CN112442189A - Preparation method of sodium humate - Google Patents
Preparation method of sodium humate Download PDFInfo
- Publication number
- CN112442189A CN112442189A CN202011361305.7A CN202011361305A CN112442189A CN 112442189 A CN112442189 A CN 112442189A CN 202011361305 A CN202011361305 A CN 202011361305A CN 112442189 A CN112442189 A CN 112442189A
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- sodium humate
- sodium
- humate
- solution
- water
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 title claims abstract description 61
- 239000011734 sodium Substances 0.000 title claims abstract description 61
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 61
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 54
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000003245 coal Substances 0.000 claims abstract description 20
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 238000004062 sedimentation Methods 0.000 claims abstract description 12
- 238000003916 acid precipitation Methods 0.000 claims abstract description 9
- 239000003513 alkali Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 239000002244 precipitate Substances 0.000 claims abstract description 8
- 230000008569 process Effects 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 6
- 239000002253 acid Substances 0.000 claims abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 238000002386 leaching Methods 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims abstract description 4
- 230000001376 precipitating effect Effects 0.000 claims abstract description 4
- 238000005086 pumping Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 239000003077 lignite Substances 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 3
- 230000020477 pH reduction Effects 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 6
- 239000012535 impurity Substances 0.000 abstract description 6
- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 description 5
- 239000004021 humic acid Substances 0.000 description 5
- 239000002689 soil Substances 0.000 description 5
- 229910052500 inorganic mineral Inorganic materials 0.000 description 4
- 239000011707 mineral Substances 0.000 description 4
- 239000003415 peat Substances 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 239000003337 fertilizer Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 206010012735 Diarrhoea Diseases 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 239000003674 animal food additive Substances 0.000 description 1
- 238000009360 aquaculture Methods 0.000 description 1
- 244000144974 aquaculture Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 244000144972 livestock Species 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000009972 noncorrosive effect Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G99/00—Subject matter not provided for in other groups of this subclass
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Fertilizers (AREA)
Abstract
The invention discloses a preparation method of sodium humate, which comprises the following specific preparation steps: crushing the raw material coal to 20-60 meshes by a crusher; preparing a sodium hydroxide solution with the concentration of 1% by taking a proper amount of sodium hydroxide and process water; adding crushed raw material coal and sodium hydroxide solution into a reactor, stirring and leaching for 35-45min at 85-95 ℃; 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; adding a proper amount of sulfuric acid into the clear solution for acid precipitation, precipitating sodium humate from the solution in a gel state, and settling the mixture for 24 hours to allow the mixture to settle and separate automatically; separating to remove the upper layer acid water, and cleaning the precipitate with clear water for 2-3 times; and (5) drying the precipitate to obtain the sodium humate. The method can remove alkali soluble inorganic impurities in the sodium humate through acid precipitation treatment, and can purify the sodium humate, so that the purity of the sodium humate can be improved, and the use effect of the sodium humate is further improved.
Description
Technical Field
The invention relates to the technical field of humic acid preparation, in particular to a preparation method of sodium humate.
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. A large amount of humic acid exists in weathered coal, peat and lignite in the mineral soil, and can be used for processing and producing products of humic acid and humate. 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 that weathered coal, peat or lignite with low calcium and magnesium content (less than 2 wt%) is used as a coal source, NaOH is added after the weathered coal, peat or lignite is crushed to perform a neutralization reaction to obtain a sodium humate solution, and the sodium humate solution is obtained after precipitation separation and evaporation drying.
The sodium humate produced by the traditional production method of sodium humate contains some alkali-soluble inorganic impurities, and the purity of the prepared sodium humate is low, so that the use effect of the sodium humate is reduced.
Disclosure of Invention
The invention provides a preparation method of sodium humate, which can remove alkali-soluble inorganic impurities in the sodium humate through acid precipitation treatment and purify the sodium humate, thereby improving the purity of the sodium humate and further improving the use effect of the sodium humate.
In order to solve the technical problems, the invention provides the following technical scheme:
the invention provides a preparation method of sodium humate, which comprises the following raw materials in parts by weight: 1-1.5 parts of raw material coal, 0.12-0.15 part of sodium hydroxide, 10-20 parts of process water and 0.01-0.05 part of sulfuric acid.
