CN107162843A - The method that hot pickled mustard tube special fertilizer is produced with phosphate ore flotation tailings - Google Patents

Abstract

The invention discloses a method for producing special fertilizer for pickled mustard by using phosphate rock flotation tailings. Calculated by mass, 80-120 parts of phosphate rock flotation tailings, 160-200 parts of phosphate rock powder and 200-250 parts of water After adding into the reactor and mixing well, add 200-250 parts of nitric acid to react for 5-10 minutes, then filter and retain the filtrate, then add 150-180 parts of potassium fertilizer, 130-160 parts of urea, 20-30 parts of ammonium phosphate and 18-18 parts of After 22 parts of activated loosening agent is dissolved, add 170-200 parts of ammonia gas to neutralize to obtain phosphorus fertilizer slurry, and granulate or dry the phosphorus fertilizer slurry to obtain nitrophosphate fertilizer. The present invention decomposes phosphate ore flotation tailings and phosphorus by nitric acid Phosphorus pentoxide, calcium, magnesium oxide, etc. in the mineral powder generate water-soluble phosphoric acid, calcium nitrate, magnesium nitrate, magnesium phosphate, magnesium nitrate, iron nitrate and other soluble components, which are finally retained in the finished product in the form of ions. The method makes full use of all the elements useful for crop growth in the tailings and phosphate rock, and the fertilizer produced has a reasonable ratio of nitrogen, phosphorus and potassium and good porosity, and is very suitable for planting mustard.

Description

Method for producing special fertilizer for pickled mustard from phosphate rock flotation tailings

technical field

The invention relates to the technical field of harmless disposal and resource utilization of industrial solid waste, in particular to a method for producing special fertilizer for pickled mustard by using phosphorite flotation tailings.

Background technique

With the rapid development of the wet-process phosphoric acid industry, the domestic phosphate rock industry has produced a large number of low- and medium-grade flotation phosphate rock tailings. These tailings have been stockpiled for a long time, which not only occupies a large amount of land resources, but also poses safety risks for tailings ponds. Research The resource utilization of these solid industrial wastes is of great significance.

Mustard mustard is a variant of mustard. Mustard is often used to pickle pickles. As a specialty crop in the Fuling area of Chongqing, the planting area is as high as one million mu. Mustard mustard has a large demand for fertilizers, high requirements for base fertilizer, and topdressing in stages during the growth period; therefore, a special fertilizer that can meet the needs of mustard mustard is needed.

Contents of the invention

In order to solve the above technical problems, the present invention provides a method for producing special fertilizer for pickled mustard with simple process from phosphate ore flotation tailings.

The technical scheme is as follows: a method for producing special fertilizer for pickled mustard with phosphate ore flotation tailings, the key of which is to carry out according to the following steps:

Step (1): Add 80-120 parts of phosphate rock flotation tailings, 160-200 parts of phosphate rock powder and 200-250 parts of water into the reactor, mix well and stir evenly, and then add 200- 250 parts of nitric acid, filter after reacting for 5-10 minutes, and keep the filtrate;

Step (2): Add 150-180 parts of potassium fertilizer, 130-160 parts of urea, 20-30 parts of ammonium phosphate and 18-22 parts of activated loosening agent to the filtrate until it is fully dissolved;

Step (3): after dissolving, add 170-200 parts of ammonia gas to carry out neutralization reaction, control the pH value of the material after the reaction to be 5.0-6.0 to obtain phosphorus fertilizer slurry;

Step (4): Concentrating, granulating or drying the phosphate fertilizer slurry to obtain nitrophosphate fertilizer;

Each of the above components is calculated in parts by mass.

Using the above technical scheme, use nitric acid to decompose phosphorus pentoxide, calcium, magnesium oxide, etc. in phosphate rock flotation tailings and phosphate rock powder, and generate phosphoric acid, calcium nitrate, magnesium nitrate, magnesium ammonium phosphate, and magnesium nitrate that are soluble in water Soluble components such as ferric nitrate and iron nitrate are finally retained in the finished product in the form of ions, which are essential elements for crop growth; while the fluorine in the rock phosphate powder is discharged in the form of hydrogen fluoride gas, and the silica is recovered in the form of precipitation after filtration. He said that this method can fully utilize all the elements useful for crop growth in the tailings and phosphate rock, while the traditional method of sulfuric acid decomposition will produce calcium sulfate precipitation, the calcium element is filtered out, and the fertilizer produced lacks crops Calcium is necessary for growth, and other useful elements are not fully utilized.

