阅读说明：本技术 改良土壤圈的颗粒、制造方法和用途 (Soil improvement ring granule, manufacturing method and application ) 是由 弗雷德·博恩迪克 马蒂亚斯·赫格尔 于 2018-11-30 设计创作，主要内容包括：本发明涉及一种用于制造改良土壤圈的颗粒(6)的方法,包括下列步骤：a)生成原材料分散体,其包含至少一种无机二代磷酸盐(1)和至少一种反应剂(2),其中原材料分散体中的液相(4)的份额大于30％,无机二代磷酸盐(1)与反应剂(2)之间的培养时间处于1至100分钟之间；b)分离原材料分散体的部分液相(4)；c)将包括减少的液相(4)的剩余原材料分散体制成颗粒和/或使其挤压成型；d)或者在无需至少部分的重金属分离(5)的情况下,使在工艺步骤b)中分离的液相(4)回流至用于制造原材料分散体的工艺步骤a)中,或者至少部分地从在工艺步骤b)中分离的液相(4)中离析出重金属(7),并且从工艺中提取出重金属(7),随后使分离出的、贫重金属的液相(4)回流,以便以类似于工艺步骤a)的方式制造原材料分散体和/或使其回流至工艺步骤c)；以及e)重复工艺步骤a)至d)。本发明还涉及一种可用该方法制造的改良土壤圈的颗粒(6)以及一种可用于在农业、林业和/或园艺领域中供应营养物质的有涂层或者无涂层的肥料颗粒。(The invention relates to a method for producing soil improvement granules (6), comprising the following steps: a) generating a raw material dispersion comprising at least one inorganic dibasic phosphate (1) and at least one reactant (2), wherein the proportion of liquid phase (4) in the raw material dispersion is greater than 30%, and the incubation time between the inorganic dibasic phosphate (1) and the reactant (2) is between 1 and 100 minutes; b) separating a part of the liquid phase (4) of the raw material dispersion; c) granulating and/or extruding the remaining raw material dispersion comprising the reduced liquid phase (4); d) or the liquid phase (4) separated in process step b) is returned to process step a) for producing the raw material dispersion without at least partial heavy metal separation (5), or the heavy metal (7) is at least partially isolated from the liquid phase (4) separated in process step b) and the heavy metal (7) is extracted from the process, and the separated, heavy metal-depleted liquid phase (4) is subsequently returned in order to produce the raw material dispersion in a manner analogous to process step a) and/or to return it to process step c); and e) repeating process steps a) to d). The invention also relates to a granule (6) for improving soil circles, which can be produced by the method, and to a coated or uncoated fertilizer granule which can be used for the supply of nutrients in the agricultural, forestry and/or horticultural field.)

1. A soil improvement granule (6) obtainable by a process comprising the steps of:

a) generating a raw material dispersion comprising at least one inorganic dibasic phosphate (1) and at least one reactant (1), wherein the proportion of liquid phase (4) in the raw material dispersion is greater than 30%, and the incubation time between inorganic dibasic phosphate (1) and reactant (2) is between 1 and 100 minutes;

b) separating a portion of the liquid phase (4) of the raw material dispersion;

c) granulating and/or extruding the remaining raw material dispersion comprising the reduced liquid phase (4);

d) refluxing the liquid phase (4) separated in process step b) to the process step a) for producing a raw material dispersion without at least partial heavy metal separation (5),

orAt least partially isolating heavy metals (7) from the liquid phase (4) separated in process step b) and extracting the heavy metals (7) from the process, followed by refluxing the separated, heavy metal-depleted liquid phase (4) in order to produce a raw material dispersion in a similar manner to process step a) and/or to reflux it to process step c); and is

e) Repeating the process steps a) to d).

2. A method for producing soil improvement granules (6),

the method comprises the following steps:

a) generating a raw material dispersion comprising at least one inorganic dibasic phosphate (1) and at least one reactant (2), wherein the proportion of liquid phase (4) in the raw material dispersion is greater than 30%, and the incubation time between inorganic dibasic phosphate (1) and reactant (2) is between 1 and 100 minutes;

b) separating a portion of the liquid phase (4) of the raw material dispersion;

c) granulating and/or extruding the remaining raw material dispersion comprising the reduced liquid phase (4);

d) refluxing the liquid phase (4) separated in process step b) to the process step a) for producing a raw material dispersion without at least partial heavy metal separation (5),

orAt least partially isolating heavy metals (7) from the liquid phase (4) separated in process step b) and extracting the heavy metals (7) from the process, followed by refluxing the separated, heavy metal-depleted liquid phase (4) in order to produce a raw material dispersion in a similar manner to process step a) and/or to reflux it to process step c); and is

e) Repeating the process steps a) to d).

3. The particle (6) according to claim 1, or the method according to claim 2,

it is characterized in that the preparation method is characterized in that,

before the partial separation of the liquid phase (4), the raw material dispersion is set such that the solid matter fraction is less than 50%.

