CN110183682A - A kind of method that lignite thermal oxide improves Humic Acid Production Rate - Google Patents
A kind of method that lignite thermal oxide improves Humic Acid Production Rate Download PDFInfo
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- CN110183682A CN110183682A CN201910418066.5A CN201910418066A CN110183682A CN 110183682 A CN110183682 A CN 110183682A CN 201910418066 A CN201910418066 A CN 201910418066A CN 110183682 A CN110183682 A CN 110183682A
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- China
- Prior art keywords
- humic acid
- lignite
- thermal oxide
- production rate
- coal sample
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- 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 title claims abstract description 35
- 239000004021 humic acid Substances 0.000 title claims abstract description 35
- 239000003077 lignite Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- 239000003245 coal Substances 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000706 filtrate Substances 0.000 claims abstract description 15
- 239000001301 oxygen Substances 0.000 claims abstract description 15
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 15
- 239000003513 alkali Substances 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 239000012153 distilled water Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 230000003647 oxidation Effects 0.000 claims abstract description 4
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 4
- 230000001376 precipitating effect Effects 0.000 claims abstract description 4
- 239000000047 product Substances 0.000 claims abstract description 3
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 claims description 10
- 229940048086 sodium pyrophosphate Drugs 0.000 claims description 10
- 235000019818 tetrasodium diphosphate Nutrition 0.000 claims description 10
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims 1
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims 1
- 229910001948 sodium oxide Inorganic materials 0.000 claims 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 35
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 8
- 239000013049 sediment Substances 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 3
- 239000000284 extract Substances 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 235000002918 Fraxinus excelsior Nutrition 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000002956 ash Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 229910001882 dioxygen Inorganic materials 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000035558 fertility Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07G—COMPOUNDS OF UNKNOWN CONSTITUTION
- C07G1/00—Lignin; Lignin derivatives
-
- 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
Landscapes
- 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)
- Compounds Of Unknown Constitution (AREA)
Abstract
The present invention discloses a kind of method that lignite thermal oxide improves Humic Acid Production Rate, and this method carries out deliming processing to lignite first, is then rinsed and filtered using distilled water, until without Cl in filtrate‑In the presence of so dry that dry coal sample；Dry coal sample is placed in 100 ~ 240 DEG C, carried out thermal oxide 5 ~ 10 days under oxygen and/or air conditions, it then takes out and is cooled to room temperature, oxidation product mixed alkali liquor 1.5 ~ 2.5 h of alkali carries under 80 ~ 100 DEG C, stirring, mixed liquor after reaction is filtered, filtrate adjusts pH to 1 ~ 2 using the concentrated sulfuric acid, it staticly settles, is centrifuged, up to humic acid after precipitating drying；The method of the present invention solves the problems, such as China's lignite low energy source utilization rate；The yield of humic acid is improved, provides possibility for the extensive use of humic acid.
Description
Technical field
The present invention relates to the production technical fields that lignite in coal chemical industry extracts humic acid, and in particular to a kind of lignite thermal oxide
The method for improving Humic Acid Production Rate.
Background technique
The coal resources reserves in China are abundant, and wherein the content of lignite accounts for the 13% of coal gross reserves, and lignite is a kind of low
Rank coal, it has the features such as moisture content is high, volatile matter is high, and activity is good, and phosphorus content is few, content of ashes is high, calorific value is low, at present at me
State is mainly used as boiler oil and the raw material as power plants generating electricity etc., but since lignite burning is insufficient, conversion ratio is lower,
So as to cause the waste of the energy, while serious pollution is caused to environment with more by-product in lignite burning.
Therefore, very important is just become to the research of lignite.The main component of lignite is humic acid, and soil can be enhanced in this substance
Fertility, improve the physicochemical property of soil, promote the production of crops, its utility value is significantly larger than the direct combustion zone of lignite
The value come.Meanwhile greenhouse effects are reduced using the main component of lignite (humic acid).In addition to this, humic acid medicine with
And also have been widely used in some minerals processing industry productions.So extracting humic acid from lignite and being applied to it
It is necessary, has very important significance to the utilization rate for improving China's lignite.Therefore, the yield of humic acid is improved
It is very important.
