CN104026133B - A kind of N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation and preparation method thereof and special purpose device - Google Patents
A kind of N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation and preparation method thereof and special purpose device Download PDFInfo
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- CN104026133B CN104026133B CN201410216772.9A CN201410216772A CN104026133B CN 104026133 B CN104026133 B CN 104026133B CN 201410216772 A CN201410216772 A CN 201410216772A CN 104026133 B CN104026133 B CN 104026133B
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Abstract
The invention belongs to pesticide processing field, be specifically related to a kind of N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation and preparation method thereof and special purpose device.Spray in the granulation zone in fluidization granulation tower continuously through two streaming nebulizers after specifically feed liquid being heated, heated air by the pre-distributing chamber of gas and is entered into equipped with in the granulation tower of crystal seed through distribution grid as fluidizing agent by pressure fan, crystal seed under the effect of fluidized hot medium in stabilization fluid state, feed liquid is atomized rear continuous spray at peripheral " coating " granulating of crystal seed, finished granule sequentially enters dry classification region under the wind speed of different gradients and carries out screening operation, thus the purpose realizing carrying out separating in granulation tower by controlling the fluidizing velocity of zones of different obtains N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation.The present invention prepare N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation during fluidization granulation by pelletize, be dried and screening etc. completes in same flow process, be equipped with tails dedusting, purify, wash or the operation such as absorption, it is to avoid dust contact and drift, it is achieved that cleaning produces.
Description
Technical field
The invention belongs to pesticide processing field, be specifically related to a kind of N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation and system thereof
Preparation Method and special purpose device.
Background technology
N,N'-dimethyl-.gamma..gamma.'-dipyridylium chemical name is 1,1 '-dimethyl-4,4-bipyridine cation salt, is a kind of quick-acting tactile
Kill type steriland herbicide, most annual grassy weeds can be controlled and suppress perennial weeds, being generation
Boundary uses one of the widest herbicide, has become as indispensable agriculture articles for use.
At present the main product dosage form of N,N'-dimethyl-.gamma..gamma.'-dipyridylium is 20% and 25% water preparation, due to safety with wrongly take accident
Occur frequently, and do not have any medicine to effect a radical cure after wrongly taking, therefore, the Ministry of Agriculture, the Ministry of Industry and Information Technology,
State General Administration for Quality Supervision, on April 24th, 2012, combines No. 1745 bulletins of issue, for BAICAO low water
Agent limited with listing clear and definite timetable: from 1 day July in 2014, the registration of N,N'-dimethyl-.gamma..gamma.'-dipyridylium water preparation and life
Producing licence will be revoked, on July 1st, 2016, water preparation stopped at home sale and use.
For solving its safety issue, in terms of the formulation technology of N,N'-dimethyl-.gamma..gamma.'-dipyridylium, domestic have been carried out
Multiple trial, prior art is concentrated mainly on prepares water solublity colloid and water-soluble granular formulation two
Plant dosage form, though wherein N,N'-dimethyl-.gamma..gamma.'-dipyridylium water solublity colloid overcomes the shortcoming that water preparation is easily administered orally, but using
Also existing in journey and be difficult to shortcomings such as measuring, dispersibility is poor, the management simultaneously discarding packing material is also required to
Consider emphatically；The main method now preparing water-soluble granular formulation employing is conventional extruded pelletize and spray dried
Dry granulation, uses conventional extruded prilling process, need to face mother liquor concentrations problem and preparation processing,
Dust problem more serious in dry run, uses spray drying process, except the easiest
Outside generation dust, there is also the problems such as granule strength is on the low side, the defect of both prilling process is specialty
In field known to personnel, the restriction of such as factors listed above, general effect is unsatisfactory.
Summary of the invention
It is an object of the invention to the drawbacks described above for prior art, it is provided that a kind of N,N'-dimethyl-.gamma..gamma.'-dipyridylium water solublity
Granule and preparation method thereof and special purpose device.
For achieving the above object, the present invention uses the technical scheme to be:
The preparation method of a kind of N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation, through two streaming nebulizers after heating feed liquid
Spraying in the granulation zone in fluidization granulation tower continuously, heated fresh purification air is made by pressure fan
By the pre-distributing chamber of gas and enter into equipped with in the granulation tower of crystal seed through distribution grid for fluidizing agent,
Crystal seed is in stabilization fluid state under the effect of fluidized hot medium, and feed liquid is atomized to 50～100 μm even
Continuing and be sprayed on peripheral " coating " granulating of crystal seed, finished granule sequentially enters dry under the wind speed of different gradients
Stepped zone carries out screening operation, thus realizes at granulation tower by controlling the fluidizing velocity of zones of different
The purpose inside carrying out separating obtains the particle diameter N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation less than 5mm.Use the present invention's
The N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation preferable particle size that fluidized bed granulation is made is at 0.2-2.5mm.
