阅读说明：本技术 一种腐殖酸钾的制备方法 (Preparation method of potassium humate ) 是由 张玉军 于 2020-11-27 设计创作，主要内容包括：本发明公开了一种腐殖酸钾的制备方法,制备腐殖酸钾所需原料及质量份数为：含钾原料煤1-1.5份、氢氧化钾0.12-0.15份、工艺水0-20份；具体制备步骤为：将原料煤经破碎机破碎至20-60目；在反应器中放入破碎后的原料煤、工艺水、氢氧化钾,在85-95℃抽提35-45min；将反应物料放入沉降池进行初沉淀,将粗清液泵入沉降离心机进行固液分离,得到澄清液以及残渣；将澄清液在蒸发器中浓缩到8-12波美度,得到浓缩液；将浓缩液送至干燥机干燥后即成精制腐殖酸钾。本发明能通过原料煤与氢氧化钾溶液反应制备腐殖酸钾,其制备效率高、设备成本低,适宜推广使用；对于腐殖酸含量大于60％的原料煤,还可使用半干法以及干法制备腐殖酸钾,进一步提高制备效率。(The invention discloses a preparation method of potassium humate, which comprises the following raw materials in parts by weight: 1-1.5 parts of potassium-containing raw material coal, 0.12-0.15 part of potassium hydroxide and 0-20 parts of process water; the preparation method comprises the following specific steps: crushing the raw material coal to 20-60 meshes by a crusher; placing crushed raw material coal, process water and potassium hydroxide into a reactor, and extracting at 85-95 ℃ for 35-45 min; putting the reaction material into a sedimentation tank for primary sedimentation, and pumping the crude clear liquid into a sedimentation centrifuge for solid-liquid separation to obtain clear liquid and residues; concentrating the clear solution to 8-12 Baume degree in an evaporator to obtain concentrated solution; and (5) sending the concentrated solution to a dryer for drying to obtain the refined potassium humate. The invention can prepare the potassium humate by the reaction of the raw material coal and the potassium hydroxide solution, has high preparation efficiency and low equipment cost, and is suitable for popularization and use; for the raw material coal with humic acid content more than 60%, a semi-dry method and a dry method can be used for preparing potassium humate, so that the preparation efficiency is further improved.)

1. The preparation method of potassium humate is characterized by comprising the following raw materials in parts by weight: 1 to 1.5 portions of potassium-containing raw material coal, 0.12 to 0.15 portion of potassium hydroxide and 0 to 20 portions of process water.

2. The preparation method of potassium humate according to claim 1, which is characterized by comprising the following specific preparation steps:

s1: crushing the raw material coal to 20-60 meshes by a crusher;

s2: placing crushed raw material coal, process water and potassium hydroxide into a reactor, and extracting at 85-95 ℃ for 35-45 min;

s3: putting the reaction material into a sedimentation tank for primary sedimentation, and pumping the crude clear liquid into a sedimentation centrifuge for solid-liquid separation to obtain clear liquid and residues;

s4: concentrating the clear solution to 8-12 Baume degree in an evaporator to obtain concentrated solution;

s5: and (5) sending the concentrated solution to a dryer for drying to obtain the refined potassium humate.

3. The method for preparing potassium humate according to claim 2, wherein the residue separated by precipitation is placed in a washing tank, washed with process water for 2-3 times, and the washing water is recovered as water for the next extraction.

4. The method for preparing potassium humate according to claim 3, wherein the process water for extraction and washing is industrial soft water with hardness less than 5 mmol/L.

5. The method for preparing potassium humate according to claim 2, wherein the direct contact drying temperature is lower than 150 ℃ during the drying process using the dryer to prevent the decarboxylation and decomposition of humic acid.

6. The preparation method of potassium humate according to claim 1, which is characterized by comprising the following specific preparation steps:

s1: crushing the raw material coal to 20-60 meshes by a crusher;

s2: adding crushed raw material coal, potassium hydroxide and a small amount of process water into a reactor, stirring the mixture into paste, and reacting at 85-95 ℃ for 35-45 min;

s3: and (3) sending the pasty synthetic material to a dryer for drying to obtain the refined potassium humate.

