CN101602631A - Contain free-running property explosion proof ammonium nitrate for agricultural of water-soluble detonation suppressor and preparation method thereof - Google Patents
Contain free-running property explosion proof ammonium nitrate for agricultural of water-soluble detonation suppressor and preparation method thereof Download PDFInfo
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- CN101602631A CN101602631A CNA2009101579504A CN200910157950A CN101602631A CN 101602631 A CN101602631 A CN 101602631A CN A2009101579504 A CNA2009101579504 A CN A2009101579504A CN 200910157950 A CN200910157950 A CN 200910157950A CN 101602631 A CN101602631 A CN 101602631A
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Abstract
The invention provides a kind of free-running property explosion proof ammonium nitrate for agricultural and preparation method thereof.It is characterized in that: this explosion-proof ammonium nitrate contains water-soluble powdery detonation suppressor.Be in order to solve the modification of ammonium nitrate detonation suppressor of forefathers development, exist in actual use unsolved water-soluble bad, ammonium nitrate easily separates from mixture, detonation suppressor easily stops up technological deficiencies such as prilling spry, explosion-proof effect is poor, goods easily harden in storage period in the production.The water-soluble detonation suppressor that the present invention adds is made up of Explosion suppressant, fire retardant, anti-brilliant agent, heat-resistant agent and impermeable dose etc. of becoming.The continuous granulation of rotary nozzle this detonation suppressor and molten state ammonium nitrate mother liquor added in the tempering tank before the prilling spry synchronously puddles evenly, after can make the explosion-proof ammonium nitrate of tool free-running property, anti-knocking property and irreducibility.The present invention also can be used as effective detonation suppressor of powder crystallization modification of ammonium nitrate.
Description
Technical field
The present invention relates to a kind of explosion proof ammonium nitrate for agricultural and preparation method thereof, belong to modification of ammonium nitrate, particularly a kind of explosion-proof ammonium nitrate that is applicable to preparation tool free-running property, anti-knocking property and irreducibility and preparation method thereof.This modification explosion-proof ammonium nitrate is made up of ammonium nitrate and water-soluble detonation suppressor.
Background technology
Ammonium nitrate (AN) all has epochmaking effect on industrial and agricultural production and national defence, it is a kind of instant nitrogenousfertilizer, it is again the important source material of preparation multicharge, very easily be processed into " native explosive " privately, seriously bring unsafe factor to society, in order to stop from the source with the private illegal activities of frying explosive of ammonium nitrate, guarantee agricultural ammonium nitrate transportation safety and social stability, Chinese Government has issued No. 52 files of State Council in 2002, to the ammonium nitrate stringent regulations, forbid ammonium nitrate is sold as agrochemical.Simultaneously,, allow modification of ammonium nitrate is handled, make it to lose explosive as agrochemical sale and use owing to the market requirement of some farm crop to nitrate fertilizer.
In order to solve the technical need of modification of ammonium nitrate or passivation, since the sixties in 20th century, the countries in the world scientific and technical personnel have carried out a large amount of research work to modification of ammonium nitrate: at first every Western Europe country succeeds in developing calcium ammonium nitrate improving the breed as ammonium nitrate, but owing to reasons such as production technology and production units, this method of modifying is not applied; Then United States Patent (USP) 3366468 is reported in and adds 10% above ammonium hydrogen phosphate (MAP) in the ammonium nitrate or primary ammonium phosphate (DAP) is made fire retardant, and reduces ammonium nitrate nitrogen content in agricultural fertilizer, thereby the explosivity of reduction ammonium nitrate fertilizer; During 2002～2003, Chinese patent 02156254.7,03117530.9, report has been developed various detonation suppressors, adopts and United States Patent (USP) 366468 similar techniques approach, promptly adopts physics blending MAP and inertia breeze to come passivation ammonium nitrate; Subsequently, Chinese Northcentral University comes passivation ammonium nitrate with single component material such as magnesium basic carbonates, has improved forefathers' explosion-proof effect.But above-mentioned so far various detonation suppressor research is explored, and does not all obtain industrialness and produces in batches and use.Have mainly that detonation suppressor adds that consumption is big, detonation suppressor water-soluble bad, ammonium nitrate easily separates from mixture, produce in detonation suppressor easily stop up technological deficiencies such as prilling spry, explosion-proof effect is poor, goods easily harden in storage period.Face the anti-terrorism and the domestic multiple fertile market requirement, further study the passivating technique and the effective detonation suppressor of ammonium nitrate, become technical barrier anxious to be solved.