Described feed liquid is atomized to 50～100 μm and is sprayed on peripheral " coating " granulating of crystal seed continuously, and maintains
Temperature in granulation tower is at 70～180 DEG C, and in granulation process, steam granulation tail gas is taken away, tail gas
Processing through built-in sack cleaner and dust removal installation udst separation, after process, fine dust returns to fluidisation and makes
Grain tower is as crystal seed, and tail gas sequentially passes through at washing absorption tower and activated carbon adsorber purification further again
Reason, then empties under the effect of air-introduced machine.
Return after the tail gas drying dehydration of described scrubbed absorption tower and activated carbon adsorber purified treatment
Reuse in the pre-distributing chamber of fluidization granulation tower, the particle dust of trapping returns to fluidization granulation tower and makees
For crystal seed.
Further, feed liquid is heated to 40～70 DEG C, through two after further preferred 50～60 DEG C
Streaming nebulizer sprays in the granulation zone in fluidization granulation tower continuously, pressure fan will be heated to 160～
280 DEG C, the fresh purification air of further preferred 200～240 DEG C is pre-by gas as fluidizing agent
Distributing chamber also enters into equipped with in the granulation tower of crystal seed through distribution grid, and crystal seed is at the work of fluidized hot medium
With lower in stabilization fluid state, feed liquid is atomized to 50～100 μm continuous sprays in the peripheral " painting of crystal seed
Cloth " granulating, control inlet amount maintain the temperature in granulation tower at 70～180 DEG C, further preferred 80～
120 DEG C, steam granulation tail gas is taken away, tail gas generated by granulation through built-in cloth bag or successively through two stage cyclone and
Pulse is returned and is blown bag-type dust purified treatment, and fine dust returns to fluidization granulation tower as crystal seed, and tail gas is again
Sequentially pass through washing absorption and the further purified treatment of activated carbon adsorption operation, under the effect of air-introduced machine
Emptying, changes adsorption tower and absorbing liquid after the N,N'-dimethyl-.gamma..gamma.'-dipyridylium dust content in periodic analysis tail gas, granule becomes
Product utilize while granulating and drying fluidizing velocity gradient continuously enter stepped zone carry out separate behaviour
Make, the Double-layer packaging bag envelope that qualified particle uses internal layer to be the outer alclad case of water soluble package as finished product
Dress, defective particle returns to pelletize again in material liquid tank or granulation tower.
Described feed liquid refer to paraquat dichloride, surfactant, stink agent, emetic, pigment and
The mixture of filler；
Or mixing after add water, the addition of water be paraquat dichloride, surfactant, stink agent,
The 1-80% (preferably 5-30%) of weight after emetic, pigment and filler mixing；Described it is configured to
Feed liquid is heated to 40～70 DEG C, stand-by.
Other solvent can be dissolved during paraquat dichloride content height by described feed liquid；N,N'-dimethyl-.gamma..gamma.'-dipyridylium two
Need when chloride content is low add water and then help dissolve other auxiliary agent.
The particle diameter that described pelletize obtains is less than in the N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation of 5mm percentage by weight
Than counting, paraquat dichloride 40-95% (paraquat cation 30-69%), surfactant 1-30%,
Stink agent 0-2%, emetic triazolo pyrimidine ketone is equivalent to the 0-2% of paraquat dichloride, pigment 0-2%
With filler 1-58%；Described paraquat dichloride content is preferably 50～80%.
Described surfactant is to be selected from but is not limited to one or more in following material: alkyl
Arylsulphonate, di alkylaryl sulfonate, dialkyl group virtue sulfosuccinate, lignosulfonates,
Naphthalene sulfonic acid-formaldehyde condensation product, alkylated naphthalene sulfonic formaldehyde condensation compound, polyethylene oxide alkyl benzene sulphonate
Salt, polyoxyalkylene succinate, polyoxyethylene alkyl ether, polyethylene oxide alkylbenzene
Base ether, sorbitan fatty acid ester, polyoxyethylene sorbitan fatty acid ester, polyoxyl 40 stearate
Fat acid esters, ethylene oxide condensate.Wherein, ethylene oxide condensate is selected from but is not limited to fatty acid
With ethylene oxide condensate, condensation compound of alkyl phenol and epoxy ethane, fatty alcohol and ethylene oxide condensate,
Oleum Ricini/castor oil hydrogenated and ethylene oxide condensate.
Described filler is selected from but is not limited to potassium chloride, sodium chloride, ammonium chloride, ammonium sulfate, sulfur
Acid sodium, potassium sulfate, sodium benzoate, sucrose, glucose, carbamide, water soluble starch in one or
Several.
