CN110668847B - Production method of large-particle magnesium nitrate - Google Patents
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- CN110668847B CN110668847B CN201911067219.2A CN201911067219A CN110668847B CN 110668847 B CN110668847 B CN 110668847B CN 201911067219 A CN201911067219 A CN 201911067219A CN 110668847 B CN110668847 B CN 110668847B
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C5/00—Fertilisers containing other nitrates
- C05C5/005—Post-treatment
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- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
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Abstract
The invention discloses a production method of large-particle magnesium nitrate, which comprises the following steps: 1) diluting nitric acid with desalted water; 2) after the measurement, the magnesium nitrate and the magnesium oxide which are added into a stock bin in advance are controlled, the magnesium nitrate and the magnesium oxide are simultaneously added into a magnesium nitrate reaction tank according to a proportion, and dilute nitric acid and the magnesium oxide are quickly and fully reacted under a stirring state; 3) removing impurities by filter pressing of a filter press; 4) concentrating the low-concentration magnesium nitrate clear solution by a first-stage evaporator of an ammonium nitrate device; 5) magnesium nitrate solution is pumped into a primary mixing tank of a nitrocompound fertilizer granulation tower, is fully stirred with returned materials screened by a system and overflows into a secondary mixing tank; 6) and the second-stage mixing tank enters a mechanical rotary granulator through overflow, then spraying granulation is carried out, and the lower tower particles enter a packaging system after being subjected to cooling rotary drum and screen screening treatment to obtain magnesium nitrate particles. The invention solves the blank of the production of large-particle magnesium nitrate in China at present and improves the operating rate of the nitro compound fertilizer high tower device.
Description
Technical Field
The invention relates to a production process of magnesium nitrate, belongs to the technical field of fertilizer production, and particularly relates to a method for producing large-particle magnesium nitrate by using a high tower device for co-producing ammonium nitrate and nitro compound fertilizer.
Background
Because the current high tower device for coproducing the ammonium nitrate and the nitro-compound fertilizer has low operating rate, the average operating rate throughout the year is about 30 percent in China, and the productivity is extremely compressed. Therefore, if the device can be used for producing other products, the products are diversified, and the defect can be compensated.
At present, magnesium nitrate produced in China can generate a large amount of high-content ammonia nitrogen wastewater in the concentration process, and the wastewater is directly discharged into a sewage station for treatment, so that the load on the sewage treatment station is large, and the treatment and the discharge requirements are difficult to meet.
According to the research of Chinese plant nutrition and fertilizer science, about 21 percent of soil in China has magnesium deficiency and obvious deficiency, and 54 percent of soil needs to be supplemented with magnesium-containing fertilizer in different degrees. For a long time, with the large input of nitrogen, phosphorus and potassium fertilizers, the improvement of the crop multiple cropping index and the application of new varieties, the crop yield and biomass are continuously improved. The magnesium carried away from the soil by the crops is increased continuously, and the phenomenon of magnesium deficiency of the plants continuously appears in different areas and on different crops, thereby influencing the yield of the plants.
Chinese patent CN102320885B discloses a method for producing spherical magnesium nitrate. The production method is characterized in that a granulation tower with the tower height of 60m is used for production, and the particle size of the produced product is smaller than 1 mm. Because the average particle size of the fertilizer product is smaller, the contact area between the fertilizer product and soil and the atmosphere is increased, the process of accelerating the interaction between the fertilizer product and the soil can promote the fixation and loss of the fertilizer product by the soil, the absorption rate is reduced, and the fertilizer product is easy to absorb moisture, agglomerate or deliquesce.
