CN102320885B - Spherical magnesium nitrate and tower granulation method thereof - Google Patents
Spherical magnesium nitrate and tower granulation method thereof Download PDFInfo
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- CN102320885B CN102320885B CN 201110235752 CN201110235752A CN102320885B CN 102320885 B CN102320885 B CN 102320885B CN 201110235752 CN201110235752 CN 201110235752 CN 201110235752 A CN201110235752 A CN 201110235752A CN 102320885 B CN102320885 B CN 102320885B
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Abstract
The invention discloses a spherical magnesium nitrate and a tower granulation method thereof, relates to nitrate manufacture technology and solves problems of weak flowing property, long manufacturing period and high energy consumption of prior granular magnesium nitrate. The spherical magnesium nitrate has a spherical or near spherical shape, smooth surface, semitransparent appearance, a magnesium nitrate hexahydrate content higher than 98.0% and a particle size of 1.0-6.0mm. The preparation steps comprise that a concentrated magnesium nitrate solution at 95-100 DEG C is transferred to an insulation storage tank at the top of a granulation tower and sprayed out through a nozzle to form near spherical liquid drops under surface tension; the liquid drops contact with upward flowing air to be cooled gradually and solidified into near spherical solid particles, which are treated with a surface treatment and packaged to obtain a finished product. The product of the invention has advantages of high hardness, good flowing property and no caking; and the tower granulation technology is at low energy consumption and suitable for continuous large batch production.
Description
Technical field
The present invention relates to the nitrate manufacturing technology, be specifically related to a kind of spherical magnesium nitrate and high tower prilling method thereof.
Background technology
The prilling process of inorganic salt is a lot, but high tower prilling is one of most important method in numerous methods, except ammonium nitrate, saltpetre, urea and other compound fertilizer granulatings successfully adopt the high tower prilling manufacturing, the inorganic salt that contain crystal water adopt this method difficulty bigger, are not applied for a long time and develop
Existing magnesium nitrate product is the granular product that contains six crystal water mostly; this magnesium nitrate in use free-running property is poor; manufacturing process is to adopt interrupter method; need through long crystallisation by cooling, separation; production cycle is long, and energy consumption and comprehensive cost are higher, in addition; a spot of free moisture content is contained on the crystal grain surface, in the phenomenon of transporting and storage process lumps through regular meeting's generation.
Chinese patent CN1762923 discloses a kind of melt slime granulating composite fertilizer and manufacture method thereof, be with mixtures such as urea, Repone K or vitriolate of tartar, ammonium phosphate, weighting agents, adopt high-temperature fusion urea to do carrier, raw material is merged evenly, again through cat head spray cooling granulating.Chinese patent CN1935748 discloses the method that basic granular composite fertilizer is urinated in a kind of high tower prilling production, comprise slurrying, granulation, described slurrying is the pulping method of progressively lowering the temperature continuously of connecting in three steps, may further comprise the steps: in the fusion groove, add fusing assistant and urea, will flow into first step tempering tank behind the urea watery fusion; In first step tempering tank, in the fused urea soln, add not the raw material with its reaction, the molten materials that obtains after mixing is flowed in the tempering tank of the second stage; In the tempering tank of the second stage, add monoammonium phosphate, mix the time less than 4 minutes with melts, obtain the mixed melting slip; The double speed rotating granulation shower nozzle of mixed melting slip by high tower sprays to enter finishes granulation in the prilling tower.Chinese patent CN201346454 discloses a kind of high tower melt pelletization production unit that comprises refrigerating unit.And relevant spherical magnesium nitrate and high tower prilling method domestic and foreign literature do not appear in the newspapers.
Summary of the invention
The present invention is poor for the free-running property that solves existing particulate state magnesium nitrate existence, and the manufacturing process cycle is long, the problem that energy consumption is high, and a kind of spherical magnesium nitrate and high tower prilling method thereof are provided.
The present invention is achieved by the following technical solutions:
A kind of spherical magnesium nitrate, profile are spherical or subsphaeroidal, smooth surface, the outward appearance state that is translucent, and the quality percentage composition of magnesium nitrate hexahydrate is greater than 98.0%, and particle diameter is 1.0mm-6.0mm.
The high tower prilling method of described spherical magnesium nitrate may further comprise the steps:
(1) solution is equipped with: the outfit mass concentration is the magnesium nitrate solution more than 50%, then solution is transported to the insulation storage tank at prilling tower top, and the temperature of maintenance solution is between 95～100 ℃;
(2) granulation: with the magnesium nitrate solution of temperature between 95～100 ℃ is the shower nozzle ejection of 0.5～5.0mm from the aperture, under capillary effect, form spherical or subsphaeroidal drop, drop is the air generation thermal exchange of 0.1～0.3m/s with the speed of upwards carrying in dropping process, cooled and solidified globulate or subglobose solid particulate, wherein the distance of fall of drop is 10～60 meters;
(3) surface treatment: it is that the acetone soln of 1～10% paraffin carries out surface treatment that the solid particles surface behind the granulating and forming is sprayed one deck mass concentration, gets product.