Prepare the fluidization granulation tower of N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation, including fluidising chamber 3, pre-distributing chamber 1,
Distribution grid 2, dividing plate 4, built-in cloth bag 5 and the pond 6 that gathers materials, the top of described fluidising chamber 3 is provided with tail gas
Outlet and inside top are provided with multiple cloth bag 5, are provided with between described fluidising chamber 3 and pre-distributing chamber 1
Distribution grid 2 and be positioned at fluidising chamber 3 bottom, described distribution grid 2 be provided with multiple by fluidising chamber 3 with pre-
The through hole of distributing chamber 1 connection, the lower sides of described fluidising chamber 3 is provided with dog-house, hand hole and goes out
Material mouth, in described fluidising chamber 3, bottom is separated into multiple region by dividing plate 4；Described pre-distributing chamber 1
Sidewall be provided with multiple air inlet, the bottom of described pre-distributing chamber 1 is provided with the pond 6 that gathers materials.Wherein, feed intake
Mouth and discharging opening are respectively arranged on both sides, and the outer wall in each region is all provided with hand hole.
The dividing plate that in described fluidising chamber, bottom is provided with it is separated into from left to right granulation zone, dry section and
Graded region；Wherein, to be provided with feed liquid nebulizer, dry section and graded region top reserved on the top of granulation zone
Nebulizer interface, can decide whether to enable according to actual particle size distribution situation；Each dividing plate and distribution grid
Spacing be 30～100mm, left and right distance according to grain graininess require and treating capacity adjust.
Described distribution grid is porous type, cone hat type or cover-plate type；Wherein, the hole on distribution grid is circular,
Equilateral triangle or square, percent opening scope is 3～10%.
Described feed liquid nebulizer is single or the granulation zone being positioned in fluidising chamber of branched arrangement and dry section
In, feed liquid nebulizer is 300～1400mm with the spacing of distribution grid；Its feed liquid nebulizer can use
Upper-spraying type or following spray.When described feed liquid nebulizer is branched arrangement, can be to be single or multiple lift mode
Arrangement；Atomizer structure form can be mechanical type or pressure type.Preferably pressure atomizer, its gas
Liquid mass ratio is 0.1～1.0, and the atomizing angle of nozzle is 30 °～120 °.
A kind of device preparing N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation, including fluidization granulation tower, material liquid tank, removes
Dirt equipment, washing absorption tower, charcoal trap, wherein, cleaner, washing absorption tower, work
Property charcoal absorption tower and air-introduced machine pass sequentially through pipeline and communicate；Cleaner air inlet and fluidization granulation tower tail
Gas outlet is connected by pipeline, and cleaner gas outlet is connected by pipeline with scrubbing tower air inlet；Stream
Change feed liquid nebulizer charging aperture in granulation tower to be connected with material liquid tank by pipeline, feed liquid nebulizer air scoop
It is connected with air compressor machine by pipeline.
Advantage for present invention:
1. the selection of surfactant in the N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation that prepared by the present invention, it is ensured that each
Cooperating of component function.Dispersion, moistening, infiltration, solubilising and the froth breaking etc. that each component is played
Effect ensure that the biological activity of N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation, and is verified by biological activity test,
Its preventive effect is substantially excellent in the comparison commercially available 20% N,N'-dimethyl-.gamma..gamma.'-dipyridylium water preparation of medicament, illustrates that the present invention prepares water-soluble
Property granule biological activity excellent, significant herbicidal effect can be played after using；And then obtain granule tool
Have epigranular, to enter water disintegrate fast, safe and convenient to use, excellent water miscible on the basis of, particle
There is good intensity, which ensure that product will not cause particle efflorescence because of external force in transportation.
Avoid contact and the drift of dust in pelletization simultaneously, reduce the danger of accidental or intentional absorption.
Additionally the property indices of gained water-soluble granular formulation meets national sector standard HG
Requirement to water-soluble granular formulation in 2467.16-2003.
2. the present invention prepare N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation during fluidization granulation by pelletize, be dried and
Screening waits and completes in same flow process, is equipped with tails dedusting, purifies, washs or the operation such as absorption, keeps away
Exempt from dust contact and drift, solve N,N'-dimethyl-.gamma..gamma.'-dipyridylium self severe toxicity, the most dirty to operator and environment
The problem of dye, it is achieved that cleaning produces.The mechanism that simultaneously prepared by the present invention is that injection mother solution is to outside crystal seed
Enclose " onion " structure formed in " coating " mode, prepared granule good sphericity, have excellent molten
Solution property and granule strength.
Accompanying drawing explanation
The N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation preparation technology flow chart that Fig. 1 provides for the embodiment of the present invention, wherein
11-air compressor machine 12-material liquid tank 13-granulation tower 14-finished product bin 15-dust removal installation 16-heater
17-pressure fan 18-washing absorption tower 19-activated carbon adsorber 20-air-introduced machine.
