CN108623333A - The manufacturing method of granular oxamides - Google Patents
The manufacturing method of granular oxamides Download PDFInfo
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- CN108623333A CN108623333A CN201711224786.5A CN201711224786A CN108623333A CN 108623333 A CN108623333 A CN 108623333A CN 201711224786 A CN201711224786 A CN 201711224786A CN 108623333 A CN108623333 A CN 108623333A
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- oxamides
- granular
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- water
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C11/00—Other nitrogenous fertilisers
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G5/00—Fertilisers characterised by their form
- C05G5/10—Solid or semi-solid fertilisers, e.g. powders
- C05G5/12—Granules or flakes
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Fertilizers (AREA)
Abstract
The present invention provides that shape stability during a kind of fertiliser granulates hardness is high and water is high, the granular oxamides with stable sustained-release, can reduce top dressing number and mitigate top dressing workload.By relative to the mixture containing more than 0.5 parts by weight polyvinyl alcohol or modified polyvinylalcohol of 100 parts by weight of oxamides powder in the mixing pan container of apsacline High Shear Mixer Granulator, be then dried and manufacture.
Description
Technical field
The present invention relates to a kind of manufacturing methods of granular oxamides, in more detail, it is high and in water to be related to a kind of fertilizer hardness
The manufacturing method of high, with stable sustained-release fertilizer efficiency the granular oxamides of disintegration resistance in sweetening of the soil.
Background technology
One of the feature changed to the structure of agricultural production in 2015 in 2010 is agriculture management body quantity, sale peasant household quantity
Slip was highest in the past, and agriculture practitioner is constantly aging.Therefore, in farmland, the physical work of fertilising operation is reduced to the greatest extent
The fertilizer added with slow release nitrogen that work amount and reduction top dressing number can be completed is utilized extensively.Oxamides (Oxamide)
[(CONH2)2] it is one of its typical example, it is odorless white powder, solubility is low in water, and does not have to crops
Drug illeffects etc. is excellent slow release nitrogenous fertilizer, therefore is used always.
But powder oxamides can occur inorganization faster (to refer to that oxamides is decomposed into because of the microorganism in soil
The form being absorbed by plants), inorganization nitrogen component is easy soluble easily in water with ammonium sulfate, urea, ammonium chloride and ammonium nitrate etc.
Chemical nitrogen fertilizer is similarly easy tod produce to be lost caused by loss etc., therefore is unable to give full play the slow release feature of oxamides.
In addition, so that it is contained oxamides even if being kneaded oxamides in chemical fertilizer, since fertiliser granulates can be disintegrated quickly under irrigation condition,
Therefore can by with decompose relevant microorganism fast decoupled, can not also play slow release fertilizer efficiency.
In general, oxamides is dissolved out and inhibited into water sweetening of the soil by control oxamides and decomposes the micro- of oxamides
Biological can reduce the inorganization speed of oxamides, make the fertilizer efficiency slow of oxamides.Oxamides is controlled to neutralize to water
It is dissolved out in soil, needs granule strength high as much as possible, and be formed in water sweetening of the soil the granular of not easy disintegrating.
Granulation when pelletizing as fertilizer promotes material (binder), it is known to use bentonite, molasses, lignin sulfonic acid
Salt, starch, konjaku flour, sodium alginate, carboxymethyl cellulose (CMC), polyvinyl alcohol (PVA), polyacrylamide (PAM), gypsum,
Sodium humate etc. (non-patent literature 1).
As using these materials, it is intended to which the granule strength and particle for improving the fertiliser granulates containing oxamides are not disintegrated in water
And keep the characteristic (shape stability in water) of its shape etc. and control dissolution, inhibit oxamides to decompose relevant microorganism with it
The technology of contact, discloses and fertilizer is made as follows：It is combined and is squeezed into oxamides powder by polyvinyl alcohol
Type is rodlike, and graininess (patent document 1) is then made；It is stick to be combined extrusion forming with oxamides powder by polyvinyl alcohol
Graininess molding after graininess then is made, is deformed into spherical (patent document 2) by shape using high speed rotation granulator；Profit
With Pan granulator, granulator etc. is squeezed, to containing the iron compounds such as oxamides and ferric sulfate, iron chloride, ferric nitrate and phosphorus
The composition of the ammonium phosphate salts such as sour monoammonium is pelletized (patent document 3)；Using Pan granulator, extruding granulator etc., to containing
There is the composition of the ammonium phosphate salts such as the aluminium compounds such as oxamides, gypsum and aluminum sulfate, aluminium chloride, aluminum nitrate and ammonium phosphate to carry out
It pelletizes (patent document 4)；Fertilizer is set to contain oxamides and ammonium chloride, Diammonium phosphate (DAP), gypsum and utilization Pan granulator, squeeze system
Grain machine etc. is pelletized (patent document 5).
In addition, patent document 6 discloses following invention：Fertilizer is set to contain 90 moles of 1800 or less the degree of polymerization, saponification degree %
Polyvinyl alcohol and raw material fertilizer below (specially process slag phosphatic manure, slag silicate matter fertilizer, mixed phosphate fertilizer,
Chemical fertilizer) and it is pelletized using Pan granulator, provide that a kind of granule strength is high, the excellent grain of disintegration in water especially at low temperature
Shape fertilizer.
But in the method for patent document 1, the hardness of graininess oxamides is relatively low, be 2kgf hereinafter, have molding after
The problem of dusting occurs in bag.In the method for patent document 2, the hardness of spherical oxamides is relatively low, be 3kgf hereinafter, and to
It is made spherical, needs after being mixed with twin shaft roll shape mixing machine, extrusion forming, reuse Fuji Paudal Co., Ltd.