The extracting method of humic acid mainly has lye extraction at present, and acid solution is extracted, and microbial degradation method extracts, and neutral salt mentions
It follows the example of, most common method is that lye extracts, but coal sample is directly carried out lye extraction, and yield is not high, generally 10 ~
40 %, which greatly limits the applications of humic acid.
Summary of the invention
In view of the problems of the existing technology and insufficient, the present invention provides a kind of lignite thermal oxide and improves Humic Acid Production Rate
Method, it is intended to solve the problems, such as that lignite extraction Humic Acid Production Rate is lower, be humic acid in agricultural, medical, industrial application mentions
For higher value, and realize environmental protection.
The method of the present invention is to carry out deliming processing to lignite first, is then rinsed and is filtered using distilled water, until
Without Cl in filtrate-In the presence of so dry that dry coal sample；Will dry coal sample be placed in 100 ~ 240 DEG C, under oxygen and/or air conditions into
Row thermal oxide 5 ~ 10 days, then take out and be cooled to room temperature, oxidation product mixed alkali liquor 80 ~ 100 DEG C, stirring under alkali carries 1.5 ~
2.5 h filter the mixed liquor after reaction, and filtrate adjusts pH to 1 ~ 2 using the concentrated sulfuric acid, staticly settle, and are centrifuged, and precipitating is dried
Up to humic acid after dry.
The deliming processing is using HCI:HF:H2O volume ratio is the HCI-HF-H of 2:3:52O mixed liquor is right at 90 DEG C
Lignite handles 1.5 h.
The centrifugation is carried out at 6000 ~ 8000 r/min.
The oxygen mix with air in use, the volume ratio of oxygen and air be 0.2 ~ 0.5, oxygen concentration 99.9%.
It is obtained that the mixed alkali liquor is that sodium hydroxide and the sodium pyrophosphate ratio of 7:15 ~ 2:3 in mass ratio are dissolved in water.
The beneficial effects of the present invention are:
1, in the method for the present invention, lignite is China's energy resources abundant, and source is than wide.Its main component is utilized and is met
Using energy source and environmental protection theme；
2, in the method for the present invention, lignite is China's energy resources abundant, carries out research and benefit to its main component (humic acid)
With meeting using energy source and environmental protection theme；
3, in the method for the present invention, the method for improving Humic Acid Production Rate using humic acid thermal oxide, oxidation process is easy to operate, gained
The yield of humic acid improves 10 ~ 40%；
4, in the method for the present invention, the oxidizing atmosphere of use is air and oxygen, and air source is cheap and easy to get, and oxygen is high purity oxygen
Gas.
Specific embodiment
Below by embodiment, invention is further described in detail, but the scope of the present invention is not limited in described
Hold.
Embodiment 1: HCI-HF-H is used2O mixed liquor (HCI:HF:H2O volume ratio be 2:3:5) at 90 DEG C to lignite into
Row 1.5 h of processing, are then rinsed and are filtered using distilled water, using AgNO3Solution detects filtrate, until detection
Into filtrate without Cl-In the presence of；3h is dried in 60 DEG C of drying box to get dry coal sample is arrived；Dry coal sample is placed in again
100 DEG C, carry out thermal oxide 10 days under air atmosphere, then take out and be cooled to room temperature, with the mixing of sodium hydroxide and sodium pyrophosphate
Lye (sodium hydroxide and the sodium pyrophosphate ratio of 7:15 in mass ratio be dissolved in water obtained) carries out alkali carries under 80 DEG C, stirring
2.5 h filter the mixed liquor after reaction, filtrate are poured into beaker and with the concentrated sulfuric acid tune pH to 1 of 3 mol/L, stand
Precipitating；It is centrifuged under 8000r/min revolving speed, takes supernatant liquor, lower sediment is dried to obtain humic acid；
The yield of gained humic acid improves 10.12 %.