The N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation pelletize classifying equipoment structure chart that Fig. 2 provides for the embodiment of the present invention,
Wherein a1～a4 offgas outlet b1～b4 feed liquid nebulizer c1～c4 hand hole, manhole d1～
D4 fresh air inlet e1～e4 gathers materials a mouthful f dog-house g discharging opening 1-pre-distributing chamber 2-distribution grid 3-
Fluidising chamber 4-dividing plate 5-built-in cloth bag 6-gathers materials pond.
Detailed description of the invention
The N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular of the present invention is described in detail underneath with embodiment and comparative example
Agent.Following example are only for illustrating the present invention, should not be construed as scope
Restriction." % " that occur in following example all represents weight percentage, simultaneously each portion in device
Part all can obtain under the conditions of commercial.Mother solution in following embodiment is purchased from Shandong green despot chemical industry share
Company limited, in mother solution, the content of paraquat dichloride is 42%.
The water-soluble granular formulation containing N,N'-dimethyl-.gamma..gamma.'-dipyridylium of the present invention, in addition to using each component mixed preparing, also
The paraquat dichloride mother solution containing frowziness agent, emetic and pigment can be directly used to prepare,
The paraquat dichloride mother solution mentioned in invention is as referred both to containing frowziness agent, emetic without specified otherwise
The paraquat dichloride mother solution of agent and pigment.
Embodiment 1
N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation is grouped into by the one-tenth of following weight percents: paraquat dichloride
70%, surfactant Oleum Ricini/castor oil hydrogenated and ethylene oxide condensate EL-20,15%,
Stink agent pyridine 0.1%, emetic triazolo pyrimidine ketone is equivalent to the 0.18% of paraquat dichloride, color
Element 0.05%, surplus is filler ammonium chloride；
Prepare the device of N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation, set including fluidization granulation tower, material liquid tank, dedusting
Standby, washing absorption tower, charcoal trap, wherein, cleaner, washing absorption tower, activated carbon
Absorption tower and air-introduced machine pass sequentially through pipeline and communicate；Cleaner air inlet goes out with fluidization granulation tower tail gas
Mouth is connected by pipeline, and cleaner gas outlet is connected by pipeline with scrubbing tower air inlet；Fluidisation is made
In grain tower, feed liquid nebulizer charging aperture is connected with material liquid tank by pipeline, and feed liquid nebulizer air scoop passes through
Pipeline is connected with air compressor machine.
Fluidization granulation tower, including fluidising chamber, pre-distributing chamber, distribution grid, dividing plate and cloth bag, described stream
The top of change room is provided with offgas outlet and inside top is provided with multiple cloth bag, the end of described fluidising chamber
Portion is provided with distribution grid, and described distribution grid is provided with multiple through hole fluidising chamber connected with pre-distributing chamber,
The lower sides of described fluidising chamber is provided with dog-house, hands mouth and discharging opening, bottom in described fluidising chamber
It is separated into granulation zone, dry section and graded region by dividing plate；The sidewall of described pre-distributing chamber is provided with multiple
Air inlet, the bottom of described pre-distributing chamber is provided with multiple mouth that gathers materials.Fluidising chamber passes through 2 dividing plates from a left side
Granulation zone, dry section and graded region it is followed successively by the right side；Wherein, the sidewall of pre-distributing chamber be provided with multiple enter
Air port, each air inlet controls obstructed flow velocity, not only ensures that the granule of zones of different is in fluidisation shape
State and have motive force from left to right to realize the separation of different grain size granule.
Granulation zone and arid region that described dividing plate is divided into are built-in with feed liquid nebulizer；Wherein, respectively
Individual dividing plate is 30mm with the spacing of distribution grid.The version of described distribution grid is cover-plate type；Perforate cloth
The mode of putting is equilateral triangle；Percent opening is 6%.Feed liquid nebulizer is 900mm with the spacing of distribution grid；
Its feed liquid nebulizer can use upper-spraying type.Described feed liquid nebulizer is pressure type, and its gas-liquid mass ratio is
0.4, the atomizing angle of nozzle is 60 °.