The Spheroidgranulatemachine of manufacture needs two or more equipment to manufacture as high speed rotation granulator.In addition, patent document 3,4,
It is 5~9kgf, the ratio due to additive relative to powdery oxamides although the hardness of granular fertilizer is high in 5 method
Height, therefore the shortcomings that tail off there are the nitrogen quantity from oxamides in granular fertilizer.In addition, about slow with the stabilization of granular oxamides
The property released fertilizer efficiency has shape stability in the water of direct relation, is in patent document 12 weeks, is 1 hour in patent document 3,4, specially
In sharp document 5 be 10 hours, result is the short time, as under irrigation condition in water with the slow release fertilizer efficiency in soil not
Fully.In addition, in the water that the technology of patent document 6 provides the excellent granular fertilizer of disintegration with as the object of the invention in water
In not easy disintegrating granular oxamides it is different.
In patent document 7, the example for nitrifying the method for granulating for inhibiting material mixed fertilizer is coated as manufacturing,
In, the cladding nitrification, which inhibits material mixed fertilizer, to be inhibited by coating cladding nitrification made of nitrification inhibitor with covering material
What material was mixed with the fertilizer containing ammonium nitrogen and/or urea nitrogen, it records and puts into nitre in tilting dish-type granulator
Change the powder such as inhibitor, fertilizer, and the method that the aqueous solution of lignosulfonates, molasses etc. are pelletized as binder；
Use the method for squeezing granulator；Use the vertical method etc. for being permitted the mixer-granulators such as (EIRICH) mixing machine of love.
In patent document 8, as the example for inhibiting the method for granulating of material for manufacturing cladding nitrification, wherein the packet
It is that nitrification inhibitor (wherein, contains nitric nitrogen and ammonium nitrogen form as nitrogen component with diluent to cover nitrification to inhibit material
Except chemical fertilizer and urea) it mixes and carries out made of granular nitrification made of spheroidizing inhibits material to be coated with covering material, work
It for the example of method of granulating, records and puts into the powder such as nitrification inhibitor, chemical fertilizer in tilting dish-type granulator, and by lignin
The method that aqueous solution, molasses of sulfonate etc. are pelletized as binder；Use the method for squeezing granulator；Permitted using love is vertical
The method etc. of the mixer-granulators such as mixing machine.
But apsacline is not utilized to love vertical mixing machine perhaps in the spheroidizing of oxamides manufacture.
Existing technical literature
Patent document
Patent document 1：Japanese Unexamined Patent Application 59-169527 bulletins
Patent document 2：Japanese Unexamined Patent Publication 2-145493 bulletins
Patent document 3：Japanese Patent Publication 6-2628 bulletins
Patent document 4：Japanese Patent Publication 6-2629 bulletins
Patent document 5：Japanese Patent Publication 6-2630 bulletins
Patent document 6：Japanese Unexamined Patent Publication 2006-21968 bulletins
Patent document 7：Japanese Unexamined Patent Publication 2000-53481 bulletins (1,0011 section of claim, Production Example 1,6)
Patent document 8：Japanese Unexamined Patent Publication 2000-53482 bulletins (1,0014 section of claim, Production Example 1,2)
Non-patent literature
Non-patent literature 1：" fertilizer processing is learned " granulation promotes material (binder) BSI bioscience research institute
Invention content
It is high the issue of the present invention is to provide a kind of fertilizer hardness and in water with the disintegration resistance in soil it is high, have
The granular oxamides of stable sustained-release fertilizer efficiency.
The present inventor is concentrated on studies in order to solve the above problems, as a result, it has been found that, it is poly- by making oxamides contain
Vinyl alcohol or modified polyvinylalcohol, and High Shear Mixer Granulator and drying are carried out in apsacline mixing pan container, fertilizer can be improved
Expect hardness, and can also keep grain shape stability higher under the conditions of water storage condition and dry land, so as to complete this hair
It is bright.
That is, the main points of the present invention are as follows.
(1) a kind of manufacturing method of granular oxamides, which is characterized in that will be relative to 100 parts by weight of oxamides powder
Mixture containing more than 0.5 parts by weight polyvinyl alcohol or modified polyvinylalcohol high-speed stirring in the mixing pan container of apsacline
Mixing grain, is then dried.
(2) manufacturing method according to above-mentioned (1), wherein High Shear Mixer Granulator is carried out using high-speed stirring mixer,
The high-speed stirring mixer includes：The mixing pan of rotation, configuration are on the position for deviateing the mixing pan center and independent
The blend tool that is rotated in mixing pan, be fixedly arranged on the mixing pan inside scraper plate.
(3) manufacturing method according to above-mentioned (2), wherein after addition polyvinyl alcohol or modified polyvinylalcohol and water
High Shear Mixer Granulator time be 13~60 minutes.
Invention effect
According to the present invention, by provide fertilizer hardness it is high and in water with the disintegration resistance in soil it is high, can play stably
The granular oxamides of slow release fertilizer efficiency can reduce the top dressing number in arviculture, can to adjoint in recent years agricultural from
Dealer is aging and mitigates fertilising workload.
Description of the drawings
Fig. 1 is the general perspective of an example for the high-speed stirring mixer for indicating to use in carrying out the present invention.
Fig. 2 is the figure for indicating inorganization test result under the conditions of 25 DEG C, paddy field.