Summary of the invention
The objective of the invention is to overcome above-mentioned existing disadvantages of background technology, design a kind of preparation method that the preparation explosion proof ammonium nitrate for agricultural is provided, and must design abundant, with low cost, the water-soluble powdery detonation suppressor of a kind of raw material sources, this detonation suppressor can be in granulation ammonium nitrate or ammonium nitrate crystals production process be used as effective passivator, makes the explosion-proof ammonium nitrate that good free-running property was arranged in tool anti-knocking property, unreducible and storage period.
The present invention design: in the explosion-proof ammonium nitrate of design is formed, be added into a constituent element performance complement, can overcome the polynary composite anti-explosion agent system of above-mentioned background technical deficiency.Being intended to make concentration is in 98.5%～99.0% the molten state ammonium nitrate and the tempering tank of detonation suppressor before prilling spry, by melt compounding, shower nozzle granulation, to obtain the ammonium nitrate granulin molecule model of a kind of even mixed crystal and dense structure.For this reason, this explosion-proof ammonium nitrate passivator must become agent, fire retardant, heat-resistant agent, impermeable dose and Explosion suppressant is formed by anti-brilliant.Fire retardant in the composition is based on " heat absorption-filling " insensitiveness theory in the HOT SPOT INITIATION OF EXPLOSIVES mechanism, and main rising stops igniting, and the effect that stops focus to generate and transmit, and reduces the ignition rate of ammonium nitrate-fuel oil system; The effect of heat-resistant agent is thermotolerance and the heat decomposition temperature that improves detonation suppressor, guarantees the security of production use; Impermeable dose is the explosion-proof coating that easily generates barrier film with ammonium nitrate, its action principle is: in the granulating of producing ammonium nitrate, drying process, this impermeable dose can bond and be wrapped in the ammonium nitrate particle surface, form protectiveness impermeabilisation film, effectively combustible agent diesel oil is separated with the oxygenant ammonium nitrate particle, reduce diesel oil level of interpenetration in ammonium nitrate, thereby, intercepted the generation of blast from having stoped the source that produces blast by redox reaction in essence; The wherein anti-brilliant design that becomes agent and Explosion suppressant is the most key: anti-ly brilliantly become agent and adopted in group and the ammonium nitrate molecule ammonium ion similar anion surfactant on structure and profile, this group is attached on the ammonium nitrate molecule interface, play the irreversible change of control ammonium nitrate crystalline form and the effect of slow variation, to keep goods that stable crystalline form is arranged, thereby goods of the present invention keep good free-running property be difficult for adhesion, non-sclerous, difficult brilliant the change in storage period; The Explosion suppressant of most critical, forming physics mixed crystal double salt structure more than 90 ℃ with ammonium nitrate, granule strength, hardness and the density of ammonium nitrate have been improved, thereby the propagation of prevention detonation wave in ammonium nitrate-fuel oil mixture, hinder the chain reaction of detonation process, the blast that has caused is suppressed at once and decays or extinguish.
According to above-mentioned design: the polynary composite powder detonation suppressor system of a constituent element performance complement of design, fire retardant is selected the organic or inorganic functionalization fire retardant material of high specific heat, difficult to burn for use, and this class material is: halowax, clorafin, ammonium chloride, aluminium hydroxide, magnesium hydroxide, decabromodiphynly oxide, inorganic phosphate, hexabromocyclododecane, triphenylphosphate, organonitrogen heterocyclic compound cyanogen etc.; Heat-resistant agent is selected the high organic diffusant of heat decomposition temperature for use, generally adopts the sulfonate of Nai Gaore, band naphthalene nucleus; The impermeable dose of anti-hydrocarbon material that must adopt the natural or synthetic polymer of lower molecular weight water-soluble, that be insoluble to hydrocarbons, this class material is: agar, gelatin, polyvinyl alcohol, treated starch, polyvinyl butyral acetal, chitosan, sodium hydroxyethlcellulose, polyethers, poly carboxylic acid fat etc.; Anti-brilliant change agent employing polar functionalities-COOH ,-SO
4H ,-SO
3H ,-PO
4The plane configuration anion surfactant of H; Explosion suppressant adopts and generates the mineral sulfates that heat is big, lattice energy is big, soluble in water, inexpensive, and this class material is vitriolate of tartar, sodium sulfate, zinc sulfate, sal epsom, ammonium sulfate, Tai-Ace S 150 etc.