Preparation:
According to the above ratio raw material is mixed, stirs, use electrical heating that feed liquid is heated to 60 DEG C,
In two streaming pressure atomizer sent into by feed pump, then in nebulizer sprays into fluidization granulation tower continuously
In pelletize and arid region, pressure fan will warm up the fresh purification air of 220 DEG C as fluidizing agent
Being entered into equipped with in the granulation tower of crystal seed by the effect of the pre-distributing chamber of gas and distribution grid, crystal seed is in warm
In stabilization fluid state under the effect of fluidizing agent, fluidizing velocity is at 0.4m/s, and N,N'-dimethyl-.gamma..gamma.'-dipyridylium feed liquid is by mist
Change to 50～60 μm continuous sprays at peripheral " coating " granulating of crystal seed, and maintain the temperature in granulation tower
At 80～90 DEG C, tail gas combines udst separation through two stage cyclone separator and cloth envelop collector successively and processes,
Fine dust returns to fluidization granulation tower as crystal seed, sequentially pass through again after tail gas removing dust washing absorption and
The further purified treatment of activated carbon adsorption operation, empties, the fine grained of trapping under the effect of air-introduced machine
Dust returns to fluidization granulation tower as crystal seed, utilize different densities granule have different fluidizing velocity,
Carrying velocity and the characteristic of deposition velocity, along with feed liquid spraying pelletize be carried out continuously granule be on the increase and
Growing up, granulated pellet completes to be dried and divide at the beginning of fine powder, granule under the effect of fluidizing agent at dry section
Automatically flow into graded region, make qualified products be in fluidized state by the intake of the pre-distributing chamber of control and enter
Enter material discharge region, and coarse granule falls into more greatly, due to density its fluidizing velocity big, the pond that gathers materials, thus realize
The purpose separated is carried out in granulation tower.N,N'-dimethyl-.gamma..gamma.'-dipyridylium granule, at pelletize dwell time in the tower 40min, obtains grain
The footpath N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular less than 5mm (0.2-2.5mm), rear finished product is packed after testing,
Fine grained particle returns to granulation tower.
Embodiment 2
N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation is grouped into by the one-tenth of following weight percents: 50% N,N'-dimethyl-.gamma..gamma.'-dipyridylium dichloro
Compound, 0.1% stink agent, emetic triazolo pyrimidine ketone be equivalent to paraquat dichloride weight 0.18%,
0.05% pigment, 10% surfactant fatty alcohol and ethylene oxide condensate AEO-3, remaining is with filling out
Fill agent ammonium sulfate to supply.
Preparation: raw material is mixed and added into preparing paraquat dichloride in granule, table by aforementioned proportion
The water of weight 12% after face activating agent, stink agent, emetic, pigment and filler mixing, stirring is all
Even, use electrical heating that feed liquid is heated to 60 DEG C, in two streaming pressure atomizer sent into by feed pump,
Air is heated to 220 DEG C and is entered by the effect of the pre-distributing chamber of gas and distribution grid as fluidizing agent
To equipped with in the fluidization granulation tower of crystal seed, crystal seed under the effect of fluidized hot medium in stabilization fluid state,
It is peripheral at crystal seed to 50～60 μm continuous sprays that N,N'-dimethyl-.gamma..gamma.'-dipyridylium feed liquid is atomized device atomization, controls inlet amount dimension
Holding the temperature in granulation tower at 90～100 DEG C, steam granulation tail gas is taken away, and tail gas is successively through two
Level cyclone separator and cloth envelop collector combination udst separation process, and fine dust returns to fluidization granulation tower
As crystal seed, sequentially pass through washing absorption after tail gas removing dust again and activated carbon adsorption operation is the cleanest
Change processes, and empties under the effect of air-introduced machine, and the particle dust of trapping returns to fluidization granulation tower and makees
For crystal seed, finished granule sequentially enters dry classification region under the wind speed of different gradients and carries out screening behaviour
Making, N,N'-dimethyl-.gamma..gamma.'-dipyridylium granule, at pelletize dwell time in the tower 40min, obtains particle diameter less than 5mm (0.2-2.5
Mm) N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular, rear finished product is packed after testing, and fine grained particle returns to make
Grain tower continues pelletize.
Fluidization granulation tower structure form is ibid, described in order to support crystal seed and the distribution of dispersion fluidizing agent
The version of plate is cone hat type；Perforate arrangement is equilateral triangle；Percent opening is 8%.Described material
Liquid atomization device is the spacing being located at fluidization granulation tower both sides, feed liquid nebulizer and distribution grid of branched arrangement
From for 900mm；It, feed liquid nebulizer is upper-spraying type.
Described feed liquid nebulizer is pressure type, and its gas-liquid mass ratio is 0.4, and the atomizing angle of nozzle is 80 °.
Embodiment 3
N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation is grouped into by the one-tenth of following weight percents: 60% N,N'-dimethyl-.gamma..gamma.'-dipyridylium dichloro
Compound, 0.1% stink agent, emetic triazolo pyrimidine ketone be equivalent to paraquat dichloride weight 0.18%,
0.05% pigment, 20% surfactant polyethylene fatty acid ester PEG-400, remaining use filler sulfur
Acid sodium is supplied.