Accompanying drawings symbol description
1 high-speed stirring mixer
2 mixing pans
3 blend tools
4 scraper plates
Specific implementation mode
The polyvinyl alcohol or modified polyvinylalcohol used in the present invention, the degree of polymerization are 1300~2400, viscosity (mPa
S it is) 15~50, saponification degree (mol%) is 90 or more；Preferably, the degree of polymerization be 1700~1800, viscosity (mPaS) be 20~
30, saponification degree (mol%) is 98.0~99.7, but is not limited to above range.
It is not particularly limited as modified polyvinylalcohol, it is, for example, possible to use sour modified polyvinylalcohol is (hereinafter also referred to
" sour modified PVA "), ethylene modified polyvinyl alcohol etc..
Sour modified PVA is the carboxyl containing specified amount and sulfonic vinyl alcohol polymer, the former is referred to as carboxyl acid modified
PVA, the latter are known as sulfonic acid modified PVA.
Carboxyl acid modified PVA can by with existing known method by the compound with carboxyl be introduced into polyvinyl alcohol come
It is manufactured.As the compound with carboxyl, there are：Fumaric acid, maleic acid, itaconic acid, maleic anhydride, phthalic acid
Acid anhydride, trimellitic anhydride, acrylic acid and their salt etc..
Sulfonic acid modified PVA can be by that will have sulfonic compound to be introduced into polyvinyl alcohol with existing known method
To be manufactured.As with sulfonic compound, there are：Ethionic acid, propene sulfonic acid, methacrylic sulfonic acid, 2- third
The salt etc. of acrylamide -2- methyl propane sulfonic acids and they.
Ethylene modified polyvinyl alcohol is obtained by the copolymer saponification by vinyl esters and ethylene, as vinyl esters,
It there are：Vinyl formate, vinylacetate, vinyl propionate, pivalic acid vinyl acetate etc..
The content of polyvinyl alcohol or modified polyvinylalcohol in the granular oxamides of the present invention, from ensuring in pellet hardness and water
It sets out in terms of shape stability, is 0.5 parts by weight or more, preferably 1~10 weight relative to 100 parts by weight of oxamides powder
Part, more preferably 1~2 parts by weight.If the content of the polyvinyl alcohol or modified polyvinylalcohol is less than 0.5 parts by weight, making
Effect when grain as binder can die down, and improve the effect of pellet hardness after pelletizing and can reduce；On the other hand, if it exceeds 10
Parts by weight, then the nitrogen component of granular oxamides can be lower, the quality of ingredient can reduce.
The preferred embodiment of the manufacturing method of the granular oxamides of the present invention is illustrated below.
First, polyvinyl alcohol or modified polyvinylalcohol are dissolved according to following main points.Normal-temperature water is stirred on one side, on one side
Slowly polyvinyl alcohol or modified polyvinylalcohol of the input through metering, begins to warm up in the state of lasting stirring.Solution temperature reaches
To after 90~95 DEG C, persistently stirred while keeping temperature 1~2 hour.It is then shut off heat source, reduces mixing power, it is slowly cold
But, certain density polyvinyl alcohol or modified poly ethylene alcohol solution are prepared.The concentration of polyvinyl alcohol or modified polyvinylalcohol liquid
It is not particularly limited, but as viscosity when handling and additive amount when manufacture fertilizer, 10%~15% solution is suitable.It connects
It, polyvinyl alcohol or modified polyvinylalcohol liquid prepared by dissolving is slowly added, to reach it relative to the oxalyl for being put into granulator
100 parts by weight of amine powder are the weight ratio of 0.5 parts by weight or more, and the High Shear Mixer Granulator in apsacline mixing pan container makes
Object of pelletizing is dried.About the polyvinyl alcohol or modified polyvinylalcohol being added in oxamides powder, in order to make between raw material powder
Binding force is average, is advisable so that liquid addition is made, but can also powdery addition when additive amount is few.In addition, in order to adjust unit weight
And prevent from floating in water, other than oxamides powder, mineral dust etc. can also be added.
Granulator for granulation, which is that Japanese love is vertical, is permitted holding with apsacline mixing pan for (EIRICH) Co., Ltd. manufacture
The High Speed Stirring Machine (hereinafter referred to as apsacline love is vertical is permitted mixing machine) of device, details are recorded in Japanese Patent No. 4406328
Number bulletin, the granulation of the high-performance mixing machine characterized by careful high yield《The basis of powder technology and application》Chemical device 9
The moon supplement, industrial communication society, 2005.
Fig. 1 is the general perspective of an example for the high-speed stirring mixer for indicating to use in carrying out the present invention.
As shown in Figure 1, the high-speed stirring mixer 1 used in the present invention includes：Mixing pan 2, receiving are stirred object,
It is rotated in the state that receiving is stirred object；Blend tool (also referred to as " blender ") 3, is located at the inside of the mixing pan 2,
It configures on the position of center for deviateing mixing pan 2, is rotated independently of mixing pan 2；And scraper plate 4, fixation are matched
It sets in the inside of mixing pan 2.The direction respectively independently rotated and rotating speed can be arranged in mixing pan 2 and blend tool 3, under can passing through
The case where stating two kinds of stirring means to be stirred, i.e., setting the direction of rotation of mixing pan 2 and blend tool 3 to opposite direction
Under, and in the case of setting the direction of rotation of mixing pan 2 and blend tool 3 to the same direction.