Explosion proof ammonium nitrate for agricultural of the present invention, its component by quality % is:
Ammonium nitrate 95.0～98.0
Detonation suppressor 2～5
Wherein composite anti-explosion agent component by quality % is:
50～90 Explosion suppressants: Tai-Ace S 150 or sodium sulfate or ammonium sulfate or vitriolate of tartar
3～20 fire retardants: potassium primary phosphate or aluminium hydroxide or cyanuric acid or decabromodiphynly oxide
3～10 anti-brilliant agent that become: sodium lignosulfonate or Sodium Lauryl Sulphate BP/USP or sodium metnylene bis-naphthalene sulfonate or butylbenzene sodium sulfonate
2～10 heat-resistant agents: methylene radical benzyl naphthalene sodium sulfonate or dispersing agent MF or dispersion agent S or benzyl naphthalene sulfonic formaldehyde condensation compound
2～10 impermeable doses: polyvinyl butyral acetal or treated starch or agar or polyvinyl alcohol
The best of explosion proof ammonium nitrate for agricultural of the present invention is formed:
97 ammonium nitrate
3 detonation suppressors
Wherein the composite anti-explosion agent by quality % is best the composition:
75 Explosion suppressants: Tai-Ace S 150;
10 fire retardants: potassium primary phosphate;
The 5 anti-brilliant agent that become: sodium lignosulfonate;
5 heat-resistant agents: methylene radical benzyl naphthalene sodium sulfonate;
5 impermeable doses: polyvinyl butyral acetal.
The preparation method of explosion-proof ammonium nitrate of the present invention design: the production technique and the equipment that adopt the shower nozzle granulation of present ammonium nitrate factory, the continuous granulation of rotary nozzle water-soluble powdery detonation suppressor and molten state ammonium nitrate mother liquor added in the tempering tank before the prilling spry synchronously puddles evenly, after can make the explosion-proof ammonium nitrate of tool free-running property, anti-knocking property and irreducibility.
According to above-mentioned design, explosion-proof ammonium nitrate preparation method and the step implementing the present invention and design are: at first with in powdery detonation suppressor that measures and the tempering tank that measures before the molten state ammonium nitrate mother liquor adds prilling spry synchronously, it is 2%～5% of ammonium nitrate quality that detonation suppressor adds concentration, molten state ammonium nitrate mother liquor concentration is 98.5%～99.0% in the tempering tank, temperature is generally at 168 ℃-173 ℃ in the tempering tank, the separator vacuum degree control is 0.075MPa-0.085MPa, after mixing about 4-6min, with the 10t/h--12t/h flow, make explosion-proof ammonium nitrate through the continuous granulation of rotary nozzle, goods enter quantitative package machine through feed belt and pack and put in storage the stacking storage.
The present invention compared with prior art has following advantage:
The passivation antiknock that multinomial passivating technique-flame-retarded technology, anti-brilliant change technology, cladding insensitiveness technology and eutectic technological synthesis is used for ammonium nitrate of 1 success of the present invention, thereby the present invention makes the serial powder type explosive of ammonium oil lose blast performance fully effectively, reliably.
2 groups of in one's duty pulverulent water-soluble detonation suppressors, detonation suppressor easily stops up the prilling spry phenomenon in not only having avoided producing, and the present invention is difficult for separating from mixture, promptly has an irreducibility;
3 groups of in one's duty anti-brilliant agent that become were stored the explosion-proof ammonium nitrate goods that made by the present invention six months, did not lump, and non-sclerous, its shatter value is more than 95%.