Preparation:
According to the above ratio raw material is mixed, stirs, use electrical heating that feed liquid is heated to 60 DEG C,
In two streaming pressure atomizer sent into by feed pump, air is heated to 220 DEG C and leads to as fluidizing agent
The effect crossing the pre-distributing chamber of gas and distribution grid enters into equipped with in the fluidization granulation tower of crystal seed, and crystal seed exists
In stabilization fluid state under the effect of fluidized hot medium, N,N'-dimethyl-.gamma..gamma.'-dipyridylium feed liquid is atomized device and is atomized to 70～80
μm continuous spray is peripheral at crystal seed, control inlet amount maintain the temperature in granulation tower at 100～110 DEG C,
Steam granulation tail gas is taken away, and tail gas combines through two stage cyclone separator and cloth envelop collector successively and removes
Dirt purified treatment, fine dust returns to fluidization granulation tower as crystal seed, warp the most successively after tail gas removing dust
Cross washing absorption and the further purified treatment of activated carbon adsorption operation, empty under the effect of air-introduced machine,
The particle dust of trapping returns to fluidization granulation tower as crystal seed, and finished granule is at the wind of different gradients
Sequentially entering dry classification region under speed and carry out screening operation, N,N'-dimethyl-.gamma..gamma.'-dipyridylium granule stops in granulation tower
Time 30min, obtains the particle diameter N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular less than 5mm (0.2-2.5mm), through inspection
After survey, finished product is packed, and fine grained particle returns to continue in granulation tower pelletize.
Fluidization granulation tower structure form is ibid, described in order to support crystal seed and the distribution of dispersion fluidizing agent
The version of plate is cover-plate type；Perforate arrangement is equilateral triangle；Percent opening is 8%.Described material
Liquid atomization device is the both sides being located at fluidization granulation tower of branched arrangement, between feed liquid nebulizer and distribution grid
Distance is 900mm；It, feed liquid nebulizer is upper-spraying type.
Described feed liquid nebulizer is pressure type, and its gas-liquid mass ratio is 0.3, and the atomizing angle of nozzle is 100 °.
Embodiment 4
N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation is grouped into by the one-tenth of following weight percents: 40% N,N'-dimethyl-.gamma..gamma.'-dipyridylium two
Chloride, 0.1% stink agent, emetic triazolo pyrimidine ketone are equivalent to paraquat dichloride weight
0.18%, 0.05% pigment, 25% surfactant polyoxyethylene sorbitan fatty acid ester
TWEEN-80, remaining supply with filler ammonium sulfate,
Preparation:
Raw material is mixed and added into preparing paraquat dichloride in granule, surface activity by aforementioned proportion
After agent, stink agent, emetic, pigment and filler mixing, the water of weight 20% stirs, and uses
Feed liquid is heated to 60 DEG C by electrical heating, and in two streaming pressure atomizer sent into by feed pump, air is through adding
Heat is entered into equipped with crystalline substance by the effect of the pre-distributing chamber of gas and distribution grid to 220 DEG C as fluidizing agent
Kind fluidization granulation tower in, crystal seed under the effect of fluidized hot medium in stabilization fluid state, N,N'-dimethyl-.gamma..gamma.'-dipyridylium
It is peripheral at crystal seed to 70～80 μm continuous sprays that feed liquid is atomized device atomization, controls inlet amount maintenance and makes
Temperature in grain tower is at 110～120 DEG C, and steam granulation tail gas is taken away, and tail gas revolves through two-stage successively
Wind separator and cloth envelop collector combination udst separation process, and fine dust returns to fluidization granulation tower conduct
Crystal seed, sequentially passes through after tail gas removing dust at washing absorption and the purification further of activated carbon adsorption operation again
Reason, empties under the effect of air-introduced machine, and the particle dust of trapping returns to fluidization granulation tower as crystalline substance
Kind, finished granule sequentially enters dry classification region under the wind speed of different gradients and carries out screening operation,
N,N'-dimethyl-.gamma..gamma.'-dipyridylium granule, at pelletize dwell time in the tower 30min, obtains particle diameter less than 5mm (0.2-2.5mm)
N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular, after testing after finished product pack, fine grained particle returns to granulation tower
Middle continuation pelletize.
Fluidization granulation tower structure form is ibid, described in order to support crystal seed and the distribution of dispersion fluidizing agent
The version of plate is cone hat type；Perforate arrangement is circular；Percent opening is 5%.Described feed liquid mist
Change device be branched arrangement be located at fluidization granulation tower both sides, feed liquid nebulizer with the spacing of distribution grid is
1000mm；It, feed liquid nebulizer is upper-spraying type.