The summary of operating procedure is as follows.After fertilizer material is put into equipment, the peripheral speed of rotor is improved (usually
For 1~10m/s, preferably 2~6m/s) it is mixed, keep raw material uniform.Then polyvinyl alcohol or modified polyvinylalcohol liquid is added
With addition water.The peripheral speed (being usually 10~40m/s, preferably 15~35m/s) for improving rotor, is disperseed and is pelletized.
About the High Shear Mixer Granulator time after addition polyvinyl alcohol or modified polyvinylalcohol and water, from the production rate of target grain size
Aspect is set out, preferably 13 minutes or more, from preventing from becoming bulk state aspect because particle is attached to each other, preferably
60 minutes or less.The time of above-mentioned High Shear Mixer Granulator is more preferably 15~45 minutes, further preferably 20~45 minutes.So
Afterwards, the peripheral speed (1~10m/s, preferably 2~6m/s) for reducing rotor is handled, and is finally discharged from mixing machine.Dry
The shot-like particle that heat drying obtains in dry device, to manufacture granular oxamides.Drying temperature is usually 65~130 DEG C, preferably
90~120 degrees Celsius.
The shapes and sizes of the granular oxamides of the present invention are not particularly limited, and usually have grain within the scope of 1~10mm
Diameter it is granular.Especially granular oxamides of the grain size within the scope of 2~4mm, operability is good, dispersing when can mitigate fertilising
Deng, therefore preferably.In addition, even if seldom occurring if in the case where mixing the granulating composition of the present invention with other chemical fertilizer
Classification, good mixing.
Embodiment
The present invention is described in further details below by embodiment and comparative example, but the present invention is not implemented by these
Example limitation.
The purity that polyvinyl alcohol (PVA) or modified polyvinylalcohol (modified PVA) use is 94.00% or more.Its additive amount
(%) is indicated with the weight ratio relative to oxamides powder.
(embodiment 1) likes the vertical granular oxamides for being permitted mixing machine manufacture added with 1% modified PVA using apsacline
The 5L beakers for being put into 2.7 parts by weight water are placed in the hot bath of room temperature, stirring motor is set, is stirred on one side
Water, be slowly added on one side 0.3 parts by weight modified polyvinylalcohol (Kuraray Co., Ltd.'s system, the degree of polymerization 1300, saponification degree 92~
98).It is heated, after reaching 95 DEG C, is stirred 2 hours while keeping temperature while agitating.Confirm that modified PVA is complete
Dissolving reduces mixing power and Slow cooling, to prepare 10% solution.
The oxamides powder of 20 parts by weight is put into the vertical mixing machine perhaps of apsacline love, and (Japan's love is vertical to be permitted Co. Ltd. system
Make, intensive mixer R02 types, similarly hereinafter) mixing pan container in after, addition 2 parts by weight prepare 10% solution of modified PVA, with
Rotor peripheral speed 6m/s (900rpm) mixes 1 point 15 seconds.Then the water for adding 3.53 parts by weight, with rotor peripheral speed 19m/
S (3000rpm) carries out dispersion and granulation in 23 minutes, and rotor peripheral speed is down to 6m/s (900rpm) and carries out 1 point 30 seconds
It is discharged after identical processing.After being dried the granular product of discharge 4 hours with 105 DEG C of driers, it is sized to 2~4mm's of grain size
Range, to obtain the granular oxamides added with 1% modified PVA.
(embodiment 2) likes the vertical granular oxamides for being permitted mixing machine manufacture added with 2%PVA using apsacline
The 10L beakers for being put into 5.4 parts by weight water are placed in the hot bath of room temperature, stirring motor is set, is stirred on one side
Water is slowly added the PVA of 0.6 parts by weight on one side.It is heated while agitating, after reaching 95 DEG C, is keeping the same of temperature
When stir 2 hours.Confirm that PVA is completely dissolved, reduce mixing power and Slow cooling, to prepare 10% solution.
After the oxamides powder of 20 parts by weight is put into the vertical mixing pan container for being permitted mixing machine of apsacline love, addition 4
PVA10% solution prepared by parts by weight is mixed 1 minute with rotor peripheral speed 6m/s (900rpm).Further 1.66 weights of addition
The water for measuring part is carried out dispersion and granulation in 21 minutes with rotor peripheral speed 19m/s (3000rpm), rotor peripheral speed is dropped
It is discharged to 6m/s (900rpm) and after carrying out identical processing in 2 minutes.The granular product of discharge are dried 4 with 105 DEG C of driers
After hour, it is sized to the range of 2~4mm of grain size, to obtain the granular oxamides added with 2%PVA.
(embodiment 3) likes the vertical granular oxamides for being permitted mixing machine manufacture added with 1%PVA using apsacline
After the oxamides powder of 20 parts by weight is put into the vertical mixing pan container for being permitted mixing machine of apsacline love, addition 2
The PVA10% solution prepared in parts by weight of example 2 is mixed 1 minute with rotor peripheral speed 6m/s (900rpm).Further add
The water for adding 3.63 parts by weight is carried out dispersion and granulation in 22 minutes with rotor peripheral speed 19m/s (3000rpm), rotor is justified
Circular velocity is down to 6m/s (900rpm) and is discharged after carrying out identical processing in 2 minutes.With 105 DEG C of driers by the granular of discharge
After product are dried 4 hours, it is sized to the range of 2~4mm of grain size, to obtain the granular oxamides added with 1%PVA.
