CN111171335A - Method for preparing sodium humate from low-calcium magnesium ore source - Google Patents
Method for preparing sodium humate from low-calcium magnesium ore source Download PDFInfo
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- CN111171335A CN111171335A CN202010072268.1A CN202010072268A CN111171335A CN 111171335 A CN111171335 A CN 111171335A CN 202010072268 A CN202010072268 A CN 202010072268A CN 111171335 A CN111171335 A CN 111171335A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
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Abstract
The invention discloses a method for preparing sodium humate from a low-calcium magnesium mineral source. The method comprises the steps of using mineral source soil raw materials with calcium and magnesium contents of 2-5 wt%, firstly using a wet ball mill to crush the mineral source soil, and then using Na2CO3The double decomposition reaction method comprises the steps of extracting to obtain a sodium humate solution, and carrying out spray drying on the sodium humate solution to obtain the sodium humate with higher purity, wherein the content (in terms of dry basis) of soluble humic acid of the produced sodium humate is more than 50%. The invention has the advantages that: the process is simple and the operation is convenient; the waste mineral source soil is utilized, so that the environment is friendly; the utilization rate of the mineral source soil is high; the prepared sodium humate has high purity and high content of soluble humic acid.
Description
Technical Field
The invention belongs to the field of mineral source soil treatment and sodium humate production, and particularly relates to a method for preparing sodium humate by using calcium and magnesium-containing mineral source soil.
Background
The main components of the mineral source soil are weathered coal, peat, lignite and other impurities. Due to the difficulty of separation and insufficient carbon content, the utilization rate of the mineral source soil is low. The weathered coal, peat and lignite in the mineral soil contain a large amount of humic acid, and can be used for processing products for producing the humic acid and humate (soil report, 2003, 34(4): 343-345.). Humic acid exists in mineral soil mainly in two forms of free humic acid, calcium humate and magnesium salt.
The sodium humate is black amorphous particles, is nontoxic, odorless and non-corrosive, and is very easy to dissolve in water. It is mainly used for astringing, stopping bleeding and stopping diarrhea. Meanwhile, the fertilizer is used as a compound fertilizer in agriculture, can change the soil structure and has the effects of preventing diseases, resisting diseases, increasing yield and increasing income for crops; as a feed additive in livestock breeding; the compound is used as a synergist in aquaculture, and remarkable economic benefits are obtained. The traditional production method is to use weathered coal, peat or lignite with low content of calcium and magnesium (less than 2 wt%) as a coal source, add NaOH to perform a neutralization reaction after crushing to obtain a sodium humate solution, perform precipitation separation and evaporation drying to obtain a sodium humate sample (environmental science and management, 2008, 33(12): 37-40.).
The traditional production method of sodium humate has low utilization rate of mineral source soil containing calcium and magnesium as raw materials, and insoluble calcium humate and magnesium salts in weathered coal, peat and lignite can not be extracted. Meanwhile, the problems of high energy consumption and long consumed time in the traditional production process are solved, and the economic benefit is not realized.
Sodium humate prepared from ore source soil containing calcium and magnesium (2-5 wt%), and Na2CO3Carrying out double decomposition reaction to effectively utilize insoluble calcium magnesium humate in the mineral source soil to prepare the sodium humate with high purity and high soluble humic acid content.
Disclosure of Invention
The invention aims to overcome the problems in the prior art, the mineral source soil with the calcium and magnesium content of 2-5 wt% is used as the raw material to prepare the sodium humate, the indissolvable calcium magnesium humate in the mineral source soil is effectively utilized, and the utilization rate of the mineral source soil is improved.
The technical scheme for solving the technical problems is as follows:
a preparation method of sodium humate comprises the following steps of taking ore source soil with calcium and magnesium contents of 2-5 wt% as raw materials, crushing the raw materials into coal slurry through wet ball milling, and then adding Na with the concentration of 15 wt%2CO3The pH value of the mixed slurry is 9.0-10.0 through the solution, the double decomposition reaction temperature is 80-90 ℃, and the stirring time is 30-50 min; then, centrifugal solid-liquid separation is utilized to obtain supernatant, and simultaneously soft water is utilized to wash solid waste after solid-liquid separation; and finally, spray drying the supernatant at an inlet temperature of 220-240 ℃ and an outlet temperature of 90-110 ℃ to obtain sodium humate solid powder, wherein the content of soluble humic acid (calculated on a dry basis) is more than 50%.