4. The particle (6) according to claim 1 or 3, or the method according to claim 2 or 3,

it is characterized in that the preparation method is characterized in that,

the pH value of the raw material dispersion produced before partial separation of the liquid phase (4) is in the range between 1.5 and 3.5.

5. The particle (6) according to claim 1, 3 or 4, or the method according to claim 2, 3 or 4,

it is characterized in that the preparation method is characterized in that,

the at least partial separation of the heavy metals (7) from the liquid phase (4) separated in process step b) is effected by one or more precipitation reactions and subsequent separation of the precipitated product.

6. The particle (6) according to one or more of claims 1, 3, 4 or 5, or the method according to one or more of claims 2 to 5,

it is characterized in that the preparation method is characterized in that,

before and during the partial separation of the liquid phase (4), the pH of the raw material dispersion produced is less than 2.

7. The particle (6) according to one or more of claims 1, 3, 4, 5 or 6, or the method according to one or more of claims 2 to 6,

it is characterized in that the preparation method is characterized in that,

the at least partial separation of the heavy metals (7) from the liquid phase separated in process step b) is effected by one or more selective separation methods.

8. The particle (7) according to one or more of claims 1, 3, 4, 5, 6 or 7, or the method according to one or more of claims 2 to 7,

it is characterized in that the preparation method is characterized in that,

the moisture content of the raw material dispersion from process step b) comprising the reduced liquid phase (4) is between 10% and 40%.

9. The particle (8) according to one or more of claims 1, 3, 4, 5, 6, 7 or 8, or the method according to one or more of claims 2 to 8,

it is characterized in that the preparation method is characterized in that,

the pH of the raw material dispersion comprising the reduced liquid phase (4) is in the range of 4 to 8.

10. The particle (6) according to one or more of claims 1 or 3 to 9, or the method according to one or more of claims 2 to 9,

it is characterized in that the preparation method is characterized in that,

■ the liquid phase (4) separated in process step b) is supplied to at least partial heavy metal separation (5),

■ is at least partially freed from the heavy metals (7) and is subsequently supplied to a process step a) for producing a raw material suspension, wherein the reactant (2) can be at least partially supplied to the liquid phase (4) before or during the reflux to process step a),

■ the raw material dispersion comprising a reduced liquid phase (4) which has undergone process step b) has a solids content of 40% to 70%, and

■ the raw material dispersion comprising a reduced liquid phase (4) is supplied to the granulation.

11. The particle (6) according to one or more of claims 1 or 3 to 10, or the method according to one or more of claims 2 to 10,

it is characterized in that the preparation method is characterized in that,

immediately after granulation, the resulting nutrient granules (6) are fractionated, wherein the crude fraction and/or the fine fraction are ground and can be supplied at least partially to steps a), b) and/or c).

12. The particle according to one or more of claims 1 or 3 to 11, or the method according to one or more of claims 2 to 11,

it is characterized in that the preparation method is characterized in that,

a total of 1% to 70% of the phosphorus-removed crystalline product can be supplied to steps a), b) and/or c).

13. The particle according to one or more of claims 1 or 3 to 12, or the method according to one or more of claims 2 to 12,

it is characterized in that the preparation method is characterized in that,

drying is carried out at a temperature of 100 ℃ or higher, based on the temperature of the material during the drying process.

14. An apparatus for making a particle according to any of the preceding claims 1 or 3 to 13, the apparatus comprising:

■ at least one first mixing vessel for supplying and/or mixing at least one of the inorganic dibasic phosphate (1) and the reactant (2), thereby obtaining a raw material dispersion, wherein for the incubation time, either the first mixing vessel is used and/or there is a further vessel into which the raw material dispersion is transferred and mixed during the incubation time;

■ at least one separation unit for separating at least a part of the liquid phase (4), wherein the separation unit is integrated in the first mixing vessel or independent of the first mixing vessel;

■ at least one granulating and/or extruding unit for granulating and/or extruding the remaining raw material dispersion from process step b) comprising the reduced liquid phase (4), wherein in the granulating and/or extruding unit further ingredients (3) can be supplied, and/or the raw material dispersion can be mixed, wherein there is at least one supply unit originating from the separating unit for transferring the raw material dispersion to the granulating and/or extruding unit;

■ at least one reflux unit suitable for the liquid phase (4) separated without heavy metal deposition (5) or after partial isolation of the heavy metals (7), which leads to the mixing vessel for the production of a raw material dispersion in a similar manner to process step a) and/or to the pelletizing and/or extrusion unit.

15. The apparatus of claim 14, wherein the first and second electrodes are disposed on opposite sides of the substrate,

it is characterized in that the preparation method is characterized in that,

the pelletizing and/or extrusion unit is an intensive mixer, a pelletizer disk or a fluidized bed reactor or a spouted bed reactor.