7. The preparation method of potassium humate according to claim 1, which is characterized by comprising the following specific preparation steps:

s1: crushing the raw material coal to 20-60 meshes by a crusher;

s2: placing the crushed raw material coal into a stirring reactor, heating the raw material coal to 85-95 ℃, and stirring the raw material coal at a high speed of 300-400 r/min;

s3: and spraying and adding a potassium hydroxide solution into the stirring reactor during the stirring process, and continuously stirring and reacting for 35-45min to obtain the crude potassium humate.

Technical Field

The invention relates to the technical field of humic acid preparation, and particularly relates to a preparation method of potassium humate.

Background

The water-soluble potassium salt resource in China is very little, and the storage capacity (equivalent to K2O) of the potassium salt is only 2.1 hundred million tons and only accounts for 2.2 percent of the world storage capacity at present. According to statistics, the total yield of potassium chloride, potassium sulfate and potassium magnesium sulfate fertilizers, namely Chinese resource type potassium fertilizers in 2012, is 377 ten thousand tons (converted to pure K2O), and the self-feeding rate of potassium salts (fertilizers) is 47.8 percent. The domestic potash fertilizer yield can reach 400 ten thousand tons in 2015 predicted; compared with the apparent consumption of 795.4 ten thousand tons (converted from pure K2O) in 2012, the water-soluble potassium salt resource in China has problems in both short-term supply capacity and long-term guarantee degree. The potassium humate is a high-efficiency organic potassium fertilizer. The potassium humate is a macromolecular non-uniform aromatic hydroxycarboxylic acid salt, is a black particle or powdery solid in appearance, is prepared by chemical reaction of humic acid and potassium hydroxide, is instantly dissolved in water, is alkaline, has various active groups such as carboxyl, phenolic hydroxyl and the like, and has various functions such as ion exchange, adsorption, complexation, flocculation, dispersion, bonding and the like. The potassium humate can improve the content of quick-acting potassium in soil, reduce the loss and fixation of potassium, increase the absorption and utilization rate of potassium by crops, improve the soil, promote the growth of crops, improve the stress resistance of crops, improve the quality of crops, protect the agricultural ecological environment and the like, and can be prepared into a high-efficiency multifunctional compound fertilizer after being mixed with a nitrogen fertilizer, a phosphate fertilizer, a potassium fertilizer and the like. Therefore, a method for efficiently and quickly preparing potassium humate is needed.

Disclosure of Invention

The invention provides a preparation method of potassium humate, which can prepare the potassium humate by reacting raw material coal with a potassium hydroxide solution, has high preparation efficiency and low equipment cost, is suitable for popularization and application, and can prepare the potassium humate by using a semi-dry method and a dry method for the raw material coal with the humic acid content of more than 60 percent, thereby further improving the preparation efficiency.

In order to solve the technical problems, the invention provides the following technical scheme:

the invention provides a preparation method of potassium humate, which comprises the following raw materials in parts by weight: 1 to 1.5 portions of potassium-containing raw material coal, 0.12 to 0.15 portion of potassium hydroxide and 0 to 20 portions of process water.

As a preferred technical scheme of the invention, the preparation method specifically comprises the following steps:

s1: crushing the raw material coal to 20-60 meshes by a crusher;

s2: placing crushed raw material coal, process water and potassium hydroxide into a reactor, and extracting at 85-95 ℃ for 35-45 min;

s3: putting the reaction material into a sedimentation tank for primary sedimentation, and pumping the crude clear liquid into a sedimentation centrifuge for solid-liquid separation to obtain clear liquid and residues;

s4: concentrating the clear solution to 8-12 Baume degree in an evaporator to obtain concentrated solution;

s5: and (5) sending the concentrated solution to a dryer for drying to obtain the refined potassium humate.

As a preferred technical scheme of the invention, the residue separated by precipitation is put into a washing tank, washed by process water for 2-3 times, and the washing water is recycled as water for next extraction.

As a preferred technical scheme of the invention, the process water for extraction and washing is industrial soft water, and the hardness of the industrial soft water is less than 5 mmol/L.

As a preferable technical scheme of the invention, in the drying process by using the dryer, the direct contact drying temperature is lower than 150 ℃ in order to prevent the decarboxylation and decomposition of the humic acid.

As a preferred technical scheme of the invention, the specific preparation steps can also be as follows:

s1: crushing the raw material coal to 20-60 meshes by a crusher;

s2: adding crushed raw material coal, potassium hydroxide and a small amount of process water into a reactor, stirring the mixture into paste, and reacting at 85-95 ℃ for 35-45 min;

s3: and (3) sending the pasty synthetic material to a dryer for drying to obtain the refined potassium humate.