Described feed liquid nebulizer is pressure type, and its gas-liquid mass ratio is 0.5, and the atomizing angle of nozzle is 90 °
Embodiment 5
N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation is grouped into by the one-tenth of following weight percents: 80% N,N'-dimethyl-.gamma..gamma.'-dipyridylium two
Chloride (, 0.1% stink agent, emetic triazolo pyrimidine ketone be equivalent to paraquat dichloride weight
0.18%, 0.05% pigment, 8% surfactant polyethylene fatty acid ester PEG-400, remaining is with filling out
Fill agent sodium chloride to supply.
Preparation:
According to the above ratio raw material is mixed, stirs, use electrical heating that feed liquid is heated to 60 DEG C,
In two streaming pressure atomizer sent into by feed pump, air is heated to 220 DEG C and leads to as fluidizing agent
The effect crossing the pre-distributing chamber of gas and distribution grid enters into equipped with in the fluidization granulation tower of crystal seed, and crystal seed exists
In stabilization fluid state under the effect of fluidized hot medium, N,N'-dimethyl-.gamma..gamma.'-dipyridylium feed liquid is atomized device and is atomized to 90～100
μm continuous spray is peripheral at crystal seed, control inlet amount maintain the temperature in granulation tower at 110～120 DEG C,
Steam granulation tail gas is taken away, and tail gas combines through two stage cyclone separator and cloth envelop collector successively and removes
Dirt purified treatment, fine dust returns to fluidization granulation tower as crystal seed, warp the most successively after tail gas removing dust
Cross washing absorption and the further purified treatment of activated carbon adsorption operation, empty under the effect of air-introduced machine,
The particle dust of trapping returns to fluidization granulation tower as crystal seed, and finished granule is at the wind of different gradients
Sequentially entering dry classification region under speed and carry out screening operation, N,N'-dimethyl-.gamma..gamma.'-dipyridylium granule stops in granulation tower
Time 20min, obtains the particle diameter N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular less than 5mm (0.2-2.5mm), through inspection
After survey, finished product is packed, and fine grained particle returns to continue in granulation tower pelletize.
Fluidization granulation tower structure form is ibid, described in order to support crystal seed and the distribution of dispersion fluidizing agent
Plate structure form is porous type；Perforate arrangement is equilateral triangle；Percent opening is 7%.Described feed liquid
Nebulizer is the spacing being located at fluidization granulation tower both sides, feed liquid nebulizer and distribution grid of branched arrangement
For 1200mm；It, feed liquid nebulizer is following spray.
Described feed liquid nebulizer is pressure type, and its gas-liquid mass ratio is 0.5, and the atomizing angle of nozzle is 60 °
The various embodiments described above gained water-soluble granular formulation, its property indices is excellent, and measurement result is such as
Shown in table 1:
Table 1 N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation performance indications testing result
Separately, by the N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation 40-100g of the present invention, it is dissolved in 25kg water formation all
Target weeds are carried out stem and leaf spraying treatment by one solution.
Embodiment 6
Biological activity determination:
In order to compare with embodiments of the invention, under greenhouse experiment, by embodiment 1～embodiment 3 profit
By potted plant test method, (it is purchased from Shandong green despot chemical industry share limited with commercially available 20% N,N'-dimethyl-.gamma..gamma.'-dipyridylium water preparation
Company) carry out biological activity test for comparison medicament.When using, N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation is prepared
After becoming aqueous solution, weeds are carried out spraying treatment and test its activity of weeding.
Quantitative Setaria glauca seed is sowed at respectively in the height Disposable paper cup for 9cm, after broadcasting
Earthing 0.5cm, cultivates after suppression, trickle in greenhouse according to a conventional method.Treat Setaria glauca 3.5 leaf
During the phase, by EXPERIMENTAL DESIGN dosage crawler type crops sprayer, (Britain Engineer Research Ltd. sets
Family planning is produced) carry out stem and leaf spraying treatment (atomisation pressure 1.95kg/cm2, spouting liquid 500L/ha, crawler belt
Speed 1.48km/h).Test is repeated 4 times.
Examination material processes and is placed on handling hall, after medicinal liquid natural air drying, is put in greenhouse according to a conventional method
Management, observes and records the weeds response situation to medicament, and weeds are prevented and kill off by periodical visual inspection investigation medicament
Effect.The periodical visual inspection investigation medicament preventive effect to weeds, result is as shown in table 2, table 3.