(embodiment 4) likes the vertical granular oxamides for being permitted mixing machine manufacture added with 4% modified PVA using apsacline
The 10L beakers for being put into 4.8 parts by weight water are placed in the hot bath of room temperature, stirring motor is set, is stirred on one side
Water is slowly added the modified polyvinylalcohol of 1.2 parts by weight on one side.It is heated, after reaching 95 DEG C, is being kept while agitating
It is stirred 2 hours while temperature.Confirm that modified PVA is completely dissolved, reduces mixing power and Slow cooling, it is molten to prepare 20%
Liquid.
After the oxamides powder of 20 parts by weight is put into the vertical mixing pan container for being permitted mixing machine of apsacline love, addition 4
20% solution of modified PVA prepared by parts by weight is mixed 1 minute with rotor peripheral speed 6m/s (900rpm).Further addition
The water of 2.3 parts by weight carries out dispersion and granulation in 18 minutes with rotor peripheral speed 19m/s (3000rpm), by rotor circumference speed
Degree is down to 6m/s (900rpm) and is discharged after carrying out identical processing in 2 minutes.The granular product of discharge are done with 105 DEG C of driers
After dry 4 hours, it is sized to the range of 2~4mm of grain size, to obtain the granular oxamides added with 4% modified PVA.
(embodiment 5) likes the vertical granular oxamides for being permitted mixing machine manufacture added with 0.5% modified PVA using apsacline
After the oxamides powder of 20 parts by weight is put into the vertical mixing pan container for being permitted mixing machine of apsacline love, addition 1
10% solution of modified PVA prepared in parts by weight of example 1 mixes 1 point 15 seconds with rotor peripheral speed 6m/s (900rpm).
Then the water for adding 4.4 parts by weight carries out dispersion and granulation in 23 minutes with rotor peripheral speed 19m/s (3000rpm), will turn
Sub- peripheral speed is down to 6m/s (900rpm) and is discharged after carrying out 1 point of identical processing in 30 seconds.It will be discharged with 105 DEG C of driers
Granular product dry 4 hours after, the range of 2~4mm of grain size is sized to, to obtain the granular oxalyl added with 0.5% modified PVA
Amine.
(embodiment 6) likes the vertical granular oxamides for being permitted mixing machine manufacture added with 0.5%PVA using apsacline
After the oxamides powder of 20 parts by weight is put into the vertical mixing pan container for being permitted mixing machine of apsacline love, addition 1
The PVA10% solution prepared in parts by weight of example 2 mixes 1 point 15 seconds with rotor peripheral speed 6m/s (900rpm).Then add
The water for adding 4.4 parts by weight carries out dispersion and granulation in 23 minutes with rotor peripheral speed 19m/s (3000rpm), by rotor circumference
Speed is down to 6m/s (900rpm) and is discharged after carrying out 1 point of identical processing in 30 seconds.With 105 DEG C of driers by the granular of discharge
After product are dried 4 hours, it is sized to the range of 2~4mm of grain size, to obtain the granular oxamides added with 0.5%PVA.
(comparative example 1) likes the vertical granular oxamides for being permitted mixing machine manufacture added with 1% modified PVA using horizontal type
The oxamides powder of 20 parts by weight is put into the vertical mixing machine perhaps of horizontal type love, and (Japan's love is vertical to be permitted Co. Ltd. system
Make, intensive mixer DE14 types) mixing pan container in after, it is molten to add the modified PVA 10% for preparing in 2 parts by weight of example 1
Liquid is mixed 1 minute with rotor peripheral speed 13m/s (600rpm).The further water of 3.65 parts by weight of addition, with rotor circumference speed
Dispersion and granulation that 31m/s (1500rpm) is carried out 25 minutes are spent, rotor peripheral speed is down to 13m/s (600rpm) and carries out 2
It is discharged after minute identical processing.After the granular product of discharge are dried 4 hours with 105 DEG C of driers, be sized to grain size 2~
The range of 4mm, to obtain the granular oxamides added with 1% modified PVA.
(comparative example 2) manufactures the granular oxamides added with 1% modified PVA using Pan granulator
The oxamides powder of 20 parts by weight is put into the Pan granulator (electricity of Sumitomo Heavy Industries, Ltd's manufacture
Machine drive-type makes disk granulator by oneself) mixing pan container in after, add the modified PVA 10% prepared in 2 parts by weight of example 1
Solution is mixed 15 minutes with the peripheral speed 1.6m/s (40rpm) of disk.It is further slowly added the water of 8.02 parts by weight, simultaneously
Granulation in 30 minutes is carried out with the peripheral speed 1.6m/s (40rpm) of disk.The granular product for being obtained granulation with 105 DEG C of driers
After 4 hours dry, it is sized to the range of 2~4mm of grain size, to obtain the granular oxamides added with 1% modified PVA.
(comparative example 3) is using the manufacture of extruding granulator added with the granular oxamides of 1% modified PVA
The powder oxamides of 20 parts by weight is put into twin shaft roll shape mixing machine (manufacture of Fuji Paudal Co., Ltd.)
Afterwards, the water of the modified PVA 10% solution and 6.46 parts by weight that are prepared in 2 parts by weight of example 1 is added, is fully kneaded.
Mixture is put into screw extruding granulator (Fuji Paudal Co., Ltd. manufactures, sieve sieve pore 1.2mm), into
Row squeezes granulation.After being dried 24 hours from the granulation object squeezed out in sieve with 105 DEG C of driers, cut into 0.5~1cm's
Length obtains the small granular granular oxamides added with 1% modified PVA.