Further, described surface treatment method can be that the solid particles surface sprinkling one deck mass concentration behind granulating and forming is 1～5% the spirituous solution that contains tensio-active agent, and described tensio-active agent is octadecane amine, cetylamine or tetradecylamine.
Spherical granules of magnesium nitrate of product of the present invention and existing crystallization granules of magnesium nitrate were deposited 30 days under 50% humidity and 30 ℃ of environment respectively, and caking phenomenon does not take place in the former, and the latter is lumpd seriously.After tested, the power that the crushing of the simple grain of the spherical granules of magnesium nitrate of the present invention needs is 50-100N, and the crushing force of crystalloid granules of magnesium nitrate simple grain is 10-30N.
The present invention compared with prior art has the following advantages:
(1) spherical magnesium nitrate magnesium nitrate, profile is closely spherical, and Diaspora Performance is good more than the magnesium nitrate that crystallization processes obtains, for the use of product brings a lot of facilities;
(2) high tower prilling is than crystallization processes low cost of manufacture, also is fit to serialization and produces in enormous quantities, to the automatization of the technology controlling and process condition of providing convenience;
(3) the spherical magnesium nitrate of the present invention is not easy to break in aftertreatment or transportation than the product particle hardness height of additive method production.
Description of drawings
Fig. 1 is the technological process block diagram of the high tower prilling method of a kind of spherical magnesium nitrate of the present invention.
Embodiment
Embodiment 1
A kind of spherical magnesium nitrate, profile are spherical or subsphaeroidal, smooth surface, the outward appearance state that is translucent, and the quality percentage composition of magnesium nitrate hexahydrate is greater than 98.0%, and particle diameter is 1.0mm～6.0mm, prepares according to following steps:
Adopting content is that 40% nitric acid is raw material greater than 90% magnesium oxide and mass concentration, earlier nitric acid is joined in the reactor, under whipped state, magnesium oxide is progressively added, the PH of regulator solution is built in 5.0～6.0, continue stirring reaction after 1 hour, filter the removal mechanical impurity, solution is sent into vaporizer, and to be concentrated to magnesium nitrate content be 50%; Then magnesium nitrate solution is transported to while hot the insulation storage tank at the top of prilling tower, the temperature that keeps solution is between 95～100 ℃; Be that granulation is carried out in the shower nozzle ejection of 2mm with magnesium nitrate solution by injection diameter then, tower height is 30 meters, and the air movement speed of upwards carrying in the tower is 0.2m/s; The granules of magnesium nitrate diameter that obtains through granulation is substantially in the 1.0-6.0mm scope, and median size is 3.8, and the average spherical rate of goods is greater than 95%.
Spherical granules of magnesium nitrate adopted the acetone soln of 1% paraffin carry out surface treatment at course of conveying, the content of paraffin is no more than 0.1% in the finished product that obtain, and does not lump in 30 days after measured, and the power that the simple grain crushing of spheroidal particle needs is 60-100N.
Embodiment 2-11
Adopt with embodiment 1 same process process and method to prepare spherical magnesium nitrate, only change part processing parameter and granulation condition, processing condition and the product performance comparing result such as the following table 1 that obtain.
Table 1 embodiment 2-10 main technique condition and result
| Embodiment | Tower height/m | Air movement speed/(m/s) | Injection diameter/the mm of shower nozzle | Mg(NO 3) 2.6H 2O content/% | Finished product median size/mm | Particle pressure break intensity/N | The time of not luming/sky |
| 2 | 30 | 0.1 | 3.0 | 99.0 | 3.8 | >50 | >30 |
| 3 | 30 | 0.2 | 3.0 | 99.0 | 4.0 | >50 | >30 |
| 4 | 10 | 0.3 | 3.0 | 98.0 | 4.0 | >50 | >30 |
| 5 | 60 | 0.2 | 3.0 | 99.0 | 3.8 | >50 | >30 |
| 6 | 40 | 0.2 | 3.0 | 99.0 | 3.8 | >50 | >30 |
| 7 | 50 | 0.2 | 0.5 | 99.0 | 1.2 | >50 | >30 |
| 8 | 40 | 0.2 | 1.0 | 99.0 | 1.8 | >50 | >30 |
| 9 | 20 | 0.2 | 2.0 | 99.0 | 2.5 | >50 | >30 |
| 10 | 40 | 0.2 | 4.0 | 99.0 | 4.4 | >50 | >30 |
| 11 | 40 | 0.2 | 5.0 | 99.0 | 5.6 | >50 | >30 |
Embodiment 12
Employing is carried out high tower prilling with the processing parameter of embodiment 1, in spherical magnesium nitrate product collection and course of conveying, 5% the acetone soln that sprays into paraffin continuously carries out surface treatment, paraffinicity is less than 0.2% in the product that obtains at last, the Diaspora Performance of product is significantly improved, and the non-caking time was increased to more than 3 months.