Detonation suppressor consumption among 4 the present invention adds consumption than forefathers and lacks, and but effect is obvious, produces safe and convenient to usely, and low production cost is easy to promote.
Embodiment
Embodiment
1 presses following optimum formula (quality %) implements:
97 ammonium nitrate
3 detonation suppressors
Wherein the composite anti-explosion agent is implemented by following best form (quality %):
75 Explosion suppressants: Tai-Ace S 150
10 fire retardants: potassium primary phosphate
The 5 anti-brilliant agent that become: sodium lignosulfonate
5 heat-resistant agents: methylene radical benzyl naphthalene sodium sulfonate
5 impermeable doses: polyvinyl butyral acetal
1.1 the preparation of detonation suppressor: at first 5kg methylene radical benzyl naphthalene sodium sulfonate is dried by the fire 4h in 90-100 ℃ baking oven, and 10kg potassium primary phosphate and 75kg Tai-Ace S 150 are pulverized in rotating speed is the ball mill of 40r/min respectively, fineness needed more than the 425 μ m80%; Handle qualified raw materials with above-mentioned three kinds then and add together in the stirrer of double-layer spiral structure with 5kg sodium lignosulfonate and 5kg polyvinyl butyral acetal, puddle 30～40min after, product is promptly made in discharging.
1.2 preparation of the present invention: at first in the tempering tank of high tower prilling production ammonium nitrate production line, (mother liquid concentration is 98.5%～99.0% to inject metering molten state ammonium nitrate mother liquor, temperature is generally at 168 ℃-173 ℃ in the tempering tank), the powdery detonation suppressor that in tempering tank, adds metering by reinforced belt, the separator vacuum degree control is 0.075MPa-0.085MPa, after mixing about 4-6min, opening tempering tank all falls to drench, with 10t/h--12t/h granulation flow, make the granular explosion-proof ammonium nitrate of the about 1～2mm of diameter through the continuous granulation of rotary nozzle.
The explosion-proof granulation ammonium nitrate of the free-running property of the present invention of utilizing above-mentioned preparation method to make, outward appearance is pure white, and free-running property is good, and it is constant to store after six months the product appearance physical condition after testing, shatter value is 96.5%, contrasts referring to 1 with the goods shatter value that does not contain detonation suppressor of the present invention.
Table 1 goods shatter value in storage period
2 press following composition (quality %) implements:
95 ammonium nitrate
5 detonation suppressors
Wherein the composite anti-explosion agent is implemented by following composition (quality %):
90 Explosion suppressants: sodium sulfate
3 fire retardants: aluminium hydroxide
The 3 anti-brilliant agent that become: Sodium Lauryl Sulphate BP/USP
2 heat-resistant agents: dispersing agent MF
2 impermeable doses: treated starch
The present invention makes with reference to embodiment 1.
Utilize the present invention, be applied to the manufacturing of No. 2 ammonium nitrate-fuel oil mixtures: utilize the explosion-proof ammonium nitrate of free-running property of the present invention, after ball mill is pulverized, be heated to 70 ℃, oxygenant as No. 2 ammonium nitrate-fuel oil mixtures, with combustible agent diesel oil, the wood powder of metering, in ball grinder or on the continuous flow tube method production line, heat is mixed and is made uniform No. 2 ammonium nitrate-fuel oil mixtures.According to Chinese industry standard " WJ9050--2006 agricultural ammonium nitrate capability of antidetonance test method and judgement ", the capability of antidetonance of this ammonium nitrate-fuel oil mixture is detected.
By the check of following regulation condition for surveys and method contain goods of the present invention the capability of antidetonance: with the ammonium nitrate-fuel oil mixture sample for preparing, be 0.85～0.90g/cm according to packing density
3Scope, the diameter of packing into is that 80mm, pipe range are in the irony sample hose of 160mm, makes powder stick, an end seals with kraft liner, the other end is uncovered; After the general steel plate base is placed the level ground, support is placed on the base, the thicker witness plate of carbon structure steel 1mm is lain on the support, and powder stick is placed on witness plate central authorities, uses blasting cap initiation.Criterion regulation: three verification experimental verification plates all do not puncture or tear, and then the capability of antidetonance is qualified.The capability of antidetonance of this ammonium nitrate-fuel oil mixture is carried out detected result, referring to table 2.