In order to improve the situation, large-particle magnesium nitrate needs to be produced, and no research report on the production of the large-particle magnesium nitrate by a high-tower device exists so far.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a production method of large-particle magnesium nitrate, which is used for producing the large-particle magnesium nitrate by utilizing a high tower device for co-producing the nitro-compound fertilizer by using ammonium nitrate, so as to solve the blank of producing the large-particle magnesium nitrate at present in China, solve the problem that waste water generated in the concentration process of the magnesium nitrate is difficult to treat, better improve the operating rate of the high tower device for the nitro-compound fertilizer and promote the utilization rate of the magnesium fertilizer to be improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a production method of large-particle magnesium nitrate, which comprises the following steps:
1) diluting nitric acid with desalted water;
2) after the metering, the magnesium nitrate and the magnesium oxide which is added into a stock bin in advance are simultaneously added into a magnesium nitrate reaction tank in proportion by controlling the magnesium nitrate reaction tank and the magnesium oxide to carry out rapid and sufficient reaction under the stirring state;
3) removing impurities by filter pressing of a filter press;
4) concentrating the low-concentration magnesium nitrate clear solution by a first-stage evaporator of an ammonium nitrate device;
5) magnesium nitrate solution is pumped into a primary mixing tank of a nitrocompound fertilizer granulation tower, is fully stirred with returned materials screened by a system, and overflows into a secondary mixing tank;
6) and the second-stage mixing tank enters a mechanical rotary granulator through overflow, then is sprayed for granulation, and the lower tower particles enter a packaging system after being subjected to cooling drum and screen screening treatment to obtain magnesium nitrate particles.
Further, in step 1), dilute nitric acid at 58% was diluted with desalted water to 38% concentration.
Further, in step 2), the metering is metered by a flowmeter; the magnesium oxide is light-burned magnesium oxide; the control of the simultaneous addition of the two in proportion is carried out by using a variable frequency screw; the proportion is as follows according to mole ratio, nitric acid: the magnesium oxide is 2: 1; the reaction of dilute nitric acid and magnesium oxide is completed when the pH value of the final solution is 5.5-6.
Further, in step 3), the filter press is a two-stage filter press.
Further, in the step 4), the concentration is carried out to obtain magnesium nitrate with the content of 58.5-60%.
Further, the step 4) comprises the step of returning the high ammonia nitrogen-containing wastewater generated by concentration to a circulating water pool for secondary utilization after electrodialysis treatment of an ammonium nitrate device.
Further, in the step 5), a magnesium nitrate solution is pumped into a primary mixing tank of a nitro compound fertilizer granulation tower to use a melting pump; the viscosity of the feed liquid is controlled by the added returning material.
Further, in the step 6), the final granulation temperature is controlled to 90-95 ℃, the rotation speed of the granulator is controlled to be 15-17HZ for inward rotation, and 20-21HZ for outward rotation; the screen is a drum screen with the aperture of 3-4 mm.
The invention provides a tower device for producing large-particle magnesium nitrate by utilizing ammonium nitrate and nitro-compound fertilizer co-production, which is prepared by the production method, wherein the particle size of magnesium nitrate particles is 3-4 mm.
Furthermore, the particle size of the magnesium nitrate particles with the particle size of 3-4mm is not less than 95%, and the strength is 45-60N.
Compared with the prior art, the invention has the following beneficial effects:
1) the magnesium nitrate granules produced by the method have the grain size of 3-4mm, belong to large granules, can slow down the process of interaction between the magnesium nitrate granules and soil, can reduce the fixation and loss of the magnesium nitrate granules by the soil, and promote the absorption rate of the magnesium nitrate.
2) The high tower device for producing the large-particle magnesium nitrate by utilizing the ammonium nitrate and the co-produced nitro compound fertilizer creates the precedent of China, so that the device can be fully utilized to improve the operating rate of enterprises, the diversification of products produced by the device can be realized, the production requirement can be met without adding large investment, the multiple purposes of one tower are realized, and the energy conservation and the consumption reduction are realized.
3) The method can well solve the problem of wastewater treatment generated in the concentration process of magnesium nitrate, and return the qualified treated water into the circulating water for secondary utilization, thereby achieving the effects of energy conservation and consumption reduction.
Drawings
FIG. 1 is a flow diagram of a process for producing large-particle magnesium nitrate according to the present invention;
FIG. 2 is a schematic diagram of the configuration of a high tower apparatus required for the production of large particle magnesium nitrate according to the present invention;
the reference numbers in the figures are as follows:
1: a nitro compound fertilizer prilling tower; 2: a first-stage mixing tank; 3: a secondary mixing tank; 4: a rotary granulator;
FIG. 3 is a flow chart of the method and the equipment for producing large-particle magnesium nitrate.