16. The apparatus according to claim 14 or 15,

it is characterized in that the preparation method is characterized in that,

the device comprises a unit for isolating the heavy metal (7), in which unit at least a part of the heavy metal can be separated from the liquid phase (4) separated in process step b) and can be extracted from the process, wherein at least one supply unit is present which originates from the separation unit and is used for transferring the partially separated liquid phase (4) into the unit for isolating the heavy metal (7).

17. A coated or uncoated fertilizer granule (6),

it is characterized in that the preparation method is characterized in that,

the fertilizer granules (6) contain at least one inorganic dibasic phosphate (1) and a proportion of neutral ammonium citrate-soluble P2O5 of more than 60%, based on the total phosphate content in the fertilizer granules (6).

18. Coated or uncoated fertilizer granule (6) according to claim 17,

it is characterized in that the preparation method is characterized in that,

the fertilizer granules (6) contain at least one inorganic dibasic phosphate (1) and a proportion of neutral ammonium citrate-soluble P2O5 of more than 60%, based on the total phosphate content in the fertilizer granules (6), wherein the water solubility of the phosphate proportion from the inorganic dibasic phosphate (1) in the P2O5 proportion is less than 40%.

19. Coated or uncoated fertilizer granule (6) according to claim 17 or 18,

it is characterized in that the preparation method is characterized in that,

the fertilizer granules (6) contain 0.1 to 25% in total of humic acid, fulvic acid and salts thereof (humates, fulvates), and/or 0.1 to 30% in total of organic acids, and/or 0.1 to 50% in total of structural substances.

20. Coated or uncoated fertilizer granule (6) according to one or more of claims 17 to 19,

it is characterized in that the preparation method is characterized in that,

the fertilizer granules (6) contain one or more crystalline products precipitated from phosphorus removal in a concentration range of 1% to 70%.

21. Use of a fertilizer granule (6) according to one or more of claims 17 to 20 for the supply of nutrients in the agricultural, forestry and/or horticultural field,

it is characterized in that the preparation method is characterized in that,

the fertilizer granules (6) contain at least one inorganic dibasic phosphate (1) and a proportion of neutral ammonium citrate-soluble P2O5 of more than 60%.

Example 3 (according to the invention):

similar to example 2, a raw material dispersion was generated from 140kg of water, 110kg of phosphoric acid (85%) and 100kg of sewage sludge ash (P2O5 content 21.0%, 38% of which is neutral ammonium citrate soluble, < 1% is water soluble; heavy metal content 178mg/kg of Pb, 75mg/kg of Ni and 18.3mg/kg of Cd) and maintained for an incubation time of 25 minutes.

After the incubation time, the raw material dispersion thus produced is supplied to solid-liquid separation. By means of a filter press, the majority of the liquid phase is separated from the undissolved solid matter, so that preferably a wet solid matter mixture with a humidity of less than 20% is formed.

The separated solution still containing nutrients is refluxed to the process for the next batch of manufacturing raw material dispersion and preferably replaces the water share in the formula of the raw material dispersion listed above in equal amounts. In the case of a continuously running process control, an equilibrium cycle of the dissolved substances is established in this subcycle. Correspondingly, after establishing this equilibrium, the amount of phosphate added by the sewage sludge ash is transferred to the granulation and thus, as desired, into the granules.

The wet solid-matter mixture resulting from the solid-liquid separation is transferred to an intensive mixer (alli corporation, R16W) and is intensively mixed there. Preferably, the ratio of solid matter to liquid phase is set in the intensive mixer by adding water or powder (such as sewage sludge ash) so that during intensive mixing a granular green body of the desired size is formed. The formed green pellets are then dried at 110 ℃ and fractionated into a pellet body having a diameter in the range between 2 and 5 mm. The distillate of the particle body with the diameter less than 2mm and the distillate of the particle body with the diameter more than 5mm are refluxed to granulation after being ground in advance.

After establishing the equilibrium cycle described hereinabove, the resulting particles advantageously have a rounded and compact particle shape in the range of 2-5mm with a total content of P2O5 of 46%, of which 93% is ammonium citrate soluble and 61% is water soluble. The resulting fertilizer granules contain approximately 52% of the used sewage sludge ash, so that the following heavy metal concentrations result in the resulting fertilizer granules as a result of the simultaneous input of sewage sludge ash: a lead concentration of 92mg/kg, a nickel concentration of 39mg/kg and a cadmium concentration of 10 mg/kg.

The advantage of this embodiment compared to example 1 is that the reaction between ash and acid takes place in the resulting raw material dispersion, which is thus controllable, and that due to the small amount of free acid, corrosion problems hardly occur.

The main advantage compared to example 2 is that a portion of the liquid phase is mechanically separated from the raw material dispersion. Thus, only a very small amount of water has to be evaporated, which saves a lot of energy costs and thus makes the process more economical.