In the above-mentioned method for producing sodium humate, Na is added at a concentration of 15 wt% in the above-mentioned step2CO3The solution is such that the pH of the mixed slurry is preferably 9.0.
In the above method for preparing sodium humate, the metathesis reaction temperature in the step is preferably 90 ℃.
In the above method for producing sodium humate, the stirring time in the step is preferably 40 min.
In the above method for preparing sodium humate, in the step, the supernatant is spray-dried, preferably at an inlet temperature of 230 ℃ and preferably at an outlet temperature of 100 ℃.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the preparation method of the sodium humate, mineral soil containing calcium and magnesium (2-5 wt%) is used as a raw material, and insoluble calcium magnesium humate in the mineral soil is effectively utilized.
2. The preparation method of the sodium humate has high economic benefit, not only saves the production cost and the production time, but also increases the utilization rate of raw materials.
3. The preparation method of the sodium humate has simple process and convenient and fast operation; the waste mineral source soil is utilized, so that the environment is friendly; the utilization rate of the mineral source soil is high; the purity and the content of the soluble humic acid of the prepared sodium humate are high, and the content of the soluble humic acid (calculated by dry basis) is more than 50 percent.
Detailed Description
The present invention will be further described with reference to the following examples, but it should be noted that the scope of the present invention is not limited to these examples.
Example 1
A preparation method of sodium humate comprises the following steps: taking ore source soil with calcium and magnesium contents of 2-5 wt% as raw materials, firstly crushing the raw materials into coal slurry through wet ball milling, and then adding Na with the concentration of 15 wt%2CO3The solution enables the pH value of the mixed slurry to reach 9.0, the double decomposition reaction temperature is 80 ℃, and the stirring time is 30 min; then obtaining supernatant by centrifugal solid-liquid separation, washing the solid waste residue after the solid-liquid separation by using soft water, wherein the washing water can be used for preparing Na2CO3And (3) solution. And finally, spray drying the supernatant at an inlet temperature of 220 ℃ and an outlet temperature of 90 ℃ to obtain sodium humate solid powder, wherein the content of soluble humic acid (calculated on a dry basis) reaches 52%.
Example 2
A preparation method of sodium humate comprises the following steps: taking ore source soil with calcium and magnesium contents of 2-5 wt% as raw materials, firstly crushing the raw materials into coal slurry through wet ball milling, and then adding Na with the concentration of 15 wt%2CO3The solution enables the pH value of the mixed slurry to reach 10.0, the temperature of double decomposition reaction is 90 ℃, and the stirring time is 40 min; then obtaining supernatant by centrifugal solid-liquid separation, washing the solid waste residue after the solid-liquid separation by using soft water, wherein the washing water can be used for preparing Na2CO3And (3) solution. And finally, spray drying the supernatant at an inlet temperature of 240 ℃ and an outlet temperature of 100 ℃ to obtain sodium humate solid powder, wherein the content of soluble humic acid (calculated on a dry basis) reaches 53%.
Example 3
A preparation method of sodium humate comprises the following steps: taking ore source soil with calcium and magnesium contents of 2-5 wt% as raw materials, firstly crushing the raw materials into coal slurry through wet ball milling, and then adding Na with the concentration of 15 wt%2CO3The pH value of the mixed slurry is 10.0 through the solution, the temperature of double decomposition reaction is 85 ℃, and the stirring time is 50 min; then obtaining supernatant by centrifugal solid-liquid separation, washing the solid waste residue after the solid-liquid separation by using soft water, wherein the washing water can be used for preparing Na2CO3And (3) solution. Finally, the supernatant is spray-dried, the inlet temperature is 230 ℃, and the outlet temperature is 1And (3) obtaining sodium humate solid powder at 10 ℃, wherein the content of soluble humic acid (calculated on a dry basis) reaches 51%.