Detailed Description
The invention discloses a production method of large-particle magnesium nitrate, which is carried out by adopting a high tower device for co-producing nitro compound fertilizer by ammonium nitrate, wherein the equipment flow of the method comprises a storage bin, a magnesium nitrate reaction tank, a filter press, an ammonium nitrate device, an evaporator, a nitro compound fertilizer granulation tower 1 and a primary mixing tank 2; a secondary mixing tank 3, a rotary granulator 4 (fig. 2), a screen and a packaging system.
In addition, as shown in fig. 1-3, the method for producing large-particle magnesium nitrate by using the high tower device for co-producing ammonium nitrate and nitro compound fertilizer comprises the following steps:
1) diluting 58% dilute nitric acid with desalted water to 38% concentration;
2) after metering by a flowmeter, the light-burned magnesia and the light-burned magnesia are fed into a storage bin in advance and are controlled by a frequency conversion screw, and the light-burned magnesia are mixed according to a molar ratio of nitric acid: the magnesium oxide is 2: 1, simultaneously adding the mixed solution into a magnesium nitrate reaction tank, and quickly and fully reacting dilute nitric acid and magnesium oxide under the stirring state, wherein the final reaction end point is when the pH value of the solution is 5.5-6;
3) removing impurities by pressure filtration through a two-stage filter press;
4) concentrating the low-concentration magnesium nitrate clear solution by a first-stage evaporator of an ammonium nitrate device to ensure that the content of magnesium nitrate is 58.5-60%, and returning the high-ammonia nitrogen-containing wastewater generated by concentration to a circulating water tank for secondary utilization after electrodialysis treatment of the ammonium nitrate device;
5) pumping 58.5-60% magnesium nitrate solution into a primary mixing tank 2 of a nitro compound fertilizer granulation tower 1 through a melting pump, fully stirring the magnesium nitrate solution with returned materials screened by a system, overflowing the magnesium nitrate solution into a secondary mixing tank 3, and controlling the viscosity of the feed liquid through the added returned materials;
6) and the secondary mixing tank 3 enters a mechanical rotary granulator 4 through overflow, the final granulation temperature is controlled to 90-95 ℃, the rotation speed of the granulator 4 is controlled to be 15-17HZ in inward rotation and 20-21HZ in outward rotation, then spraying granulation is carried out, the lower tower particles enter a packaging system after being screened by a cooling rotary drum and a rotary screen with the screen mesh aperture of 3-4mm, and the magnesium nitrate particles with uniform, white and bright particles are obtained.
The method provided by the invention has the advantages that the waste water generated in the magnesium nitrate concentration process is subjected to electrodialysis treatment by the ammonium nitrate device, and the qualified water after treatment is returned into the circulating water for secondary utilization, so that the effects of energy conservation and consumption reduction are achieved.
The present invention will be described in more detail below with reference to specific preferred embodiments and drawings, but the present invention is not limited to the following embodiments.
Example 1
A production method of large-particle magnesium nitrate comprises the following steps:
1) diluting 58% dilute nitric acid to 38% concentration with desalted water, metering by a flowmeter, and controlling with light-burned magnesium oxide added into a stock bin in advance by a frequency conversion spiral, wherein the dilute nitric acid and the light-burned magnesium oxide are nitric acid: magnesium oxide ═ 2: 1, simultaneously adding the mixed solution into a magnesium nitrate reaction tank, and quickly and fully reacting dilute nitric acid and magnesium oxide under the stirring state, wherein the final reaction end point is when the pH value of the solution is 5.5-6;
2) then, after impurities are removed through filter pressing of a two-stage filter press, low-concentration magnesium nitrate clear liquid is concentrated through a first-stage evaporator of an ammonium nitrate device to enable the content of magnesium nitrate to be 58.5-60%, high ammonia nitrogen-containing wastewater generated through concentration is returned to a circulating water tank for secondary utilization after electrodialysis treatment of the ammonium nitrate device, 58.5-60% of magnesium nitrate solution is pumped into a mixing tank of a nitro compound fertilizer granulation tower through a melting pump, is fully stirred with returned materials screened by a system and overflows into a secondary tank, and the viscosity of the feed liquid is controlled through the added returned materials;
3) and the secondary tank enters a mechanical rotary granulator through overflow, the final granulation temperature is controlled to 90-95 ℃, the rotation speed of the granulator is controlled to be 16HZ inward rotation and 20HZ outward rotation, then spraying granulation is carried out, the lower tower particles are subjected to screening treatment by a cooling rotary drum and a rotary screen with the screen mesh aperture of 3-4mm and then enter a packaging system, and the magnesium nitrate particles with uniform and bright white particles are obtained.
