Contain loose compound fertilizer of loosening agent and preparation method thereof
The present invention relates to a kind of agricultural mineral manure and preparation method thereof, dense loose compound fertilizer of particularly a kind of polynary height and preparation method thereof.The composite fertilizer that this free-running property is good is made up of multicomponent composite fertilizer and powdery inner additive.
The development of advancing by leaps and bounds along with chemical fertilizer industry, the dense composite fertilizer of polynary height has become the main developing direction of mineral manure with compound fertilizer, but in the production process of composite fertilizer with in storage period, there are defectives such as easy moisture absorption, the easy adhesion of fertiliser granulates, easy efflorescence, thereby become the technical barrier of essential solution.
Since nineteen seventies so far, a series of employing compounded oil external parcel technology are arisen at the historic moment; Handle composite fertilizer by the employing oil of the nineties France scholar L. nanowatt Si Kusi (Chinese patent 95 118864,1996) invention, the melts of wax class, product grain intensity is low, and the atomizing defective also is not resolved; By Finland T. A Ennasi (Chinese patent 96 198625.5,1998) find: the treatment technology that in mineral oil, fuses into dibasic amino acid salt composite fertilizer, though composite fertilizer is obtained satisfied moistureproof preventing blocking effect, but adopt raw material production cost height, produce the use inconvenience, adopt a large amount of solvents dangerous again, so be difficult to practical application; By water-soluble " peanut " fertilizer additive of Spain's invention, because this invention is the sticky state of milkiness, packing, transportation are all inconvenient; Chinese patent (the patent number of accepting 01129002.1), the technology of forefathers Finland T. A Ennasi is developed and improved to the contriver, adopt inexpensive carboxylic acid and amine, under 90 ℃ of melting process temperature, reaction has generated the amides of effective control compound fertilizer from caking and dust formation tendency, and it is compound that low HLD value, laminar oleophylic shape fluffy powder and oils are made in this invention, external parcel agent as composite fertilizer, effect is more remarkable in reality is now used, and consumption is few, can obviously improve the anti-anti-caking of composite fertilizer.But in actual applications, still exist to need adopt oils and melting unit, exist facility investment big, account for place, wayward, the more high disadvantage of production cost of technology; And find again: the composite fertilizer that adopts the external parcel technology to obtain since the outer coated of its particle one deck oil film, goods are water-soluble to be reduced significantly, can not satisfy the requirement of southern area peasant household; In addition, solid sheet fluffy powder also is difficult to and powdery easily lump material (ammonium nitrate, urea, vitriolate of tartar etc.) uniform mixing thereby automatic gauge enforcement continuously in adopting during adding technology.Therefore, how to substitute forefathers' multiple oily external parcel technology, become current composite fertilizer preventing blocking technology field technical barrier anxious to be solved.
The objective of the invention is to overcome the deficiency of technical background, design provides a kind of preparation method who obtains loose compound fertilizer without composite fertilizer's external parcel technology, and necessary design is a kind of and composite fertilizer's component thermal compatibility is good, raw material sources abundant, processed powders shape fluffy powder with low cost, easy, without the compounded oil compatibility, directly use as inner additive, make the composite fertilizer of good free-running property and energy long storage in composite fertilizer's production process.
