule leather material like this, by to having stoped the crosslinked of glue after the melamine resin adhesive etherificate, can make the micro-capsule cyst wall evenly, rounding.In preparation process, acidifying acid adjustment speed is comparatively obvious to size and the distribution influence of microcapsule diameter, and the present invention determines to regulate pH value to 2.5 in 60min.Through experimental test, the encapsulation ratio of Acetochlor microcapsule suspending agent of the present invention is stabilized in more than 98%, and average grain diameter is at 7.0~8.9 μ m, and the coefficient of dispersion is 0.25~0.29.
Intelligent control system comprises one in main frame, and system's control is special-purpose soft, each cover of hardware, software probe instrument one cover.The detection of systematic parameter is input to host A/D modular converter by the detected data of sensor through each transmitter, carries out analog-to-digital conversion, through the laggard line output of Computer Processing, printing, tabulation, record, drawing, warning etc.Production process of the present invention does not have waste gas, waste residue produces, and industrial water mainly is the flushing of boiler and equipment, and basic unharmful substance can be done the general back discharging of handling, and environment is not had influence.
Implement according to technique scheme, prove that proportioning component of the present invention rationally, effectively, the processing of Acetochlor microcapsule suspending agent, storage and convenient transportation, safety, micro-capsule has core/shell structure, particle diameter is even, do not contain organic solvent compositions such as dimethylbenzene in the preparation, reduced the pollution to environment, can not produce poisoning because of the medicament volatilization; Avoid photodissociation, make dosage reduce half, drug effect doubles, and has saved agriculture production cost; Lasting period increases, and a drug can be controlled weeds harm the long period; The concentration of crops contact medicament reduces, and safety improves; Need not shallow mixed soil during dispenser, reduced labour intensity, improved efficient; Preparation process adopts intelligent control automated production; the equipment configuration is reasonable, compact; sealed production line operation is safe, time saving and energy saving; unharmful substance pollutes, and is conducive to environmental protection, the production efficiency height; good product quality; cost is low, materials are economized, and has good economic benefit and social benefit, has reached predetermined purpose preferably.
Description of drawings
Accompanying drawing is technological process of production schematic diagram of the present invention.
Among the figure, 1-core materials, 2-emulsifier, 3-dispersant, 4-thinner, 5-capsule leather material, 6-thickener, 7-regulating acid agent, 8-anti-agglomerating agent, 9-adjusting auxiliary agent, 10-defoamer, 11-antifreeze; A-measuring tank, B-charge pump, C-preparation still, D-capsule-core emulsion reactor, D1-capsule skin reactor, E-capsule-core homogenizer, E1-capsule skin homogenizer, F-homogeneous material basin, G-homogeneous material pump, H-encystation reactor, J-curing condenser, K-finished product condenser, L-discharge pump, M-finished product storage tank, N-device of full automatic packaging, R-encystation, Z-microcapsule suspending agent finished product, W-calculator, X-lead, Q-sensor; I-preparation emulsifying step, II-pre-polymerization homogenizing step, III-curing condensing steps, IV-froth breaking finished product step, V-automatic packaging step.
Embodiment
With reference to the accompanying drawings the specific embodiment of the present invention is illustrated.
The measuring tank A of microcapsule suspending agent automatic assembly line, charge pump B, preparation still C, capsule-core emulsion reactor D, capsule skin reactor D1, capsule-core homogenizer E, capsule skin homogenizer E1, homogeneous material basin F, homogeneous material pump G, encystation reactor H, curing condenser J, finished product condenser K, discharge pump L, finished product basin M, device of full automatic packaging N, be formed by connecting by pipeline, handle control by intelligent control system, constitute the sealing automatic production line.Technological process is as follows:
The main line equipment preparation still C of preparation emulsifying step I selects 1500L capacity enamel jar 1 cover, capsule-core emulsion reactor D selects 4 of 1000L capacity enamel oil bath reactors, capsule skin reactor D1 selects 2 of the oily molten heating reactors of the enamel of 1000L capacity, corollary equipment measuring tank A selects 4 in the enamel jar of 100L~300L, charge pump B selects 4 of FLB25 type corrosion protection pumps, the processing step process is: press proportioning with core materials 1, emulsifier 2, dispersant 3, thinner 4 adds measuring tank A separately respectively, squeezed among the preparation still C by pipeline by corresponding charge pump B, again by pipeline input capsule-core emulsion reactor D, again with thickener 6, regulating acid agent 7 adds by proportioning; Capsule leather material 5 melt and dissolved backs add capsule skin reactor D1 simultaneously, mix separately, speed of agitator is 1500r/min, heat to 60 ℃ and carry out combination reaction, 20min is warming up to 85~90 ℃, makes capsule-core emulsion and capsule skin material behind the 30min respectively, and capsule skin reactor D1 speed of agitator transfers to 800r/min, capsule-core emulsion and capsule skin material transfer to capsule-core homogenizer E, capsule skin homogenizer E1 respectively behind the 40min, enter pre-polymerization homogenizing step II.