Example 4
A preparation method of sodium humate comprises the following steps: taking ore source soil with calcium and magnesium contents of 2-5 wt% as raw materials, firstly crushing the raw materials into coal slurry through wet ball milling, and then adding Na with the concentration of 15 wt%2CO3The solution enables the pH value of the mixed slurry to reach 9.0, the metathesis reaction temperature is 90 ℃, and the stirring time is 40 min; then obtaining supernatant by centrifugal solid-liquid separation, washing the solid waste residue after the solid-liquid separation by using soft water, wherein the washing water can be used for preparing Na2CO3And (3) solution. And finally, spray drying the supernatant at an inlet temperature of 220 ℃ and an outlet temperature of 100 ℃ to obtain sodium humate solid powder, wherein the content of soluble humic acid (calculated on a dry basis) reaches 52%.
Claims (5)
1. A preparation method of sodium humate is characterized by comprising the following steps: taking ore source soil with calcium and magnesium contents of 2-5 wt% as raw materials, firstly crushing the raw materials into coal slurry through wet ball milling, and then adding Na with the concentration of 15 wt%2CO3Enabling the pH value of the mixed slurry to reach 9.0-10.0 through the solution, carrying out double decomposition reaction at 80-90 ℃, and stirring for 30-50 min; then, centrifugal solid-liquid separation is utilized to obtain supernatant, and simultaneously soft water is utilized to wash solid waste after solid-liquid separation; and finally, spray drying the supernatant, wherein an inlet is at 220-240 ℃ and an outlet is at 90-110 ℃, so as to obtain sodium humate solid powder.
2. The method for preparing sodium humate according to claim 1, wherein Na is added at a concentration of 15 wt%2CO3The solution brought the pH of the mixed slurry to 9.0.
3. The preparation method of sodium humate according to claim 1, characterized in that the metathesis reaction is carried out at 90 ℃.
4. The method for preparing sodium humate according to claim 1, wherein the stirring time is 40 min.
5. The preparation method of sodium humate according to claim 1, characterized in that the supernatant is spray dried at 230 ℃ at the inlet and 100 ℃ at the outlet.
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| CN202010072268.1A CN111171335A (en) | 2020-01-21 | 2020-01-21 | Method for preparing sodium humate from low-calcium magnesium ore source |
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| CN202010072268.1A CN111171335A (en) | 2020-01-21 | 2020-01-21 | Method for preparing sodium humate from low-calcium magnesium ore source |
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Citations (5)
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| CN106565973A (en) * | 2016-11-14 | 2017-04-19 | 内蒙古永业生物科学技术研究院 | Preparation method of mineral-based fulvic acid |
| CN107400244A (en) * | 2017-08-03 | 2017-11-28 | 山西绿能新动力环保科技有限公司 | A kind of environment-friendly production process of nitric fulvic acid potassium |
| CN109400910A (en) * | 2018-10-23 | 2019-03-01 | 宁夏天鑫源生物科技有限公司 | A kind of neutrality sodium humate and its preparation method and application |
| CN109796604A (en) * | 2019-01-30 | 2019-05-24 | 宁夏然尔特工业产业研究院（有限公司） | A method of the active humic acid rich in fulvic acid is produced by mineral resources humate |
| CN110358110A (en) * | 2019-07-24 | 2019-10-22 | 西安集佰侬生物科技有限公司 | A kind of preparation method of mineral sources potassium fulvate |
-
2020
- 2020-01-21 CN CN202010072268.1A patent/CN111171335A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106565973A (en) * | 2016-11-14 | 2017-04-19 | 内蒙古永业生物科学技术研究院 | Preparation method of mineral-based fulvic acid |
| CN107400244A (en) * | 2017-08-03 | 2017-11-28 | 山西绿能新动力环保科技有限公司 | A kind of environment-friendly production process of nitric fulvic acid potassium |
| CN109400910A (en) * | 2018-10-23 | 2019-03-01 | 宁夏天鑫源生物科技有限公司 | A kind of neutrality sodium humate and its preparation method and application |
| CN109796604A (en) * | 2019-01-30 | 2019-05-24 | 宁夏然尔特工业产业研究院（有限公司） | A method of the active humic acid rich in fulvic acid is produced by mineral resources humate |
| CN110358110A (en) * | 2019-07-24 | 2019-10-22 | 西安集佰侬生物科技有限公司 | A kind of preparation method of mineral sources potassium fulvate |
Non-Patent Citations (2)
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| 吕春和等: "用高钙镁风化煤制备植物生长刺激素", 《化学世界》 * |
| 王学江等: "山西风化煤腐植酸活化研究", 《磷肥与复肥》 * |
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