The present invention design: in the loose compound fertilizer of design is formed, add by additive compounds such as antisticking agent, brilliant control agent make performance complement, with low cost, can solve the easily polynary Powdered fluffy powder system of caking, adhesion, dust formation defective of composite fertilizer.When adding material in being intended to do, not only in production process, can feed intake with composite fertilizer's synchronous continuous measurement of each component raw material, and can compatiblely with composite fertilizer mix, spray granulating technology by composite fertilizer, form the anti-caking of the protection against the tide granulin molecule model of an even duplex grain structure, effectively composite fertilizer is played effects such as antiblocking, anti-water, control crystal conversion.At the physical property and the crystalline structure of composite fertilizer's principal constituent, this powdery inner additive must by antisticking agent, brilliant control agent, lubricant, anti-looseness agent, non-blushing thinner and fire retardant is composite be formed.Non-blushing thinner such as polyester mainly plays moisture-proof role in the composition, stops the intrusion of ambient moisture; Lubricant plays auxiliary antiblocking function, and improves the outward appearance commodity and the fragility of goods: anti-looseness agent prevents that mainly fertilizer is in the easy atomizing tendency of lay up period; The effect of fire retardant is that itself has high heat capacity, is difficult to ignite, and can improve the security of composite fertilizer's system at whitewashing high temperature granulation process.Wherein anion surfactant brilliant control agent and cats product antisticking agent are the most key; The main effect of brilliant control agent is in composite fertilizer near the easily brilliant transformation temperature that becomes material such as ammonium nitrate, the irreversible change or the slow variation of control crystalline form, and ammonium nitrate has the satisfactory stability crystal formation in the composite fertilizer to keep; The cats product antisticking agent, it acts on based on following mechanism: antisticking agent is scattered in the composite fertilizer, because antisticking agent is held migration performance, so can move to the composite fertilizer surface, greatly reduce coefficient of interal friction, improved sliding and resistance to blocking between compound fertilizer granules, thereby the composite fertilizer that the present invention is made, be difficult for adhesion in regulation in storage period, keep good free-running property.
According to above-mentioned design, the polynary powdery fluffy powder system of a constituent element performance complement of design; The antisticking agent that plays the antiblocking effect must be the cats product of the transportable property of amides tool: the crystalline substance control agent that plays the brilliant control effect of main body must adopt contain polar group-COOH ,-SO
4H ,-SO
3H ,-PO
4The plane configuration anion surfactant of H; Non-blushing thinner adopts the easy film forming material of low melting point, and this class material is ethyl cellulose, polyester etc.; Lubricant generally is the powdery or the thick material that can reduce frictional coefficient, and this class material is: talcum powder, clorafin, stearyl alcohol, Vaseline, naphthenic acid etc.: anti-looseness agent generally is primary amine salt or nonionic surface active agent; Fire retardant adopts high heat capacity maybe can generate the organic or inorganic material of non-combustible gas, and this class material is: vitriolate of tartar, ammonium chloride, colloid magnesium hydride, decabromodiphynly oxide, triphenylphosphate, ammonium polyphosphate, hexabromocyclododecane etc.
The composition of powdery loosening agent of the present invention (quality %) is:
15~60 brilliant control agent: benzyl naphthalene sulfonic formaldehyde condensation compound or sodium lauryl sulfate or poly alkyl alcohol
Oxygen Vinyl Ether or benzyl naphthalene sodium sulfonate
25~40 antisticking agents: cetylamine acetate or two stearic amide or carboxymethyl cellulose or
Erucicamide
5~15 lubricants: sebacic acid or naphthenic acid or stearic acid or talcum powder
5~15 anti-looseness agents: dialkylamine or 16 primary amine or primary octadecylamine or eicosanoic acid acid amides
4~10 non-blushing thinners: polyester or slack wax or Microcrystalline Wax or ethyl cellulose
1~5 fire retardant: ammonium polyphosphate or ammonium chloride or hexabromocyclododecane or tricarbimide three (2,
The 3-dibromopropyl) ester
Best form (the quality %) of powdery loosening agent of the present invention is:
40 brilliant control agent: benzyl naphthalene sulfonic formaldehyde condensation compound
30 antisticking agents: two stearic amides
10 lubricants: sebacic acid
10 anti-looseness agents: primary octadecylamine
7 non-blushing thinners: slack wax
3 fire retardants: hexabromocyclododecane
Preparation method's design of loose compound fertilizer of the present invention: adopt present composite fertilizer factory producing composite fertilizer by liquor jetting pelletting traditional production-line technique process and equipment, powdery loosening agent of the present invention directly added in the slurry vessel of production process or the neutralizing well melt, under agitation mixed with the composite fertilizer each component, through operations such as spray granulating dryings, can make the good composite fertilizer of free-running property.