(comparative example 4) likes that vertical mixed mechanism of being permitted is granulated shape oxamides (do not add granulation and promote material) using apsacline
After the oxamides powder of 20 parts by weight is put into the vertical mixing pan container for being permitted mixing machine of apsacline love, addition
The water of 3.81 parts by weight is mixed 1 minute with rotor peripheral speed 6m/s (900rpm).The further water of 1.82 parts by weight of addition,
The dispersion and granulation that 32 minutes are carried out with rotor peripheral speed 19m/s (3000rpm), 6m/s is down to by rotor peripheral speed
It is discharged after (900rpm) and progress identical processing in 2 minutes.After the granular product of discharge are dried 4 hours with 105 DEG C of driers,
It is sized to the range of 2~4mm of grain size, to obtain granular oxamides.
(comparative example 5) likes the vertical granular oxamides for being permitted mixing machine manufacture added with 2% starch using apsacline
The starch of the oxamides powder of 20 parts by weight and 0.4 parts by weight is put into the vertical mixing for being permitted mixing machine of apsacline love
After in disk container, mixed 1 minute with rotor peripheral speed 6m/s (900rpm).Then the water for adding 5.1 parts by weight, is justified with rotor
Circular velocity 6m/s (900rpm) is mixed 1 minute.Then dispersion in 25 minutes is carried out with rotor peripheral speed 19m/s (3000rpm)
With granulation, rotor peripheral speed is down to 6m/s (900rpm) and is discharged after carrying out identical processing in 2 minutes.With 105 DEG C do
After dry device dries the granular product of discharge 4 hours, it is sized to the range of 2~4mm of grain size, to obtain the grain added with 2% starch
Shape oxamides.
(comparative example 6) likes the vertical granular oxalyl for being permitted mixing machine manufacture added with 2% carboxymethyl cellulose (CMC) using apsacline
Amine
The CMC of the oxamides powder of 20 parts by weight and 0.4 parts by weight is put into the vertical mixing for being permitted mixing machine of apsacline love
After in disk container, mixed 1 minute with rotor peripheral speed 6m/s (900rpm).Then the water for adding 5.1 parts by weight, is justified with rotor
Circular velocity 6m/s (900rpm) is mixed 1 minute.Then dispersion in 23 minutes is carried out with rotor peripheral speed 19m/s (3000rpm)
With granulation, rotor peripheral speed is down to 6m/s (900rpm) and is discharged after carrying out identical processing in 2 minutes.With 105 DEG C do
After dry device dries the granular product of discharge 4 hours, it is sized to the range of 2~4mm of grain size, to obtain added with the granular of 2%CMC
Oxamides.
(comparative example 7) likes the vertical granular oxamides for being permitted mixing machine manufacture added with mineral, ferric sulfate and phosphoric acid using apsacline
By the sulfuric acid of the oxamides powder of 20 parts by weight and the mineral (basalt powder) of 1.25 parts by weight, 0.42 parts by weight
Iron, 2.5 parts by weight phosphoric acid liquid put into the vertical mixing pan container for being permitted mixing machine of apsacline love after, with rotor peripheral speed
6m/s (900rpm) is mixed 1 minute.Then the water for adding 3.11 parts by weight mixes 1 with rotor peripheral speed 6m/s (900rpm)
Minute.Then the dispersion and granulation that 15.5 minutes are carried out with rotor peripheral speed 19m/s (3000rpm), by rotor peripheral speed
It is down to after 6m/s (900rpm) carries out identical processing in 2.75 minutes and is discharged.The granular product of discharge are done with 105 DEG C of driers
After dry 4 hours, it is sized to the range of 2~4mm of grain size, to obtain the granular oxamides added with ferric sulfate and phosphoric acid.
(comparative example 8) likes the vertical granular oxamides for being permitted mixing machine manufacture added with 0.2% modified PVA using apsacline
After the oxamides powder of 20 parts by weight is put into the vertical mixing pan container for being permitted mixing machine of apsacline love, addition
10% solution of modified PVA prepared in 0.4 parts by weight of example 1 mixes 1 point 15 with rotor peripheral speed 6m/s (900rpm)
Second.Then the water for adding 4.88 parts by weight carries out dispersion and granulation in 23 minutes with rotor peripheral speed 19m/s (3000rpm),
Rotor peripheral speed is down to 6m/s (900rpm) and is discharged after carrying out 1 point of identical processing in 30 seconds.It will with 105 DEG C of driers
After the granular product of discharge are dried 4 hours, it is sized to the range of 2~4mm of grain size, to obtain added with the granular of 0.2% modified PVA
Oxamides.
(comparative example 9) likes the vertical granular oxamides for being permitted mixing machine manufacture added with 0.2%PVA using apsacline
After the oxamides powder of 20 parts by weight is put into the vertical mixing pan container for being permitted mixing machine of apsacline love, addition
10% solution of PVA prepared in 0.4 parts by weight of example 2 mixes 1 point 15 seconds with rotor peripheral speed 6m/s (900rpm).It connects
The water for 4.88 parts by weight of addition carries out dispersion and granulation in 23 minutes with rotor peripheral speed 19m/s (3000rpm), will turn
Sub- peripheral speed is down to 6m/s (900rpm) and is discharged after carrying out 1 point of identical processing in 30 seconds.It will be discharged with 105 DEG C of driers
Granular product dry 4 hours after, the range of 2~4mm of grain size is sized to, to obtain the granular oxamides added with 0.2%PVA.
