CN104231279A - Method of extracting humic acid from peat - Google Patents
Method of extracting humic acid from peat Download PDFInfo
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- CN104231279A CN104231279A CN201410464584.8A CN201410464584A CN104231279A CN 104231279 A CN104231279 A CN 104231279A CN 201410464584 A CN201410464584 A CN 201410464584A CN 104231279 A CN104231279 A CN 104231279A
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Abstract
The invention relates to the technical fields of comprehensive utilization of peat and humate extraction, and particularly relates to a method of extracting humic acid from peat. By combining spray drying with a centrifugal separation technology, and regulating and controlling the opportunity, the temperature and end point of adding a nitric acid liquid and an alkaline liquid into the peat to extract the humic acid, and controlling the water-washing times and the water-washing time, the humic acid in the peat can be greatly extracted, so that the extraction efficiency of the humic acid is improved, the purity of the humic acid in the humate is increased to over 80%, the humic acid extraction time is shortened, and the humic acid extraction cost is lowered.
Description
Technical field
The present invention relates to mud coal comprehensive utilization, extracted humic acid salt technical field, especially a kind of method of extracted humic acid from mud coal.
Background technology
Humic acids is the larger molecular organics matter that occurring in nature extensively exists, and is widely used in the every field such as Agriculture, forestry And Animal Husbandry, oil, chemical industry, building materials, medical and health, environmental protection, across tens industries.Particularly advocate ecological agriculture construction, pollution-less agriculture production, green food, pollution-free environmentfriendly products etc. now, more make " humic acids " to enjoy high praise, fact proved, life and the existence of the mankind be unable to do without humic acids.
Abroad pay much attention to humic acid substance development and usage, in the U.S., Russia, more to the research of humic acid substance with Japan etc., also a lot of achievement in research is achieved, over nearly 20 years, abroad greater advance is achieved to humic acid substance research agriculturally and Application and Development, become the ecotope that protection and harnessing goes from bad to worse, reduce important means and the raw materials for production of pollution etc., according to the experimental study of USSR (Union of Soviet Socialist Republics), ammonium humate can make grape yield increasing 45%, potato production promoting 45%, vegetable increase production 15%, Japan utilizes nitro humic acid magnesium can make tomato production promoting 13.2%, cucumber production promoting 80.3%, shallot volume increase 20%, Japanese agriculture portion 10% humic acids, the urea of 88% and the 5-chlorophenol of 2% are made into a kind of humic-acid kind mixed fertilizer containing weedicide, it is except having distinctive fertilizer efficiency, weeds can also be removed safely and effectively.
The research of humic acid substance is more late in China's starting, along with domestic academic is constantly paid close attention to humic acid substance research, Economic and Trade Commission of country has set up " China Humic Acid TIA " in approval in 1987, be responsible for organization of unity and coordinate national humic acids work, the production that China is having most of provinces and regions of mud and charcoal to be mainly used in humic acid fertilizer, through years of researches on the basis of summing up experience, humic acid fertilizer is furtherd investigate, from production technique, batching, the aspect such as application process and production unit has carried out putting into practice and achieving positive effect, humic acid substance receives increasing attention and concern as the soil improvement agent of excellent property and the water conditioner of processing environment pollution.
Under biological soil sand desert survey place, Chinese Academy of Sciences Xinjiang International Cooperation cause group subsidizes, jointly create desert transformation laboratory, mainly through mud coal and biological control measure, make desert Environment from soil to moisture and rate of vegetation all there occurs larger change, continue to propose in research to utilize mud and charcoal afforestation desert that global environment can be made to improve, for the husky alkali area Development of farming and animal husbandry accounting for the area in the whole world 1/3 opens new way.
Because humic acids can carry out neutralization reaction with alkali, make water-fast humic acids be converted into humate soluble in water, thus the preparation method of humate mainly alkali-soluble acid analysis method extract.
But, traditional production mainly utilizes sodium hydroxide and potassium hydroxide neutralization reaction, then Precipitation, last artificial airing, although workshop-based production technique is simple, input cost is little, but its humate purity produced is low, and the time of producing is long, causes a large amount of wastes to resource, also do not utilize industrialization to produce, and the technical literature of the production humic acid of batch production have not been reported from mud coal.
Summary of the invention
In order to solve the above-mentioned technical problem existed in prior art, the invention provides a kind of method of extracted humic acid from mud coal, it is with short production cycle, humic acid extraction rate reached in mud coal is to more than 70%, the purity of the humic acid extracted more than 80%, for humic acid produce and Application and Development has wide sight.