Main line equipment capsule-core homogenizer E, the capsule skin homogenizer E1 of pre-polymerization homogenizing step II respectively select 2 of YB2-1 type homogenizers, and corollary equipment homogeneous material basin F selects 4 of A3 steel storage tanks.The processing step process is: the capsule-core emulsion for preparing is by pipeline input capsule-core homogenizer E, capsule skin material is by pipeline input capsule skin homogenizer E1, handle through the 1500r/min high speed shear, form emulsifying liquid and pre-polymerization material respectively, separately by pipeline input homogeneous material basin F, formation pH value is 2.5 mixing emulsifying liquid, prepares to enter curing condensing steps III.
The main line equipment encystation reactor H that solidifies the condensing steps III selects 4 of the molten reactors of 1000L capacity enamel oil, solidifies condenser J and selects 10m 2Enamel condenser 3 covers, corollary equipment homogeneous material pump G selects 1 of FLB25 type corrosion protection pump, the processing step process is: homogeneous material pump G extracts the emulsifying liquid among the homogeneous material basin F out, by pipeline input encystation reactor H, in encystation reactor H, inject regulating acid agent 7 and anti-agglomerating agent 8 by proportioning then, stir, be warming up to 85~90 ℃ and react 60min, it is 4.0 that preceding 20min regulates the pH value, and it is 2.5 that back 40min regulates the pH value, and the encystation material is exported in the cooling back, add curing condenser J by pipeline, form the synthetic microcapsule structure encystation R of capsule-core capsule skin, by pipeline input finished product condenser K, enter froth breaking finished product step IV then.
The main line equipment finished product condenser K of froth breaking finished product step IV selects 10m 23 of condensers, corollary equipment discharge pump L selects 1 of FLB25 type corrosion protection pump, and finished product basin M selects 4 of A3 steel storage tanks.The processing step process is: encystation R enters finished product condenser K, add by proportioning then and regulate auxiliary agent 9, defoamer 10, antifreeze 11, shear through ovennodulation, condensation process 30~50min, stablize, froth breaking, make the microcapsule suspending agent particle, import finished product basin M by discharge pump L by pipeline, for packaging step V is ready automatically.
Automatically the main line equipment of packaging step V is device of full automatic packaging N, the processing step process is: the microcapsule suspending agent encystation R among the finished product basin M transfers to device of full automatic packaging N by pipeline, is microcapsule suspending agent finished product Z in the packing container of quantitatively packing into (as packaging bag, Packaging Bottle, packing jar).Sampling simultaneously detects, and warehouse-in is loaded in qualified back.
Whole process flow is controlled by preset program automatically by intelligent control system.Intelligent control system comprises one of industrial control computer W, disposes UPS uninterrupted power source, color monitor, laser printer, electronic keyboard etc. simultaneously, and input/output interface adopts newton's module, gets in touch with communication modes with main frame.The detection of systematic parameter is to connect the sensor Q that is installed on each production equipment by lead X, detected data are input to the A/D modular converter through each transmitter, carry out analog-to-digital conversion, after handling through calculator W, export, print, record, report to the police.System acquisition has with the technological parameter of control process: multiple indexs such as speed of agitator, temperature in the kettle, the capsule skin degree of polymerization and thickness, pH value, foam control, flow feeding.