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: preparing a sodium hydroxide solution with the concentration of 1% by taking a proper amount of sodium hydroxide and process water;
s3: adding crushed raw material coal and sodium hydroxide solution into a reactor, stirring and leaching for 35-45min at 85-95 ℃;
s4: 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;
s5: adding a proper amount of sulfuric acid into the clear solution for acid precipitation, precipitating sodium humate from the solution in a gel state, and settling the mixture for 24 hours to allow the mixture to settle and separate automatically;
s6: separating to remove the upper layer acid water, and cleaning the precipitate with clear water for 2-3 times;
s7: drying the precipitate to obtain sodium humate;
s8: putting the dried sodium humate into a pot, filling water in the pot, wherein the mass ratio of the sodium humate to the water is 1:360, adding alkali into the pot, adjusting the pH value to be 8-8.5, boiling for 15 minutes, and standing for 72 hours;
s9: and taking out the high-purity sodium humate solution, putting the high-purity sodium humate solution in a clean pot for concentration, and drying in the sun to obtain the high-purity sodium humate.
As a preferable technical scheme of the invention, the raw material coal is weathered coal or lignite.
In a preferred embodiment of the present invention, the acid precipitation may be carried out by using hydrochloric acid in addition to sulfuric acid.
As a preferred technical scheme of the invention, the alkali in the step of purifying the sodium humate is sodium hydroxide.
The invention has the following beneficial effects:
the method can remove alkali soluble inorganic impurities in the sodium humate through acid precipitation treatment, and can purify the sodium humate, so that the purity of the sodium humate can be improved, and the use effect of the sodium humate 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 sodium humate, which comprises the following raw materials in parts by weight: 1-1.5 parts of raw material coal, 0.12-0.15 part of sodium hydroxide, 10-20 parts of process water and 0.01-0.05 part of sulfuric acid.
The preparation method comprises the following specific steps:
s1: crushing the raw material coal to 20-60 meshes by a crusher;
s2: preparing a sodium hydroxide solution with the concentration of 1% by taking a proper amount of sodium hydroxide and process water;
s3: adding crushed raw material coal and sodium hydroxide solution into a reactor, stirring and leaching for 35-45min at 85-95 ℃;
s4: 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;
s5: adding a proper amount of sulfuric acid into the clear solution for acid precipitation, precipitating sodium humate from the solution in a gel state, and settling the mixture for 24 hours to allow the mixture to settle and separate automatically;
s6: separating to remove the upper layer acid water, and cleaning the precipitate with clear water for 2-3 times;
s7: drying the precipitate to obtain sodium humate;
s8: putting the dried sodium humate into a pot, filling water in the pot, wherein the mass ratio of the sodium humate to the water is 1:360, adding alkali into the pot, adjusting the pH value to be 8-8.5, boiling for 15 minutes, and standing for 72 hours;
s9: and taking out the high-purity sodium humate solution, putting the high-purity sodium humate solution in a clean pot for concentration, and drying in the sun to obtain the high-purity sodium humate.
The method can remove alkali soluble inorganic impurities in the sodium humate through acid precipitation treatment, and can purify the sodium humate, so that the purity of the sodium humate can be improved, and the use effect of the sodium humate 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.
Claims (5)
1. The preparation method of the sodium humate is characterized in that the raw materials and the parts by weight required for preparing the sodium humate are as follows: 1-1.5 parts of raw material coal, 0.12-0.15 part of sodium hydroxide, 10-20 parts of process water and 0.01-0.05 part of sulfuric acid.
2. The preparation method of sodium 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: removing a proper amount of sodium hydroxide and process water to prepare a sodium hydroxide solution with the concentration of 1%;
s3: adding crushed raw material coal and sodium hydroxide solution into a reactor, stirring and leaching for 35-45min at 85-95 ℃;
s4: 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;
s5: adding a proper amount of sulfuric acid into the clear solution for acid precipitation, precipitating sodium humate from the solution in a gel state, and settling the mixture for 24 hours to allow the mixture to settle and separate automatically;
s6: separating to remove the upper layer acid water, and cleaning the precipitate with clear water for 2-3 times;
s7: drying the precipitate to obtain sodium humate;
s8: putting the dried sodium humate into a pot, filling water in the pot, wherein the mass ratio of the sodium humate to the water is 1:360, adding alkali into the pot, adjusting the pH value to be 8-8.5, boiling for 15 minutes, and standing for 72 hours;
s9: and taking out the high-purity sodium humate solution, putting the high-purity sodium humate solution in a clean pot for concentration, and drying in the sun to obtain the high-purity sodium humate.