The table 2. N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation range estimation preventive effect result to Setaria glauca
The table 3. N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation ED to Setaria glauca90Value
As it appears from the above, from reagent agent range estimation preventive effect result (being shown in Table 2) to Setaria glauca,
N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation (embodiment 1#～embodiment 3#) is equal to the range estimation preventive effect of Setaria glauca
It is better than compareing medicament 20% N,N'-dimethyl-.gamma..gamma.'-dipyridylium water preparation, especially embodiment 3# from 40～320g a.i./hm2Dosage
In the range of, it is superior to compare medicament.Application DPS2000 data handling system is to reagent agent in table 1
The range estimation preventive effect data of Setaria glauca are carried out statistical analysis, calculates reagent agent to golden Canis familiaris L. tail
The ED of grass90Value (is shown in Table 3), N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation (embodiment 1#～embodiment 3#) and right
According to the medicament 20% N,N'-dimethyl-.gamma..gamma.'-dipyridylium water preparation ED to Setaria glauca90Value is respectively 238.9,244.0,175.6
With 302.4g a.i./hm2.It can thus be seen that reagent agent to Setaria glauca activity order by height
To low: embodiment 3#, embodiment 1#, embodiment 2#, 20% N,N'-dimethyl-.gamma..gamma.'-dipyridylium water preparation, the most permissible
Illustrating that the N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation of the present invention has significant activity of weeding, biological property is excellent.
Claims (3)
1. the preparation method of a N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation, it is characterised in that: warp after feed liquid is heated
Two streaming nebulizers spray in the granulation zone in fluidization granulation tower continuously, and pressure fan is by heated new
Fresh purification air enters into equipped with crystal seed by the pre-distributing chamber of gas and through distribution grid as fluidizing agent
Granulation tower in, crystal seed under the effect of fluidized hot medium in stabilization fluid state, feed liquid be atomized to
50～100 μm continuous sprays are at peripheral " coating " granulating of crystal seed, and finished granule is at the wind speed of different gradients
Under sequentially enter dry classification region carry out screening operation, thus by control zones of different fluidisation speed
The purpose that degree realizes carrying out separating in granulation tower obtains the particle diameter N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular less than 5mm
Agent；
Described feed liquid is atomized to 50～100 μm and is sprayed on peripheral " coating " granulating of crystal seed continuously, and maintains
Temperature in granulation tower is at 70～180 DEG C, and in granulation process, steam granulation tail gas is taken away, tail gas
Processing through built-in sack cleaner and dust removal installation udst separation, after process, fine dust returns to fluidisation and makes
Grain tower is as crystal seed, and tail gas sequentially passes through at washing absorption tower and activated carbon adsorber purification further again
Reason, then empties under the effect of air-introduced machine.
2. the preparation method of the N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation as described in claim 1, it is characterised in that:
Described feed liquid be paraquat dichloride, surfactant, stink agent, emetic, pigment and
The mixture of filler；
Or mixing after add water, the addition of water be paraquat dichloride, surfactant, stink agent,
The 1-80% of weight after emetic, pigment and filler mixing；The described feed liquid being configured to be heated to 40～
70 DEG C, stand-by.
3. the preparation method of the N,N'-dimethyl-.gamma..gamma.'-dipyridylium water-soluble granular formulation as described in claim 2, it is characterised in that:
Described paraquat dichloride, surfactant, stink agent, emetic, pigment and filler,
By weight percentage, paraquat dichloride 40-95%, surfactant 1-30%, stink agent
0-2%, emetic triazolo pyrimidine ketone is equivalent to the 0-2% of paraquat dichloride, pigment 0-2% and fills out
Fill agent 1-58%.
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|---|---|---|---|---|
| CN101700480A (en) * | 2009-11-11 | 2010-05-05 | 王新月 | Production method of large continuous fluidized bed for spraying, granulating and coating |
| CN101829521A (en) * | 2010-04-30 | 2010-09-15 | 王新月 | Fluidized bed granulator |
| CN102083518A (en) * | 2008-04-28 | 2011-06-01 | 亚拉国际有限公司 | Method and device for processing of granules |
| CN102578099A (en) * | 2012-01-18 | 2012-07-18 | 南京华洲药业有限公司 | Water-soluble granule formulation containing paraquat dichloride and preparation method of water-soluble granule formulation |
| CN103734126A (en) * | 2013-12-27 | 2014-04-23 | 山东省农药科学研究院 | Water-soluble granule containing paraquat dichloride and preparation method of water-soluble granule |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102083518A (en) * | 2008-04-28 | 2011-06-01 | 亚拉国际有限公司 | Method and device for processing of granules |
| CN101700480A (en) * | 2009-11-11 | 2010-05-05 | 王新月 | Production method of large continuous fluidized bed for spraying, granulating and coating |
| CN101829521A (en) * | 2010-04-30 | 2010-09-15 | 王新月 | Fluidized bed granulator |
| CN102578099A (en) * | 2012-01-18 | 2012-07-18 | 南京华洲药业有限公司 | Water-soluble granule formulation containing paraquat dichloride and preparation method of water-soluble granule formulation |
| CN103734126A (en) * | 2013-12-27 | 2014-04-23 | 山东省农药科学研究院 | Water-soluble granule containing paraquat dichloride and preparation method of water-soluble granule |
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