Set of dispense of the present invention than in core materials 1 to select purity for use be 96% Acetochlor, it is 40% Sodium Polyacrylate that emulsifier 2 is selected purity for use, it is 96% Phosphate of Polyoxyethylene Isooctyl Ether that dispersant 3 is selected purity for use, thinner 4 is selected deionized water for use, it is 50% etherificate melamine glue that capsule leather material 5 is selected purity for use, thickener 6 is selected the xanthans industrial goods for use, it is 35% hydrochloric acid that regulating acid agent 7 is selected purity for use, anti-agglomerating agent 8 is selected the industrial goods aluminium-magnesium silicate for use, regulate auxiliary agent 9 and select industrial goods sodium hydroxide for use, defoamer 10 is selected the industrial goods silicone emulsion for use, and antifreeze 11 is selected industrial goods ethylene glycol for use.The proportioning of each raw material composition is exemplified below in the recipe ingredient:
The control quality index of the microcapsule suspending agent finished product Z that makes is: core materials 1 Acetochlor gross mass mark is 23.5~26.5%, free Acetochlor mass fraction≤1.5%, pH value scope 5.0~8.0, suspensibility 〉=90%, mass fraction rate of release 〉=90% of the outer active ingredient of 20min capsule, topple over back residue≤5%, washing back residue≤1%, lasting foaming characteristic 〉=30ml, 75 μ m wet screenings test percent of pass 〉=98%, spontaneous dispersiveness 〉=95%, heat storage stability is qualified, and the freeze/thaw cyclical stability is qualified.
Product of the present invention can prolong the lasting period, be conducive to reduce dispenser quantity and frequency, reduce environmental pollution, strengthen pharmacodynamic stability, active substance is wrapped in the cyst wall, has improved safety, having realized that high-toxic pesticide is low poisons, reduced acute poisoning, the material of covering former medicine effectively swashs the property smell, reduces pesticide activity component to the stimulation of human body skin.When dispenser, alleviate simultaneously the poisoning to crops, the composite convenience that provides of the pesticidal active substance of multiple different performance is provided.Preparation method of the present invention is reasonable, the equipment configuration effectively, processing step connects closely, and intelligent control system is stable, and antijamming capability is strong, production process does not produce waste gas, waste residue, not newly-increased waste water has reduced environmental pollution, the production efficiency height, cost is low, and economic benefit and social benefit are good.

Claims (3)

1. slowly-releasing environment-friendly type microcapsule suspending agent, it is characterized in that set of dispense than by quality being: core materials (1) 25~28%, emulsifier (2) 8~12%, dispersant (3) 1~2%, thinner (4) 45~50%, capsule leather material (5) 5~8%, thickener (6) 0.2~0.4%, regulating acid agent (7) 0.05~0.15%, anti-agglomerating agent (8) 0.2~0.5%, regulate auxiliary agent (9) 0.05~0.15%, defoamer (10) 0.05~0.15%, antifreeze (11) 4~7%, make microcapsule suspending agent finished product (Z) according to the proportioning combination, core materials (1) in the set of dispense ratio is the Acetochlor of purity 96%, emulsifier (2) is the Sodium Polyacrylate of purity 40%, dispersant (3) is the Phosphate of Polyoxyethylene Isooctyl Ether of purity 95%, thinner (4) is deionized water, capsule leather material (5) is the etherificate melamine glue of purity 50%, thickener (6) is the industrial goods xanthans, regulating acid agent (7) is the hydrochloric acid of purity 35%, anti-agglomerating agent (8) is the industrial goods aluminium-magnesium silicate, regulating auxiliary agent (9) is industrial goods sodium hydroxide, defoamer (10) is industrial silicone emulsion, antifreeze (11) is industrial goods ethylene glycol, the quality index of microcapsule suspending agent finished product (Z) is: core materials (1) pH value scope 5.0~8.0, suspensibility 〉=90%, mass fraction rate of release≤90% of the outer effective ingredient of 20min capsule, topple over back residue≤5%, washing back residue≤1%, lasting foaming characteristic 〉=30ml, 75 μ m wet screenings test percent of pass 〉=98%, spontaneous dispersiveness 〉=95%, freeze/thaw cyclical stability and heat storage stability meet the relevant national standard regulation.