The magnesium nitrate granules prepared by the embodiment of the invention have the granularity of 3-4mm accounting for 95 percent and the strength of 58N, the detailed indexes are shown in the attached table, the stacking height of the fertilizer is 20 layers, and the magnesium nitrate granules are loose, free of agglomeration and pulverized within 6 months.
Example 2
A production method of large-particle magnesium nitrate comprises the following steps:
1) diluting 58% dilute nitric acid to 38% concentration with desalted water, metering by a flowmeter, and controlling with light-burned magnesium oxide added into a stock bin in advance by a frequency conversion spiral, wherein the dilute nitric acid and the light-burned magnesium oxide are nitric acid: magnesium oxide ═ 2: 1, simultaneously adding the mixed solution into a magnesium nitrate reaction tank, and quickly and fully reacting dilute nitric acid and magnesium oxide under the stirring state, wherein the final reaction end point is when the pH value of the solution is 5.5-6;
2) then, after impurities are removed through filter pressing of a two-stage filter press, low-concentration magnesium nitrate clear liquid is concentrated through a first-stage evaporator of an ammonium nitrate device to enable the content of magnesium nitrate to be 58.5-60%, high ammonia nitrogen-containing wastewater generated through concentration is returned to a circulating water tank for secondary utilization after electrodialysis treatment of the ammonium nitrate device, 58.5-60% of magnesium nitrate solution is pumped into a mixing tank of a nitro compound fertilizer granulation tower through a melting pump, is fully stirred with returned materials screened by a system and overflows into a secondary tank, and the viscosity of the feed liquid is controlled through the added returned materials;
3) and the secondary tank enters a mechanical rotary granulator through overflow, the final granulation temperature is controlled to 90-95 ℃, the rotation speed of the granulator is controlled to be 16HZ inward rotation and 20HZ outward rotation, then spraying granulation is carried out, the lower tower particles are subjected to screening treatment by a cooling rotary drum and a rotary screen with the screen mesh aperture of 3-4mm and then enter a packaging system, and the magnesium nitrate particles with uniform and bright white particles are obtained.
The magnesium nitrate granules prepared by the embodiment of the invention have the granularity of 3-4mm accounting for 95 percent, the strength of 58N, the detailed indexes are shown in the attached table, the stacking height of the fertilizer is 20 layers, and the magnesium nitrate granules are loose, free from agglomeration and pulverized within 6 months.
Comparative example 1
A production method of magnesium nitrate comprises the following steps:
1) diluting 58% dilute nitric acid to 38% concentration with desalted water, metering by a flowmeter, and controlling with light-burned magnesium oxide added into a stock bin in advance by a frequency conversion spiral, wherein the magnesium oxide and the light-burned magnesium oxide are respectively 2: 1, simultaneously adding the mixed solution into a magnesium nitrate reaction tank, and quickly and fully reacting dilute nitric acid and magnesium oxide under the stirring state, wherein the final reaction end point is when the pH value of the solution is 5.5-6;
2) then, after impurities are removed through filter pressing of a two-stage filter press, low-concentration magnesium nitrate clear liquid is concentrated through a first-stage evaporator of an ammonium nitrate device to enable the content of magnesium nitrate to be 57-58%, high ammonia nitrogen-containing wastewater generated through concentration is returned to a circulating water tank for secondary utilization after electrodialysis treatment of the ammonium nitrate device, 57-58% magnesium nitrate solution is pumped into a first mixing tank of a nitro-compound fertilizer granulation tower through a melting pump, is fully stirred with returned materials under system screening and then overflows into a second-stage tank, and the viscosity of feed liquid is controlled through the added returned materials;
3) and the secondary tank enters a mechanical rotary granulator through overflow, the final granulation temperature is controlled to 90-95 ℃, the rotation speed of the granulator is controlled to be 17HZ in the inner rotation mode and 21HZ in the outer rotation mode, then spraying granulation is carried out, and the lower tower particles enter a packaging system after being screened by a cooling rotary drum and a rotary screen with the screen mesh diameter of 2-4 mm.