Preferably: the mass ratio of N:P:K in the nitrophosphate fertilizer is 20:8:10.

Calculated by mass percentage, the activated loosening agent consists of 8-9% organic matter, 0.5% nitrate, 7.5-7.9% sodium dodecylbenzenesulfonate, and 0.3-0.4% sodium dodecylsulfonate , 0.4-0.6% of OP-10, 0.4-0.6% of KCl and the balance of water.

The above organic matter is humic acid or polypeptide. The use of humic acid and peptides in this solution not only has a good effect on improving soil compaction, but also supplements organic fertilizers to crops.

The concentration of above-mentioned nitric acid is 65-68%.

Above-mentioned potassium fertilizer is potassium chloride or potassium nitrate. Using this design, nitric acid decomposes phosphate rock powder to generate a mixed acid of phosphoric acid and nitric acid. The mixed acid reacts with potassium chloride or potassium nitrate to generate potassium dihydrogen phosphate and potassium nitrate, which supplements the potassium element in the fertilizer, and potassium element is also an essential element for crop growth. one.

The granulation method in step (4) is spray granulation; the drying is drying at 100-105°C.

Phosphate rock powder contains 28.91% of phosphorus pentoxide, 5.10% of magnesium oxide, and 0.61% of ferric oxide, among which P, Mg and Fe are finally retained in the fertilizer in the form of ions; phosphate rock flotation tailings There are also 6.06% phosphorus pentoxide, 33.51% calcium oxide, and 17.2% magnesium oxide in the mine, among which P, Ca, and Mg are all retained in the fertilizer in the form of soluble ions, which are essential elements for crop growth.

Beneficial effect: the beneficial effect of adopting the present invention is to decompose phosphorus pentoxide, calcium, magnesium oxide, etc. Ammonium magnesium phosphate, magnesium nitrate, iron nitrate and other soluble components are finally retained in the finished product in the form of ions, while the mixed acid of phosphoric acid and nitric acid will react with potassium chloride or potassium nitrate to form potassium dihydrogen phosphate and potassium nitrate, which can be added to the fertilizer The potassium element used for neutralization is also used as a source of nitrogen fertilizer to supplement the nitrogen element of the fertilizer. This method makes full use of all the elements useful for crop growth in the tailings and phosphate rock, and the fertilizer nitrogen, phosphorus, and potassium The ratio is reasonable, the porosity is good, and it is very suitable for growing mustard.

Description of drawings

Fig. 1 is the loose photo of nitrophosphate fertilizer in embodiment 3;

Fig. 2 is a photograph of the looseness of the fertilizer in comparative test example 1.

detailed description

The present invention will be further described below in conjunction with the embodiments and accompanying drawings.

Embodiment 1, a kind of method for producing mustard special fertilizer with phosphate ore flotation tailings, carries out as follows: first configure activation bulking agent, calculate by mass percentage, with 8% humic acid, 0.5% potassium nitrate, 7.5% sodium dodecylbenzene sulfonate, 0.3% sodium dodecyl sulfonate, 0.4% OP-10, 0.4% KCl and the rest of the water are mixed uniformly to obtain the activated loosening agent;

Calculated in parts by mass, add 80 parts of phosphate rock flotation tailings, 160 parts of phosphate rock powder and 200 parts of water into the reactor, fully mix and stir evenly, and then add 200 parts of 65% nitric acid into the reactor , filter after reacting for 5 minutes, retain the filtrate, then add 150 parts of potassium nitrate, 130 parts of urea, 20 parts of ammonium phosphate and 18 parts of activated loosening agent to the filtrate until it is fully dissolved, and then add 170 parts of ammonia for neutralization reaction , the pH value of the material after the control reaction is 5.0 to obtain phosphorus fertilizer slurry, and the nitrophosphate fertilizer with high nitrate nitrogen content is obtained by concentrated spraying and granulation of the phosphorus fertilizer slurry, and the mass ratio of N:P:K in this nitrate phosphate fertilizer is 20 :8:10.