2. the preparation method of a slowly-releasing environment-friendly type microcapsule suspending agent, it is characterized in that it being that various elements are raw material in comparing with the described set of dispense of claim 1, on the sealed special production line that some main line equipment and corollary equipment connect to form with pipeline respectively, carry out automated production by the intelligent control system manipulation, main line equipment adopts preparation still (C), capsule-core emulsion reactor (D), capsule skin reactor (D1), capsule-core homogenizer (E), capsule skin homogenizer (E1), encystation reactor (H), solidify condenser (J), finished product condenser (K), device of full automatic packaging (N), corollary equipment is measuring tank (A), charge pump (B), homogeneous material basin (F), homogeneous material pump (G), discharge pump (L), finished product basin (M), through preparation emulsifying stage (I), the pre-polymerization homogeneous stage (II), solidify condensation phase (III), the froth breaking finished product stage (IV), each technical process of automatic packing stage (V), under corresponding process conditions of each stage, make microcapsule suspending agent finished product (Z), the main line equipment of preparation emulsifying stage (I) is preparation still (C), capsule-core emulsion reactor (D), capsule skin reactor (D1), corollary equipment is measuring tank (A), charge pump (B), technical process is: after core materials (1) process is melt and dissolved, with emulsifier (2), dispersant (3), thinner (4) adds in the measuring tank (A) according to the proportioning ratio, transport to preparation still (C) by charge pump (B) by feeding pipe, again in pipeline input capsule-core emulsion reactor (D), with thickener (6), regulating acid agent (7) adds capsule-core emulsion reactor (D) by proportioning, add thermal agitation, make the capsule-core emulsion, simultaneously capsule leather material (5) is added in the capsule skin reactor (D1) by proportioning, add thermal agitation, make capsule skin material, capsule-core emulsion and capsule skin material are transported to capsule-core homogenizer (E) respectively by pipeline, capsule skin homogenizer (E1), enter the pre-polymerization homogeneous stage (II), its main line equipment is capsule-core homogenizer (E) and capsule skin homogenizer (E1), corollary equipment is homogeneous material basin (F), technical process is: the capsule-core emulsion is the process high speed shear in capsule-core homogenizer (E), form emulsifying liquid, capsule skin material forms the pre-polymerization material through high speed shear in capsule skin homogenizer (E1), emulsifying liquid and pre-polymerization material are by mixing in the pipeline input homogeneous material basin (F), form homogeneous pre-polymerization liquid, enter and solidify condensation phase (III), its main line equipment is encystation reactor (H), solidify condenser (J), corollary equipment is homogeneous material pump (G), technical process is: homogeneous material pump (G) is imported the homogeneous pre-polymerization liquid in the homogeneous material basin (F) in the encystation reactor (H) by pipeline, stir, mix, heat up and stir, simultaneously with regulating acid agent (7), anti-agglomerating agent (8) adds encystation reactor (H) by proportioning, regulating the pH value is 4.0, it is 2.5 that the pH value is regulated in the back, after the cooling, solidify in the condenser (J) by the pipeline input, the condensation polymerization is shaped, make the synthetic encystation (R) of capsule-core capsule skin, transport to finished product condenser (K) by pipeline then, enter the froth breaking finished product stage (IV), its main line equipment is finished product condenser (K), corollary equipment is discharge pump (L) and finished product basin (M), technical process is: encystation (R) adds finished product condenser (K), in finished product condenser (K), add adjusting auxiliary agent (9) by proportioning simultaneously, defoamer (10), antifreeze (11), shear through ovennodulation, condensation process, stablize, froth breaking, make the microcapsule suspending agent particle, stored by pipeline input finished product basin (M) by discharge pump (L), enter automatic packing stage (V), its main line equipment is device of full automatic packaging (N), technical process is: the microcapsule suspending agent particle in the finished product basin (M) is transported to device of full automatic packaging (N) by pipeline, automatically the packing container of packing into, be microcapsule suspending agent finished product (Z), the sampling inspection warehousing after passing.
3. according to the preparation method of the described slowly-releasing environment-friendly type of claim 2 microcapsule suspending agent, it is characterized in that described intelligent control system comprises that calculator (W) and system control special-purpose software, hardware, connect the sensor (Q) that is installed on the production equipment by lead (X), to detect data and feed back to calculator (W), according to preset program numerical value speed of agitator, temperature in the kettle, the capsule skin degree of polymerization and thickness, pH value, foam, the flow feeding of process be adjusted control automatically.
CN 201210110465 2012-04-16 2012-04-16 Environment-friendly slow-release micro-capsule suspension agent and preparation method thereof Expired - Fee Related CN102630668B (en)

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