Table 2 capability of antidetonance detected result
As seen from Table 2: No. 2 ammonium nitrate-fuel oil mixtures by the present invention makes reach capability of antidetonance requirement.
3 press following composition (quality %) implements:
98 ammonium nitrate
2 detonation suppressors
Wherein the composite anti-explosion agent is implemented by following composition (quality %):
50 Explosion suppressants: ammonium sulfate
20 fire retardants: cyanuric acid
The 10 anti-brilliant agent that become: sodium metnylene bis-naphthalene sulfonate
10 heat-resistant agents: dispersion agent S
10 impermeable doses: agar
Manufacturing of the present invention is with reference to embodiment 1.
Adopt Q600 type differential scanning calorimetric--thermogravimetric analysis linkage analysis (DSC--TGA method), studied the kinetics of thermal decomposition of goods of the present invention, the heat decomposition temperature detected result is referring to table 3.
Table 3 DSC--TGA test-results
As seen from Table 3: it is hot that goods of the present invention have an anti-height than forefathers goods, and so the technological temperature (168～173 ℃) during the initial heat decomposition temperature of goods of the present invention high production granulation ammonium nitrate far away particularly is production use safety.
4 press following composition (quality %) implements:
96 ammonium nitrate
4 detonation suppressors
Wherein the composite anti-explosion agent is implemented by following composition (quality %):
65 Explosion suppressants: vitriolate of tartar
15 fire retardants: decabromodiphynly oxide
The 8 anti-brilliant agent that become: butylbenzene sodium sulfonate
6 heat-resistant agents: benzyl naphthalene sulfonic formaldehyde condensation compound
6 impermeable doses: polyvinyl alcohol
The preparation of detonation suppressor is with reference to embodiment 1 among the present invention.
Utilize the present invention form in water-soluble powdery detonation suppressor, be applied to the manufacturing of the explosion-proof ammonium nitrate crystals of free-running property: the negative pressure inhaled concentration is 90%～92% the about 400Kg of ammonium nitrate mother liquor in crystallizer, add metering 1.6Kg powdery detonation suppressor simultaneously, under agitation be warming up to 120 ℃, heat of stirring mixes about 2～3min in machine, rapid vacuumizing should reach more than vacuum tightness 〉=0.07MPa vacuum-drying 5～6min in 1min; Back vacuum breaker, under agitation discharging; Goods are carried by belt, and through the helical feed refrigerating unit, through material turning and heat exchange heat radiation, goods can make loose explosion-proof ammonium nitrate crystals in packing below 70 ℃.
The explosion-proof crystallization ammonium nitrate of the free-running property of utilizing above-mentioned manufacture method to make, outward appearance is pure white, and free-running property is good, storing six months shatter values is 95.6%, and do not add the common ammonium nitrate crystals of powdery detonation suppressor among the present invention, be commonly called as into " plate nitre ", storing six months goods shatter values is 20%.
Equally, utilize that the powdery detonation suppressor makes loose explosion-proof ammonium nitrate crystals among the present invention, with reference to embodiment 2 and 3 technologies and testing method, detected result shows: the capability of antidetonance of the ammonium nitrate-fuel oil mixture that is made by the explosion-proof knot ammonium nitrate of free-running property meets industry standard " WJ9050-2006 " requirement.