According to above-mentioned design: implementing loose compound fertilizer preparation method and step that the present invention designs is: at first automatic gauge adds from the main slip of the composite fertilizer of neutralizing well in slurry vessel, the powdery loosening agent of the present invention that adds metering urea or ammonium nitrate and metering synchronously, it is 0.05%~0.15% of composite fertilizer's quality that additive adds concentration, temperature is generally 90~100 ℃ in the slurry vessel, mix stir about 10~15min, (adopt about 400 ℃ of warm air through the spray granulating drying again, the products discharging temperature is generally 85~90 ℃), goods change the lift vibrosieve over to, cooling, packaging process can make the loose compound fertilizer finished product that packaging temp is about 30~40 ℃.
The present invention compares with modern technologies has following advantage:
1 successfully makes cats product antisticking agent and anion surfactant does brilliant control agent, introduces the powdery loosening agent of composite fertilizer's modification effectively and forms.
2 interior adding technology technology of the present invention have replaced traditional inspergation or multiple oily external parcel technology effectively, need not use mineral oil, do not need again to save factory and occupy the place with compounded oil fusing and atomising unit, reduce the plant produced cost significantly.
3 powdery inner additives of the present invention are applied in the composite fertilizer, and but effect is remarkable less for consumption, and goods are stored six months shatter values more than 90%.
4 keep composite fertilizer that good water-solubility is arranged.
5 when the external parcel technical matters is implemented preparation composite fertilizer, and compounded oil is easy blocking pipe and shower nozzle in pipeline flow process and spray process, and technology is difficult to control, and the inner additive technical matters is stable.
6 powdery inner additives of the present invention are convenient to and the production that feeds intake of the synchronous automatic gauge of composite fertilizer material, use so the present invention more is applicable to continuity explained hereafter composite fertilizer producer.
Embodiment
1 by optimum formula of the present invention (quality %) is:
99.90 multi-component composite fertilizer
0.10 powdery loosening agent
Wherein the powdery loosening agent is implemented by following best form (quality %):
40 brilliant control agent: benzyl naphthalene sulfonic formaldehyde condensation compound
30 antisticking agents: two stearic amides
10 lubricants: sebacic acid
10 anti-looseness agents: primary octadecylamine
7 non-blushing thinners: slack wax
3 fire retardants: hexabromocyclododecane
The manufacturing of powdery loosening agent of the present invention: two stearic amide 300g, benzyl naphthalene sulfonic formaldehyde condensation compound 400g, sebacic acid 100g, hexabromocyclododecane 30g and pulverizing back fineness are crossed primary octadecylamine 100g and the slack wax 70g of 250 μ m sieve more than 80%, add together carry out cold stirring 30~40min in the double-deck double-stranded agitator after, discharging is goods.
Utilize the performance of the efficient compound potassium sulfate fertilizer that the above-mentioned powdery loosening agent of the present invention and composite fertilizer's implementing process obtain, test result is referring to table 1.
Table 1 goods technical feature
Common composite fertilizer goods of the present invention
The performance perameter technical indicator
Six months on-the-spot storages six months of on-the-spot storage
Appearance white particle caking, how pure white dust is, and commodity is good pure white, the smooth particle of particle adhesion white
Moisture content, % 1.60 4.00 1.37 1.40≤2.0
Granule strength, N/ particle 14.00 9.00 17.0 16.0 〉=12
Granularity (1-4.75mm), % 99.5 85.0 99.0 95.0 〉=90
Total nutrient, % 45.30 45.00 45.45 45.30 〉=40
Shatter value, % 100 50 100 92.5 〉=70
2 press following composition (quality %) implements:
99.85 multielement high-efficiency tobacco compound fertilizer
0.15 powdery loosening agent
Wherein the powdery loosening agent is implemented by following composition (quality %):
25 antisticking agents: erucicamide
60 brilliant control agent: sodium lauryl sulfate
5 lubricants: naphthenic acid
5 anti-looseness agents: 16 primary amine
4 non-blushing thinners: polyester
1 fire retardant: ammonium chloride
Manufacturing of the present invention is with reference to embodiment 1.