The prepared magnesium nitrate granules have more broken granules and flat granules, the adhesion to a tower is serious in the production process, the strength is only 20N, two layers of stacked fertilizers have serious hardening phenomenon, and the production requirement cannot be met.
Comparative example 2
A production method of magnesium nitrate comprises the following steps:
1) diluting 58% dilute nitric acid to 38% concentration with desalted water, metering by a flowmeter, and controlling with light-burned magnesium oxide added into a stock bin in advance by a frequency conversion spiral, wherein the magnesium oxide and the light-burned magnesium oxide are respectively 2: 1, simultaneously adding the mixed solution into a magnesium nitrate reaction tank, and quickly and fully reacting dilute nitric acid and magnesium oxide under the stirring state, wherein the final reaction end point is when the pH value of the solution is 5.5-6;
2) then, after impurities are removed through filter pressing of a two-stage filter press, low-concentration magnesium nitrate clear liquid is concentrated through a first-stage evaporator of an ammonium nitrate device, the content of magnesium nitrate is more than or equal to 60%, high ammonia nitrogen-containing wastewater generated by concentration returns to a circulating water tank for secondary utilization after electrodialysis treatment of the ammonium nitrate device, more than or equal to 60% of magnesium nitrate solution is pumped into a first mixing tank of a nitro compound fertilizer granulation tower through a melting pump, and overflows into a second mixing tank after being fully stirred with returned materials screened by a system, and the viscosity of feed liquid is controlled through the added returned materials;
3) and the secondary tank enters a mechanical rotary granulator through overflow, the final granulation temperature is controlled to 90-95 ℃, the rotation speed of the granulator is controlled to be 15HZ inward rotation and 19HZ outward rotation, then spraying granulation is carried out, and the lower tower particles enter a packaging system after being screened by a cooling rotary drum and a rotary screen with the screen mesh diameter of 2-4 mm.
The prepared magnesium nitrate particles are aggregated and cannot be granulated, and the tower adhesion is serious in the production process, so that the production requirement cannot be met.
Examples of Effect test
The magnesium nitrate granules prepared in the above example 1 were analyzed and detected as shown in the following table 1:
TABLE 1 analysis and detection results of magnesium nitrate granules
The results in table 1 above show that the fertilizer of example 1 according to the invention performs well, is stacked in 20 layers high, and is loose, free of caking and dusting within 6 months.
The present invention is not limited to the above-described embodiments, and various changes and modifications of the present invention are intended to be included within the scope of the claims and the equivalent technology of the present invention if they do not depart from the spirit and scope of the present invention.
Claims (7)
1. The production method of large-particle magnesium nitrate is characterized in that the method utilizes ammonium nitrate to co-produce nitro compound fertilizer in a high tower device, and comprises the following steps:
1) diluting nitric acid with desalted water;
2) after metering, the magnesium nitrate and the magnesium oxide which are added into a stock bin in advance are controlled, the magnesium nitrate and the magnesium oxide are simultaneously added into a magnesium nitrate reaction tank according to a proportion, and dilute nitric acid and the magnesium oxide are quickly and fully reacted under the stirring state;
3) removing impurities by filter pressing of a filter press;
4) concentrating the low-concentration magnesium nitrate clear solution by a first-stage evaporator of an ammonium nitrate device; concentrating to obtain magnesium nitrate with a content of 58.5-60%;
5) magnesium nitrate solution is pumped into a primary mixing tank of a nitrocompound fertilizer granulation tower, is fully stirred with returned materials screened by a system and overflows into a secondary mixing tank;
6) the secondary mixing tank enters a mechanical rotary granulator through overflow, the final granulation temperature is controlled to 90-95 ℃, then spraying granulation is carried out, and the lower tower particles enter a packaging system after being screened by a cooling rotary drum and a screen mesh to obtain magnesium nitrate particles;
the rotating speed of the granulator is controlled to be 15-17HZ in the inner rotation direction and 20-21HZ in the outer rotation direction; the screen is a drum screen with the aperture of 3-4 mm.