Claims (2)
1 one kinds lose volatile free-running property explosion proof ammonium nitrate for agricultural fully and are made up of ammonium nitrate and composite anti-explosion agent, it is characterized in that: directly adopting on granulation ammonium nitrate production line concentration is in 98.5%～99.0% the molten state ammonium nitrate mother liquor, after adding metering pulverulent water-soluble detonation suppressor heat is mixed and spares, make the granular explosion-proof ammonium nitrate of free-running property through the continuous granulation of rotary nozzle, its component by quality % is:
Ammonium nitrate 95.0～98.0
Detonation suppressor 2～5
Wherein the component of composite anti-explosion agent by quality % is:
50～90 Explosion suppressants: Tai-Ace S 150 or sodium sulfate or ammonium sulfate or vitriolate of tartar
3～20 fire retardants: potassium primary phosphate or aluminium hydroxide or cyanuric acid or decabromodiphynly oxide
3～10 anti-brilliant agent that become: sodium lignosulfonate or Sodium Lauryl Sulphate BP/USP or sodium metnylene bis-naphthalene sulfonate or butylbenzene sodium sulfonate
2～10 heat-resistant agents: methylene radical benzyl naphthalene sodium sulfonate or dispersing agent MF or dispersion agent S or benzyl naphthalene sulfonic formaldehyde condensation compound
2～10 impermeable doses: polyvinyl butyral acetal or treated starch or agar or polyvinyl alcohol.
2 free-running property explosion proof ammonium nitrate for agricultural according to claim 1 is characterized in that its component by quality % is:
97 ammonium nitrate
3 detonation suppressors
Wherein the component of composite anti-explosion agent by quality % is:
75 Explosion suppressants: Tai-Ace S 150;
10 fire retardants: potassium primary phosphate;
The 5 anti-brilliant agent that become: sodium lignosulfonate;
5 heat-resistant agents: methylene radical benzyl naphthalene sodium sulfonate;
5 impermeable doses: polyvinyl butyral acetal.
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| CN102557761A (en) * | 2012-02-29 | 2012-07-11 | 山西同德化工股份有限公司 | Inorganic explosion-proof agent and agricultural explosion-proof ammonium nitrate prepared by inorganic explosion-proof agent |
| CN102875267A (en) * | 2012-10-11 | 2013-01-16 | 石家庄成功机电有限公司 | Explosive mixed loading truck, powdery ammonium nitrate fuel oil explosive for explosive mixed loading truck and method for preparing powdery ammonium nitrate fuel oil explosive |
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| CN102557761A (en) * | 2012-02-29 | 2012-07-11 | 山西同德化工股份有限公司 | Inorganic explosion-proof agent and agricultural explosion-proof ammonium nitrate prepared by inorganic explosion-proof agent |
| CN102875267A (en) * | 2012-10-11 | 2013-01-16 | 石家庄成功机电有限公司 | Explosive mixed loading truck, powdery ammonium nitrate fuel oil explosive for explosive mixed loading truck and method for preparing powdery ammonium nitrate fuel oil explosive |
| CN102875267B (en) * | 2012-10-11 | 2016-06-15 | 石家庄成功机电有限公司 | Blasting agent mixing vehicle, powdered ammonium nitrate-fuel oil explosive and preparation method thereof for blasting agent mixing vehicle |
| CN105848732A (en) * | 2013-11-12 | 2016-08-10 | 美铝公司 | Fertilizer compositions and methods of making and using the same |
| CN105848732B (en) * | 2013-11-12 | 2021-03-09 | 美铝美国公司 | Fertilizer compositions and methods of making and using the same |
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| CN104446988B (en) * | 2014-12-03 | 2017-05-31 | 山东省农业科学院农业资源与环境研究所 | A kind of Special foliage fertilizer for wheat using retired disability single-base powder and preparation method thereof |
| CN104788174A (en) * | 2015-03-25 | 2015-07-22 | 殷海权 | High-strength and high-stability agricultural anti-explosive ammonium nitrate and preparation method thereof |
| CN105622252A (en) * | 2015-05-22 | 2016-06-01 | 成都市新都化工股份有限公司 | Phosphorus nitrate compound fertilizer containing explosion-proof agent and preparation method for compound fertilizer |
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Effective date of registration: 20190415 Address after: 710000 Unit 401, Unit 3, 29/F, No. 5, East Zhangba Road, Yanta District, Xi'an City, Shaanxi Province Co-patentee after: Anhui Haixiang New Material Technology Co., Ltd. Patentee after: Yin Haiquan Address before: 710065 Unit 401, Unit 3, Building 29, 83 Zhangba East Road, Yanta District, Xi'an City, Shaanxi Province Patentee before: Yin Haiquan |