Plant mustard by conventional methods, then apply once described nitrophosphate fertilizer by the amount of 25kg/mu during the survival period of mustard mustard, and apply once again described nitrophosphate fertilizer by the amount of 20kg/mu during the expansion period of mustard mustard.

Embodiment 2, a kind of method that uses phosphate ore flotation tailings to produce mustard mustard special fertilizer, carries out according to the following steps: first configure activation loosening agent, calculate by mass percentage, with 9% polypeptide, 0.5% sodium nitrate, 7.9% Sodium dodecylbenzenesulfonate, 0.4% sodium dodecylsulfonate, 0.6% OP-10, 0.6% KCl and 81.0% water are mixed uniformly to obtain the activated loosening agent;

Calculated in parts by mass, 120 parts of phosphate rock flotation tailings, 200 parts of phosphate rock powder and 250 parts of water are added to the reactor, fully mixed and stirred evenly, and then 250 parts of phosphate rock with a concentration of 68% are added to the reactor Nitric acid, filter after reacting for 10 minutes, keep the filtrate, then add 180 parts of potassium chloride, 160 parts of urea, 30 parts of ammonium phosphate and 22 parts of activating loosening agent to the filtrate until it is fully dissolved, then add 200 parts of ammonia gas to proceed and reaction, the pH value of the material after the reaction is controlled to be 6.0 to obtain a phosphate fertilizer slurry, and the phosphate fertilizer slurry is dried and pulverized at 100° C. to obtain a nitrophosphate fertilizer with a high nitrate nitrogen content. In this nitrate phosphate fertilizer, N:P:K The mass ratio is 20:8:10.

Plant mustard by conventional methods, then apply once described nitrophosphate fertilizer by the amount of 25kg/mu during the survival period of mustard mustard, and apply once again described nitrophosphate fertilizer by the amount of 20kg/mu during the expansion period of mustard mustard.

Embodiment 3, a kind of method that uses phosphate ore flotation tailings to produce mustard mustard special fertilizer, carries out as follows: first configure activation loosening agent, calculate by mass percentage, with 8.5% humic acid, 0.5% sodium nitrate, 7.7% sodium dodecylbenzene sulfonate, 0.35% sodium dodecyl sulfonate, 0.5% OP-10 (that is, octylphenol-10), 0.5% KCl and 82.0% water mix well obtain the activated loosening agent;

Calculated in parts by mass, add 100 parts of phosphate rock flotation tailings, 180 parts of phosphate rock powder and 220 parts of water into the reactor, fully mix and stir evenly, and then add 234 parts of phosphate rock with a concentration of 66% into the reactor Nitric acid, filter after reacting for 8 minutes, keep the filtrate, then add 168 parts of potassium chloride, 145 parts of urea, 24 parts of ammonium phosphate and 20 parts of activating loosening agent to the filtrate until it is fully dissolved, then add 182 parts of ammonia to carry out and reaction, the pH value of the material after the reaction is controlled to be 5.5 to obtain a phosphate fertilizer slurry, and the phosphate fertilizer slurry is dried and pulverized at 105° C. to obtain a nitrophosphate fertilizer with a high nitrate nitrogen content. In this nitrate phosphate fertilizer, N:P:K The mass ratio is 20:8:10.

Plant mustard by conventional methods, then apply once described nitrophosphate fertilizer by the amount of 25kg/mu during the survival period of mustard mustard, and apply once again described nitrophosphate fertilizer by the amount of 20kg/mu during the expansion period of mustard mustard.

Comparative Test Example 1, the difference between this Comparative Test Example and Example 3 is that no activation loosening agent is added during the preparation process.

Contrast test example 2, plant mustard by conventional methods, apply once commercially available Tengsheng compound fertilizer (wherein N:P:K ratio is 15:15:15) by the amount of 43kg/mu in the survival period of mustard, and in mustard mustard During the expansion period, add urea at an amount of 20kg/mu.

Below in conjunction with test and test data further illustrate the present invention.

1. Contrast of porosity: Fig. 1 is a photo of the porosity of the nitrophosphate fertilizer prepared in Example 3; Fig. 2 is a photo of the porosity of the fertilizer prepared in Comparative Test Example 1; as can be seen from the comparison of Fig. 1 and Fig. 2, the addition of activation The nitrophosphate fertilizer prepared in Example 3 of the bulking agent had better dispersibility, while the fertilizer in Comparative Test Example 1 without adding the activated bulking agent was lumpy and poor in bulk.