As a preferred technical scheme of the invention, the specific preparation steps can also be as follows:

s1: crushing the raw material coal to 20-60 meshes by a crusher;

s2: placing the crushed raw material coal into a stirring reactor, heating the raw material coal to 85-95 ℃, and stirring the raw material coal at a high speed of 300-400 r/min;

s3: and spraying and adding a potassium hydroxide solution into the stirring reactor during the stirring process, and continuously stirring and reacting for 35-45min to obtain the crude potassium humate.

The invention has the following beneficial effects:

the method can prepare the potassium humate by reacting the raw material coal with the potassium hydroxide solution, has high preparation efficiency and low equipment cost, is suitable for popularization and use, and has the advantages that residues separated by precipitation in the preparation process are put into the washing tank and washed by the process water for several times, and the washing water is recycled as water for next extraction, so that not only can the waste water be utilized to save water resources, but also the humic acid attached to the washing water can be recycled, and the waste of the humic acid is prevented; for the raw material coal with humic acid content more than 60%, a semi-dry method and a dry method can be used for preparing potassium humate, so that the preparation efficiency is further improved.

Detailed Description

The following description of the preferred embodiments of the present invention is provided for the purpose of illustration and description, and is in no way intended to limit the invention.

Example 1

The invention provides a preparation method of potassium humate, which comprises the following raw materials in parts by weight: 1 part of potassium-containing raw material coal, 0.14 part of potassium hydroxide and 15 parts of process water.

The preparation method comprises the following specific steps:

s1: crushing the raw material coal to 20-60 meshes by a crusher;

s2: placing crushed raw material coal, process water and potassium hydroxide into a reactor, and extracting at 85-95 ℃ for 35-45 min;

s3: putting the reaction material into a sedimentation tank for primary sedimentation, and pumping the crude clear liquid into a sedimentation centrifuge for solid-liquid separation to obtain clear liquid and residues;

s4: concentrating the clear solution to 8-12 Baume degree in an evaporator to obtain concentrated solution;

s5: and (5) sending the concentrated solution to a dryer for drying to obtain the refined potassium humate.

And (4) putting the residue separated by precipitation into a washing tank, washing with the process water for 2-3 times, and recovering the washing water as water for next extraction. The process water used for extraction and washing is industrial soft water with hardness less than 5 mmol/L. In the drying process by using the dryer, the direct contact drying temperature is lower than 150 ℃ in order to prevent the decarboxylation and decomposition of the humic acid.

Example 2

The invention provides a preparation method of potassium humate, which can be used for preparing the potassium humate by a semi-dry method when the content of humic acid in raw material coal is more than 60 percent.

The specific preparation steps can also be as follows:

s1: crushing the raw material coal to 20-60 meshes by a crusher;

s2: adding crushed raw material coal, potassium hydroxide and a small amount of process water into a reactor, stirring the mixture into paste, and reacting at 85-95 ℃ for 35-45 min;

s3: and (3) sending the pasty synthetic material to a dryer for drying to obtain the refined potassium humate.

Example 3

The invention provides a preparation method of potassium humate, which can be used for preparing the potassium humate by a dry method when the content of humic acid in raw material coal is more than 60 percent.

Crushing the raw material coal to 20-60 meshes by a crusher;

s2: placing the crushed raw material coal into a stirring reactor, heating the raw material coal to 85-95 ℃, and stirring the raw material coal at a high speed of 300-400 r/min;

s3: and spraying and adding a potassium hydroxide solution into the stirring reactor during the stirring process, and continuously stirring and reacting for 35-45min to obtain the crude potassium humate.

The method can prepare the potassium humate by reacting the raw material coal with the potassium hydroxide solution, has high preparation efficiency and low equipment cost, is suitable for popularization and use, and has the advantages that residues separated by precipitation in the preparation process are put into the washing tank and washed by the process water for several times, and the washing water is recycled as water for next extraction, so that not only can the waste water be utilized to save water resources, but also the humic acid attached to the washing water can be recycled, and the waste of the humic acid is prevented; for the raw material coal with humic acid content more than 60%, a semi-dry method and a dry method can be used for preparing potassium humate, so that the preparation efficiency is further improved.

Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.