(evaluation test 1)
About the various granular oxamides obtained in Examples 1 to 6 and comparative example 1~9, to dimensionally stable in hardness, water
Property carry out research and be used as the assessment of slow release nitrogenous fertilizer.These test methods are as described below.It should be noted that record below
In experiment, in obtained granular fertilizer, select grain size in the granular fertilizer of 2.85~3.50mm ranges.
Moisture：The granular oxamides crushed with pulverizer, accurate metering completely by the powder of 0.5mm sieves about
5g is dried 3 hours with 105 DEG C of driers, and the weight divided by example weight of reduction are multiplied by 100.It the results are shown in table 1, table
2, table 3.
Hardness：The particle of 20 granular oxamides is measured using log cabin formula hardometer (Grain Rigidity Tester)
Hardness the results are shown in table 1, table 2, table 3.
Shape stability in water：Into tissue cultures (Mericlone) phial for be put into 50ml water, input 20 is granular
After oxamides, rest in 25 DEG C of thermostat, at the same just plus after water, after 3 days, after 14 days, after 28 days, observation after 56 days
The disintegration state on grain surface.Disintegration state is denoted as 0：Without disintegration；1：10% or less particle surface disintegration；2：Particle surface is disintegrated
11%~30%；3：Particle surface disintegration 31%~50%；4：Particle surface disintegration 51%~70%；5：Particle surface is disintegrated
71%~90%；6：Particle surface disintegration 91%~100%, shown in table 1, table 2, table 3.
[table 1]
The comparison of method of granulating (device)
※0：Without disintegration；1：10% or less particle surface disintegration；2：Particle surface disintegration 11%~30%；3：Particle surface
Disintegration 31%~50%；
4：Particle surface disintegration 51%~70%；5：Particle surface disintegration 71%~90%；6：Particle surface disintegration 91%
~100%
It is as shown in Table 1 as a result, in method using 1~3 facility for granulating of comparative example, fertiliser granulates hardness be 3.1kgf with
Under, in contrast, embodiment 1 is 6.3kgf, and method through the invention can manufacture granular oxamides with high hardness.
Moreover, about shape stability in water, in comparative example 1~3, just plus after water particle surface immediately begins to be disintegrated, 56
Particle surface has been disintegrated 31% or more after it, and in contrast, embodiment 1 also has no disintegration after 56 days.
[table 2]
The vertical granulation for being permitted mixing machine of apsacline love promotes the comparison of material
※0：Without disintegration；1：10% or less particle surface disintegration；2：Particle surface disintegration 11%~30%；3：Particle surface
Disintegration 31%~50%；
4：Particle surface disintegration 51%~70%；5：Particle surface disintegration 71%~90%；6：Particle surface disintegration 91%
~100%
The vertical mixing machine of being permitted of apsacline love will be used to promote the result of material to be shown in table 2 to compare granulation.
The granulation that is not added with of comparative example 4 promotes the fertiliser granulates hardness of material for 3kgf or less.Comparative example 5,6 be 5.3,
4.5kgf is less than embodiment 2.Comparative example 7 is 6.6kgf, little with 2 difference of embodiment.
But about shape stability in water, in comparative example 4, the disintegration of particle surface, but 3 days just plus after water are had no
It is disintegrated later, particle surface has been disintegrated 51% or more after 56 days.Although the hardness of comparative example 5,6,7 is higher than comparative example 4,
Just plus after water particle surface immediately begins to be disintegrated, and particle surface has been disintegrated 51% or more after 56 days.In contrast, embodiment 2 exists
Also disintegration is had no after 56 days.
[table 3]
The additive amount of PVA or modified PVA compares
※0：Without disintegration；1：10% or less particle surface disintegration；2：Particle surface disintegration 11%~30%；3：Particle surface
Disintegration 31%~50%；
4：Particle surface disintegration 51%~70%；5：Particle surface disintegration 71%~90%；6：Particle surface disintegration 91%
~100%
It is as shown in table 3 as a result, the comparative example 8,9 that PVA or modified PVA additive amount are 0.2%, fertiliser granulates hardness are
2.8kgf, about shape stability in water, also just plus after water, immediately visible arrive is disintegrated.In contrast, PVA or modified PVA addition
Amount is 0.5% or more Examples 1 to 6, and hardness is 4.5kgf or more, and shape stability is also high in water.
As described above, method through the invention, it can manufacture that hardness is high, especially not easy disintegrating and dimensionally stable in water
The high granular oxamides of property.
(evaluation test 2：Inorganization experiment under the conditions of 25 DEG C, paddy field)
(1) purpose
To use apsacline love it is vertical permitted mixing machine manufacture added with 1% modified PVA granular oxamides (embodiment 1) and make
With apsacline love it is vertical permitted that mixing machine manufactures added with mineral, ferric sulfate, phosphoric acid granular oxamides (comparative example 7) in paddy field condition
Under inorganization discussed.
(2) test method
In the 60g dry ground [building wave paddy field soil (sandy loam)] (Japan) mixing for examination fertiliser granulates containing oxamides (4,
It is equivalent to nitrogen 24mg), it is put into 200ml beakers.In addition, about phosphoric acid and potassium, using monopotassium phosphate and potassium chloride as at
Point, add 12mg in every 60g dry ground.Then, addition deionized water makes to reach 140% for trying the maximum water holding capacity of soil, with poly-
Vinyl film covers, and then stands the stipulated time in 25 DEG C of constant heat storage.
After the stipulated time, oscillation filtering is carried out to the sample in beaker using 10% potassium chloride solution of 300ml,
By Kang Wei (Conway) methods to inorganic nitrogen (NH4With NO3Total amount) quantified, calculate inorganic rate.