2. The production method according to claim 1, characterized in that: in step 1), dilute nitric acid at 58% was diluted to 38% concentration with desalted water.
3. The production method according to claim 1, wherein: in step 2), the measurement is measured by a flowmeter; the magnesium oxide is light-burned magnesium oxide; the control of the simultaneous addition of the two in proportion is carried out by using a variable frequency screw; the proportion is as follows according to mole ratio, nitric acid: the magnesium oxide is 2: 1.
4. the production method according to claim 1, wherein: in the step 2), the reaction of the dilute nitric acid and the magnesium oxide is finished when the pH value of the final solution is 5.5-6.
5. The production method according to claim 1, characterized in that: in the step 3), the filter press is a two-stage filter press.
6. The production method according to claim 1, wherein: and 4) performing electrodialysis treatment on the high ammonia nitrogen-containing wastewater generated by concentration by using an ammonium nitrate device, and returning the high ammonia nitrogen-containing wastewater to a circulating water pool for secondary utilization.
7. The production method according to claim 1, wherein: in the step 5), a magnesium nitrate solution is pumped into a primary mixing tank of a nitro compound fertilizer granulation tower to use a melting pump; the viscosity of the feed liquid is controlled by the added returning material.
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| CN115155493A (en) * | 2022-07-05 | 2022-10-11 | 山西金兰化工股份有限公司 | Continuous magnesium nitrate neutralizing device and preparation process |
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| CN103979586A (en) * | 2014-06-05 | 2014-08-13 | 王静 | Magnesium nitrate, magnesium nitrate granulation equipment and magnesium nitrate production process |
| CN106396915A (en) * | 2016-08-31 | 2017-02-15 | 宜昌富升化工有限公司 | Fully water-soluble nitro-sulfur based composite fertilizer and preparation method thereof |
| CN109265224A (en) * | 2018-11-28 | 2019-01-25 | 四川金象赛瑞化工股份有限公司 | A kind of Special fertilizer for wheat and preparation method thereof |
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| CN104098115B (en) * | 2014-07-22 | 2016-03-30 | 路永宽 | A kind of method utilizing steel band tablets press to produce full water-soluble sheet magnesium nitrate |
| CN104086235B (en) * | 2014-07-22 | 2016-02-24 | 路永宽 | A kind of method utilizing steel band tablets press to produce full water-soluble ammonium nitrate magnesium |
| CN104725098B (en) * | 2015-03-20 | 2017-08-29 | 路永宽 | The method of steel band granulation production full water-soluble ammonium nitrate calcium and magnesium |
| CN104744100B (en) * | 2015-03-20 | 2017-08-11 | 路永宽 | The method that disc granulation produces full water-soluble ammonium nitrate calcium and magnesium |
| CN208776324U (en) * | 2018-09-25 | 2019-04-23 | 天津华景化工新技术开发有限公司 | A kind of production system of bulky grain magnesium nitrate |
| CN109019645B (en) * | 2018-09-25 | 2023-07-14 | 天津华景工程技术有限公司 | Production system and production method of large-particle magnesium nitrate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103979586A (en) * | 2014-06-05 | 2014-08-13 | 王静 | Magnesium nitrate, magnesium nitrate granulation equipment and magnesium nitrate production process |
| CN106396915A (en) * | 2016-08-31 | 2017-02-15 | 宜昌富升化工有限公司 | Fully water-soluble nitro-sulfur based composite fertilizer and preparation method thereof |
| CN109265224A (en) * | 2018-11-28 | 2019-01-25 | 四川金象赛瑞化工股份有限公司 | A kind of Special fertilizer for wheat and preparation method thereof |
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