3. The method for preparing sodium humate according to claim 2, wherein the raw material coal is weathered coal or lignite.
4. The method for preparing sodium humate as claimed in claim 2, wherein the acidification is carried out by using hydrochloric acid in addition to sulfuric acid.
5. The method for preparing sodium humate as claimed in claim 2, wherein the alkali in the step of purifying sodium humate is sodium hydroxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011361305.7A CN112442189A (en) | 2020-11-27 | 2020-11-27 | Preparation method of sodium humate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011361305.7A CN112442189A (en) | 2020-11-27 | 2020-11-27 | Preparation method of sodium humate |
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| CN112442189A true CN112442189A (en) | 2021-03-05 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011361305.7A Pending CN112442189A (en) | 2020-11-27 | 2020-11-27 | Preparation method of sodium humate |
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| Country | Link |
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| CN (1) | CN112442189A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115624568A (en) * | 2022-07-28 | 2023-01-20 | 萍乡市红土地腐植酸有限公司 | A kind of fulvic acid and preparation method thereof |
| CN115991881A (en) * | 2022-05-05 | 2023-04-21 | 山东金科力电源科技有限公司 | Humic acid iron removing method |
| CN116253900A (en) * | 2023-03-29 | 2023-06-13 | 山东利特纳米技术有限公司 | Preparation method of high-purity humic acid |
| CN116874813A (en) * | 2023-07-25 | 2023-10-13 | 黑龙江龙兴国际资源开发集团有限公司 | A process for extracting humic acid from lignite |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2150484C1 (en) * | 1999-04-21 | 2000-06-10 | Разумов Виктор Иванович | Method of preparing sodium humate |
| CN103549144A (en) * | 2013-10-21 | 2014-02-05 | 呼和浩特市亿羊达生物科技有限责任公司 | Rare earth and sodium humate compound feed additive and preparation method thereof |
| CN105153434A (en) * | 2015-09-09 | 2015-12-16 | 杨晓斌 | Process for extracting humic acid from coarse slime |
| CN111171334A (en) * | 2020-01-21 | 2020-05-19 | 广西大学 | Method for preparing sodium humate from high-calcium magnesium ore source |
-
2020
- 2020-11-27 CN CN202011361305.7A patent/CN112442189A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2150484C1 (en) * | 1999-04-21 | 2000-06-10 | Разумов Виктор Иванович | Method of preparing sodium humate |
| CN103549144A (en) * | 2013-10-21 | 2014-02-05 | 呼和浩特市亿羊达生物科技有限责任公司 | Rare earth and sodium humate compound feed additive and preparation method thereof |
| CN105153434A (en) * | 2015-09-09 | 2015-12-16 | 杨晓斌 | Process for extracting humic acid from coarse slime |
| CN111171334A (en) * | 2020-01-21 | 2020-05-19 | 广西大学 | Method for preparing sodium humate from high-calcium magnesium ore source |
Non-Patent Citations (1)
| Title |
|---|
| 吴仁儒: "腐植酸钠的提取及提纯", 《景德镇高专学报》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115991881A (en) * | 2022-05-05 | 2023-04-21 | 山东金科力电源科技有限公司 | Humic acid iron removing method |
| CN115991881B (en) * | 2022-05-05 | 2024-02-27 | 山东金科力电源科技有限公司 | Humic acid iron removing method |
| CN115624568A (en) * | 2022-07-28 | 2023-01-20 | 萍乡市红土地腐植酸有限公司 | A kind of fulvic acid and preparation method thereof |
| CN116253900A (en) * | 2023-03-29 | 2023-06-13 | 山东利特纳米技术有限公司 | Preparation method of high-purity humic acid |
| CN116874813A (en) * | 2023-07-25 | 2023-10-13 | 黑龙江龙兴国际资源开发集团有限公司 | A process for extracting humic acid from lignite |
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