Embodiment 13-21
Adopt the surface treatment method identical that the spherical magnesium nitrate product that high tower prilling obtains is carried out surface treatment, change concentration, composition, the solvent species of surface treatment agent respectively, treatment effect such as following table 2 with embodiment 12.
Table 2 embodiment 13-21 significant parameter and result
| Embodiment | The surface treatment agent kind | Solvent species | Surface treatment agent concentration/% | Surface treatment agent content/% in the finished product | The time of not luming/sky |
| 13 | Paraffin | Acetone | 2 | <0.2 | 〉60 |
| 14 | Paraffin | Acetone | 3 | <0.2 | 〉90 |
| 15 | Paraffin | Acetone | 8 | <0.2 | 〉90 |
| 16 | Paraffin | Acetone | 10 | <0.2 | 〉90 |
| 17 | Octadecane amine | Alcohol | 1 | <0.2 | 〉90 |
| 18 | Octadecane amine | Alcohol | 1 | <0.2 | 〉90 |
| 19 | Cetylamine | Alcohol | 2 | <0.2 | 〉120 |
| 20 | Tetradecylamine | Alcohol | 3 | <0.2 | 〉180 |
| 21 | Tetradecylamine | Alcohol | 5 | <0.2 | 〉90 |
Claims (2)
1. spherical magnesium nitrate is characterized in that profile is spherical or subsphaeroidal, smooth surface, the outward appearance state that is translucent, and the quality percentage composition of magnesium nitrate hexahydrate is greater than 98.0%, and particle diameter is 1.0mm-6.0mm;
Use the high tower prilling method during preparation, may further comprise the steps:
(1) solution is equipped with: the outfit mass concentration is the magnesium nitrate solution more than 50%, then solution is transported to the insulation storage tank at prilling tower top, and the temperature of maintenance solution is between 95～100 ℃;
(2) granulation: with the magnesium nitrate solution of temperature between 95～100 ℃ is the shower nozzle ejection of 0.5～5.0mm from the aperture, under capillary effect, form spherical or subsphaeroidal drop, drop is the air generation thermal exchange of 0.1～0.3m/s with the speed of upwards carrying in dropping process, cooled and solidified globulate or subglobose solid particulate, wherein the distance of fall of drop is 10～60 meters;
(3) surface treatment: it is that the acetone soln of 1～10% paraffin carries out surface treatment that the solid particles surface behind the granulating and forming is sprayed one deck mass concentration, promptly get profile for spherical or subsphaeroidal, smooth surface, the outward appearance state that is translucent, the quality percentage composition of magnesium nitrate hexahydrate is greater than 98.0%, and particle diameter is the spherical magnesium nitrate of 1.0mm-6.0mm.
2. the high tower prilling method of spherical magnesium nitrate according to claim 1, it is characterized in that described surface treatment method can be solid particles surface behind granulating and forming to spray one deck mass concentration be 1～5% the spirituous solution that contains tensio-active agent, described tensio-active agent is octadecane amine, cetylamine or tetradecylamine.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103833444B (en) * | 2014-03-14 | 2016-03-23 | 交城县金兰化工有限公司 | Nitrocalcite magnesium double salt type composite fertilizer and preparation method thereof |
| CN103979586A (en) * | 2014-06-05 | 2014-08-13 | 王静 | Magnesium nitrate, magnesium nitrate granulation equipment and magnesium nitrate production process |
| CN106268483A (en) * | 2016-08-29 | 2017-01-04 | 河南心连心化肥有限公司 | The preparation facilities of a kind of compound fertilizer mixed slurry and preparation method |
| CN107602160A (en) * | 2017-10-24 | 2018-01-19 | 交城县金兰化工有限公司 | A kind of tower granulation method of low melting point fused salt |
| CN110092699A (en) * | 2018-01-30 | 2019-08-06 | 徐州市禾协肥业有限公司 | A kind of high intensity fertiliser granulates |
| CN109133994A (en) * | 2018-08-29 | 2019-01-04 | 交城县金兰化工有限公司 | Spherical calcium nitrate and its tower granulation method |
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| CN1280972A (en) * | 1999-12-29 | 2001-01-24 | 化学工业部上海化工研究院 | process for preparing high-concentration granular composite N-K fertilizer |
| CN1741844A (en) * | 2002-11-26 | 2006-03-01 | 奥姆尼亚肥料有限公司 | Apparatus for producing nitrate granules |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1280972A (en) * | 1999-12-29 | 2001-01-24 | 化学工业部上海化工研究院 | process for preparing high-concentration granular composite N-K fertilizer |
| CN1741844A (en) * | 2002-11-26 | 2006-03-01 | 奥姆尼亚肥料有限公司 | Apparatus for producing nitrate granules |
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Address after: 030500 Yiwang Industrial Zone, Jiaocheng County, Luliang City, Shanxi Province Patentee after: Shanxi Jinlan Chemical Co., Ltd. Address before: 030500 Yiwang Industrial Zone, Jiaocheng County, Luliang City, Shanxi Province Patentee before: Jiaocheng Knlan Chemical Co., Ltd. |