The feature coal sample of this experiment is Yunnan lignite (YN), and Industrial Analysis and elemental analysis are shown in Table 1；
Table 1: the Industrial Analysis and elemental analysis of coal sample
。
Embodiment 2: HCI-HF-H is used2O mixed liquor (HCI:HF:H2O volume ratio be 2:3:5) at 90 DEG C to lignite into
Row 1.5 h of processing, are then rinsed and are filtered using distilled water, using AgNO3Solution detects filtrate, until detection
Into filtrate without Cl-In the presence of；3h is dried in 60 DEG C of drying box to get dry coal sample is arrived；Dry coal sample is placed in again
180 DEG C, (volume ratio of oxygen and air is 0.2) carries out thermal oxide 8 days under the mixed atmosphere of oxygen and air, then take out cold
But to room temperature, with the mixed alkali liquor of sodium hydroxide and sodium pyrophosphate, (sodium hydroxide and the sodium pyrophosphate ratio of 1:2 in mass ratio are molten
Solution is made in water) 2.0 h of alkali carries is carried out under 85 DEG C, stirring, the mixed liquor after reaction is filtered, filtrate is poured into burning
Cup and with the concentrated sulfuric acid tune pH to 1 of 3 mol/L, staticly settles；It is centrifuged under 7000r/min revolving speed, takes upper layer clear
Liquid is dried lower sediment to obtain humic acid；The yield of gained humic acid improves 15.68 %.
The feature coal sample of this experiment is Yunnan lignite, with embodiment 1.
Embodiment 3: HCI-HF-H is used2O mixed liquor (HCI:HF:H2O volume ratio be 2:3:5) at 90 DEG C to lignite into
Row 1.5 h of processing, are then rinsed and are filtered using distilled water, using AgNO3Solution detects filtrate, until detection
Into filtrate without Cl-In the presence of；3h is dried in 60 DEG C of drying box to get dry coal sample is arrived；Dry coal sample is placed in again
200 DEG C, (volume ratio of oxygen and air is 0.5) carries out thermal oxide 6 days under the mixed atmosphere of oxygen and air, then take out cold
But to room temperature, with the mixed alkali liquor of sodium hydroxide and sodium pyrophosphate, (sodium hydroxide and the sodium pyrophosphate ratio of 2:3 in mass ratio are molten
Solution is made in water) alkali carries 1.5h is carried out under 90 DEG C, stirring, the mixed liquor after reaction is filtered, filtrate is poured into burning
Cup and with the concentrated sulfuric acid tune pH to 1.5 of 3 mol/L, staticly settles；It is centrifuged under 7500r/min revolving speed, takes upper layer
Clear liquid is dried lower sediment to obtain humic acid；The yield of gained humic acid improves 25.85%.
The feature coal sample of this experiment is Yunnan lignite, with embodiment 1.
Embodiment 4: HCI-HF-H is used2O mixed liquor (HCI:HF:H2O volume ratio be 2:3:5) at 90 DEG C to lignite into
Row 1.5 h of processing, are then rinsed and are filtered using distilled water, using AgNO3Solution detects filtrate, until detection
Into filtrate without Cl-In the presence of；3h is dried in 60 DEG C of drying box to get dry coal sample is arrived；Dry coal sample is placed in again
240 DEG C, carry out thermal oxide 5 days under air atmosphere, then take out and be cooled to room temperature, with the mixed base of sodium hydroxide and sodium pyrophosphate
Liquid (sodium hydroxide and the sodium pyrophosphate ratio of 7:15 in mass ratio be dissolved in water obtained) carries out alkali carries under 100 DEG C, stirring
1.5h filters the mixed liquor after reaction, filtrate is poured into beaker and with the concentrated sulfuric acid tune pH to 2 of 3 mol/L, and it is heavy to stand
It forms sediment；It is centrifuged under 6000r/min revolving speed, takes supernatant liquor, lower sediment is dried to obtain humic acid；Institute
The yield for obtaining humic acid improves 40 %.