(3) result
Show the result in table 4 and Fig. 2.
[table 4]
<Inorganic rate (%)>
By table 4 and Fig. 2 it is found that liking the vertical granular oxamides added with 1% modified PVA for being permitted mixing machine manufacture using apsacline
With use apsacline love it is vertical permitted mixing machine manufacture added with mineral, ferric sulfate, phosphoric acid granular oxamides compared with, it is inorganization slow,
Play slow release fertilizer efficiency.
Show：The granular oxamides added with 1% modified PVA of the present invention likes that vertical mixing machine of being permitted manufactures with using apsacline
The granular oxamides added with mineral, ferric sulfate, phosphoric acid compare, although nonhomogeneous hardness is little, shape stability is high in water, hair
Shoot slow release fertilizer efficiency.
The comparison of (embodiment 7) Granulation time
The oxamides powder of 20 parts by weight is put into the vertical mixing machine perhaps of apsacline love, and (Japan's love is vertical to be permitted Co. Ltd. system
Make, intensive mixer R02 types) mixing pan container in after, it is molten to add the modified PVA 10% for preparing in 2 parts by weight of example 1
Liquid is mixed 1 minute with rotor peripheral speed 6m/s (900rpm).Then the water for adding 3.20 parts by weight, with rotor peripheral speed
19m/s (3000rpm) carries out dispersion and granulation in 5 minutes, 10 minutes or 15 minutes, and rotor peripheral speed is down to 6m/s
(900rpm) is discharged after carrying out identical processing in 30 seconds.After being dried the granular product of discharge 4 hours with 105 DEG C of driers, survey
Its fixed size distribution.
By the measurement result of size distribution (with the weight divided by total weight under 1mm sieves and on 1mm, 2mm, 4mm sieve
Percentage indicates) it is shown in table 5.
[table 5]
The comparison of Granulation time
(unit：%)
It is as shown in table 5 as a result, when the Granulation time after addition modified PVA and water is 5 minutes and 10 minutes, 2mm~
The granular oxamides of 4mm is less, and in contrast, when carrying out granulation in 15 minutes, the granular oxamides of obtained 2mm~4mm is
50% or more.
Claims (3)
1. a kind of manufacturing method of granular oxamides, which is characterized in that by containing relative to 100 parts by weight of oxamides powder
The mixture of more than 0.5 parts by weight polyvinyl alcohol or modified polyvinylalcohol high-speed stirring mixing in the mixing pan container of apsacline
Grain, is then dried.
2. manufacturing method according to claim 1, wherein carry out High Shear Mixer Granulator, institute using high-speed stirring mixer
Stating high-speed stirring mixer includes：The mixing pan of rotation, configuration are on the position for deviateing the mixing pan center and independent
The blend tool that is rotated in mixing pan, be fixedly arranged on the mixing pan inside scraper plate.
3. manufacturing method according to claim 2, wherein the height after addition polyvinyl alcohol or modified polyvinylalcohol and water
The time of speed stirring granulation is 13~60 minutes.
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2017059558 | 2017-03-24 | ||
| JP2017-059558 | 2017-03-24 | ||
| JP2017-186199 | 2017-09-27 | ||
| JP2017186199A JP6671327B2 (en) | 2017-03-24 | 2017-09-27 | Method for producing granular oxamide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108623333A true CN108623333A (en) | 2018-10-09 |
Family
ID=63705913
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711224786.5A Pending CN108623333A (en) | 2017-03-24 | 2017-11-29 | The manufacturing method of granular oxamides |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112961008A (en) * | 2021-02-25 | 2021-06-15 | 中国科学院合肥物质科学研究院 | Preparation method of low-water-solubility nitrogenous coating material and prepared nitrogenous coating material |
| EP4006003A1 (en) * | 2020-11-26 | 2022-06-01 | Everris International B.V. | Controlled release potassium chloride fertilizer |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0370532A2 (en) * | 1988-11-25 | 1990-05-30 | Ube Industries, Ltd. | Slow release oxamide fertilizer |
| JP4406328B2 (en) * | 2004-07-07 | 2010-01-27 | Ｊｆｅミネラル株式会社 | Granulating treatment method of granulated blast furnace slag |
| WO2013035106A1 (en) * | 2011-09-07 | 2013-03-14 | Indo Gulf Fertilizers | A process for manufacturing a composite fertilizer |
-
2017
- 2017-11-29 CN CN201711224786.5A patent/CN108623333A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0370532A2 (en) * | 1988-11-25 | 1990-05-30 | Ube Industries, Ltd. | Slow release oxamide fertilizer |
| JP4406328B2 (en) * | 2004-07-07 | 2010-01-27 | Ｊｆｅミネラル株式会社 | Granulating treatment method of granulated blast furnace slag |
| WO2013035106A1 (en) * | 2011-09-07 | 2013-03-14 | Indo Gulf Fertilizers | A process for manufacturing a composite fertilizer |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP4006003A1 (en) * | 2020-11-26 | 2022-06-01 | Everris International B.V. | Controlled release potassium chloride fertilizer |
| WO2022112512A1 (en) * | 2020-11-26 | 2022-06-02 | Everris International B.V. | Controlled release potassium chloride fertilizer |
| CN112961008A (en) * | 2021-02-25 | 2021-06-15 | 中国科学院合肥物质科学研究院 | Preparation method of low-water-solubility nitrogenous coating material and prepared nitrogenous coating material |
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