2. The pickled mustard planted in Example 1, Example 2 and Example 3 and the mustard planted in Comparative Test Example 1 and Comparative Test Example 2 were compared respectively, and the results are shown in Table 1.

Table 1 Yield comparison

As can be seen from the above table, the yield per mu of mustard tuber and the weight of a single mustard tuber of embodiment 1-3 are all significantly higher than the yield per mu and the single weight of comparative test example 2, thus it can be seen that the nitrophosphate fertilizer prepared by the method provided by the invention is compatible with Existing common fertilizer is more suitable for mustard mustard growth; From the above table, it can also be seen that the yield per mu of mustard planted in comparative test example 1 and the single weight comparison test example 2 all increase, but slightly lower than the implementation The mustard yield per mu of example 1-3 and the weight of a single mustard, this is mainly due to not adding activated loosening agent in the fertilizer prepared in comparative test example 1, the fertilizer porosity prepared is poor and lacks organic matter, and the crop absorption utilization rate is low, Therefore, the yield per mu and the individual weight of the mustard planted are slightly lower.

In summary, the nitrophosphate fertilizer prepared by the method for producing mustard special fertilizer from phosphate ore flotation tailings provided by the present invention is very suitable for the growth of mustard, and can significantly increase the yield and individual weight of mustard.

Finally, it should be noted that the above description is only a preferred embodiment of the present invention, and those of ordinary skill in the art can make a variety of similar implementations under the inspiration of the present invention without violating the purpose and claims of the present invention. It means that such transformations all fall within the protection scope of the present invention.

Claims (7)

1. a kind of method that hot pickled mustard tube special fertilizer is produced with phosphate ore flotation tailings, it is characterised in that carry out according to the following steps：

Step (1)：By 80-120 parts of phosphate ore flotation tailings, 160-200 parts of ground phosphate rock and 200-250 parts of water are added to reactor It is interior, it is sufficiently mixed and stirs, filters, retain after 200-250 parts of nitric acid, reaction 5-10min are then added into reactor Filtrate；

Step (2)：150-180 parts of potash fertilizer, 130-160 parts of urea, 20-30 parts of phosphorus ammoniums and 18-22 parts of work are added into filtrate Change raising agent and treat that it fully dissolves；

Step (3)：170-200 parts of ammonias are added after dissolving and carry out neutralization reaction, the pH value for controlling reacting rear material is 5.0- 6.0 obtain phosphate fertilizer slurry；

Step (4)：The phosphate fertilizer slurry is concentrated into granulation or drying obtains nitrophosphate fertilizer；

Each composition is calculated according to the mass fraction above.

2. the method according to claim 1 that hot pickled mustard tube special fertilizer is produced with phosphate ore flotation tailings, it is characterised in that：The nitre N in sour phosphate fertilizer:P:K mass ratio is 20:8:10.

3. the method according to claim 1 or 2 that hot pickled mustard tube special fertilizer is produced with phosphate ore flotation tailings, it is characterised in that：Press Mass percent is calculated, and the active and porous agent is by 8-9% organic matter, 0.5% nitrate, 7.5-7.9% dodecane Base benzene sulfonic acid sodium salt, 0.3-0.4% dodecyl sodium sulfate, 0.4-0.6% OP-10,0.4-0.6% KCl and surplus Water composition.

4. the method according to claim 3 that hot pickled mustard tube special fertilizer is produced with phosphate ore flotation tailings, it is characterised in that：It is described to have Machine matter is humic acid or polypeptide.

5. the method according to claim 1 that hot pickled mustard tube special fertilizer is produced with phosphate ore flotation tailings, it is characterised in that：The nitre The concentration of acid is 65-68%.

6. the method according to claim 5 that hot pickled mustard tube special fertilizer is produced with phosphate ore flotation tailings, it is characterised in that：The potassium Fertilizer is potassium chloride or potassium nitrate.

7. the method according to claim 1 that hot pickled mustard tube special fertilizer is produced with phosphate ore flotation tailings, it is characterised in that：Step (4) drying described in is to be dried at 100-105 DEG C.