The feature coal sample of this experiment is Yunnan lignite, with embodiment 1.
Claims (3)
1. a kind of method that lignite thermal oxide improves Humic Acid Production Rate, it is characterised in that: deliming processing is carried out to lignite first, with
It is rinsed and filters using distilled water afterwards, until without Cl in filtrate-In the presence of so dry that dry coal sample；Dry coal sample is placed in
It is carried out thermal oxide 5 ~ 10 days under 100 ~ 240 DEG C, oxygen and/or air conditions, then takes out and be cooled to room temperature, oxidation product is used mixed
Lye 1.5 ~ 2.5 h of alkali carries under 80 ~ 100 DEG C, stirring is closed, the mixed liquor after reaction is filtered, filtrate uses the concentrated sulfuric acid
PH to 1 ~ 2 is adjusted, is staticly settled, is centrifuged, up to humic acid after precipitating drying.
2. the method that lignite thermal oxide improves Humic Acid Production Rate according to claim 1, it is characterised in that: oxygen and air are mixed
Close in use, the volume ratio of oxygen and air be 0.2 ~ 0.5, oxygen concentration 99.9%.
3. the method that lignite thermal oxide improves Humic Acid Production Rate according to claim 1, it is characterised in that: mixed alkali liquor is hydrogen
Sodium oxide molybdena and the sodium pyrophosphate ratio of 7:15 ~ 2:3 in mass ratio are dissolved in water obtained.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910418066.5A CN110183682A (en) | 2019-05-20 | 2019-05-20 | A kind of method that lignite thermal oxide improves Humic Acid Production Rate |
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|---|---|---|---|
| CN201910418066.5A CN110183682A (en) | 2019-05-20 | 2019-05-20 | A kind of method that lignite thermal oxide improves Humic Acid Production Rate |
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| CN110183682A true CN110183682A (en) | 2019-08-30 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111560121A (en) * | 2020-04-03 | 2020-08-21 | 安徽工业大学 | Preparation method of modified lignite humic acid water reducer |
| CN114957702A (en) * | 2022-04-26 | 2022-08-30 | 常州大学 | Preparation method of high-activity humic acid |
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|---|---|---|---|---|
| WO2006000073A1 (en) * | 2004-06-23 | 2006-01-05 | Bioz Agri Products Inc. | Method for extracting fulvic acid molecules |
| CN103319324A (en) * | 2012-03-20 | 2013-09-25 | 北京化工大学 | Method for preparing benzene carboxylic acids by alkali-oxygen oxidation of brown coals |
| CN107417929A (en) * | 2017-07-26 | 2017-12-01 | 湖南科技大学 | A kind of method that lignite catalysis oxidation improves Humic Acid Production Rate |
-
2019
- 2019-05-20 CN CN201910418066.5A patent/CN110183682A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006000073A1 (en) * | 2004-06-23 | 2006-01-05 | Bioz Agri Products Inc. | Method for extracting fulvic acid molecules |
| CN103319324A (en) * | 2012-03-20 | 2013-09-25 | 北京化工大学 | Method for preparing benzene carboxylic acids by alkali-oxygen oxidation of brown coals |
| CN107417929A (en) * | 2017-07-26 | 2017-12-01 | 湖南科技大学 | A kind of method that lignite catalysis oxidation improves Humic Acid Production Rate |
Non-Patent Citations (3)
| Title |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111560121A (en) * | 2020-04-03 | 2020-08-21 | 安徽工业大学 | Preparation method of modified lignite humic acid water reducer |
| CN111560121B (en) * | 2020-04-03 | 2022-03-04 | 安徽工业大学 | Preparation method of modified lignite humic acid water reducer |
| CN114957702A (en) * | 2022-04-26 | 2022-08-30 | 常州大学 | Preparation method of high-activity humic acid |
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Application publication date: 20190830 |