The performance of the high dense smoke grass composite fertilizer of the free-running property of utilizing the present invention to make (sulfur acid ammonium 30%, monoammonium phosphate 30% etc.), test result is referring to table 2.
Table 2 goods technical feature
Common composite fertilizer goods of the present invention
The performance perameter technical indicator
Six months on-the-spot storages six months of on-the-spot storage
Appearance white particle caking is seriously pure white, and free-running property is good pure white, the adhesion white particle
Moisture content, % 1.80 3.60 1.64 1.40≤2.0
Granule strength, N/ particle 30 27.0 42 40 〉=12
Granularity (1-4.75mm), % 99.0 86.0 99.0 98.0 〉=90
Total nutrient content, % 52.0 50.0 51.4 51.2 〉=50
Shatter value, % 100 40 100 90.5 〉=70
3 press following composition (quality %) implements:
99.95 multi-element tobacco compound fertilizer
0.05 powdery loosening agent
Wherein the powdery inner additive is implemented by following composition (quality %):
15 brilliant control agent: fatty alcohol-polyoxyethylene ether
40 antisticking agents: cetylamine acetate
15 lubricants: stearic acid
15 anti-looseness agents: eicosanoic acid acid amides
10 non-blushing thinners: Microcrystalline Wax
5 fire retardants: ammonium polyphosphate
Manufacturing of the present invention is with reference to embodiment 1.
Utilize the water soluble characteristic of the multi-element tobacco composite fertilizer (containing ammonium nitrate 20%, ammonium chloride 22.5%) that the present invention makes, test result is referring to table 3.
Table 3 goods water soluble characteristic
Water-soluble, index,
Example classification sample name data source
Min (leaving standstill in the water) min
Comparative example does not have agent ammonium nitrate base composite fertilizer control sample 3.5≤10
The composite fertilizer document CNP96 198625.5 30.0≤10 of reference example external parcel compounded oil
The fertile control sample 22.0≤10 of the compound of reference example external parcel compounded oil
Embodiment 1 free-running property S-based compound fertilizer goods 4.5≤10 of the present invention
Embodiment 2 free-running property tobacco compound fertilizers goods 5.0≤10 of the present invention
The fertile goods 4.0≤10 of the present invention of embodiment 3 free-running property tobacco compounds
4 adopt thermal analyzer to goods of the present invention, have carried out differential scanning calorimetric analysis (TGA-DTA method), have studied the thermolysis collection of illustrative plates of goods of the present invention, and test result is referring to table 4.
Table 4 goods thermal decomposition performance
Fusing point, initial heat decomposition temperature, final heat decomposition temperature,
Example classification sample name data source
℃ T0,℃ T1,℃
Comparative example does not have agent composite fertilizer control sample 70.00 147.50 513.80
Reference example contains composite fertilizer's control sample 70.75 147.92 520.36 of external parcel oil
Embodiment 1 free-running property S-based compound fertilizer goods 79.60 149.0 544.60 of the present invention
Embodiment 2 free-running property tobacco compound fertilizers goods 72.75 148.9 548.73 of the present invention
Embodiment 3 free-running property tobacco compound fertilizers goods 84.50 225.0 538.20 of the present invention
As seen from Table 4: goods of the present invention composite fertilizer, than the excellent heat resistance of forefathers goods, the heat decomposition temperature that contains the composite fertilizer of loosening agent of the present invention all is higher than the technological temperature of making composite fertilizer's spray granulating, so production use safety.