Be achieved particular by following technical scheme:
A method for extracted humic acid from mud coal, comprises the following steps:
(1) mud coal pre-treatment: after excavating out by mud coal, is placed in Indoor Natural environment, deposits 3-5 days, adjusts and detects mud pit ash and moisture, stand-by;
(2) pulverize: by step 1) adjust and mud coal after detecting, make mud pit ash <20% and moisture <30% time, then peat dust is broken to 38-42 order, acquisition coal dust, stand-by;
(3) being oxidized: by step 2) to add concentration be in the salpeter solution of 40-45% for the coal dust that obtains, wherein the ratio of coal dust and salpeter solution is (1-2): (2-3), and its proportioning unit is kg/l; Adjustment temperature is 90-95 DEG C, after reaction 5-8min, stand-by;
(4) wash: by step 3) reaction terminate after material adopt clear water wash 1-2 time, acquisition suspension, stand-by;
(5) filtering: by step 4) suspension that obtains of washing adopts flame filter press to filter, and obtain filtrate, and to adjust filtrate moisture content is 55%, then adds alkali wherein, when adjustment pH value is 5-6, stand-by;
(6) centrifugation: again by step 5) stand-by material is placed in separating centrifuge and carries out centrifugation 0.5-4h, and the rotating speed of whizzer is 1000-1300r/min, obtains centrifugate, stand-by;
(7) dry: by step 6) obtain centrifugate spray drying treatment in spray-drier, inlet temperature during spraying dry is 500-600 DEG C, and temperature out is 40-60 DEG C, obtains dried powder, stand-by;
(8) thunder covers crushing packing: by step 7) powder that completes of drying is placed in thunder and covers pulverizer and carry out being ground into 130-140 order, obtain the finished product humate that dry product contains humic acid 80%, and its specification of wrapping according to 50kg/ is packed.
Described alkali is the one in potassium hydroxide, sodium hydroxide.
Described paper mill wastewater is 30-45%.
It is that 4r3216 thunder covers pulverizer that described thunder covers pulverizer.
The length of described spray-drier is 13-14m.
Described spray-drier, its inlet temperature and temperature out are successively decreased according to 3 DEG C/unit length, and wherein unit length is after spray-drier length is multiplied by 3 DEG C, then divided by the difference of inlet temperature and temperature out.
Compared with prior art, technique effect of the present invention is embodied in:
1. the connected applications of spraying dry and centrifugal separation technique is passed through, adjust simultaneously and control adding opportunity, temperature, add terminal when salpeter solution and alkaline solution add the lixiviate wherein carrying out humic acid, control number of times and the time of washing, make the humic acid in mud coal can by a large amount of extraction processs, and then improve the extraction yield of humic acid, increase the purity of humic acid in humate, its purity is made to reach more than 80%, and shorten the time that humic acid extracts, reduce extraction cost.
2. the filter residue filter cake in the whole process of the present invention all as building materials raw material, without discharging of waste liquid, can have the significant value of environmental protection.
3. the whole technical process that the present invention is directed to the production of high-purity humic acid salt is carried out associating holistic approach and obtains breakthrough, has both obtained highly purified humate product, achieves again the scale up test of humate simultaneously; Make the regulation obtaining humate composite humic acid sodium first class product standard, make water-soluble humic acid butt be more than 80%, insoluble butt is 10%.
Embodiment
Below in conjunction with concrete embodiment, further restriction is done to technical scheme of the present invention, but claimed scope is not only confined to done description.
Embodiment 1
A method for extracted humic acid from mud coal, comprises the following steps:
(1) mud coal pre-treatment: after excavating out by mud coal, is placed in Indoor Natural environment, deposits 3 days, adjusts and detects mud pit ash and moisture, stand-by;
(2) pulverize: by step 1) adjust and mud coal after detecting, make mud pit ash be 20% and moisture is 30% time, then peat dust is broken to 38 orders, acquisition coal dust, stand-by;
(3) being oxidized: by step 2) to add concentration be in the salpeter solution of 40% for the coal dust that obtains, wherein the ratio of coal dust and salpeter solution is 1:2, and its proportioning unit is kg/l; Adjustment temperature is 90 DEG C, after reaction 5min, stand-by;
(4) wash: by step 3) reaction terminate after material adopt clear water wash 1 time, obtain suspension, stand-by;
(5) filtering: by step 4) suspension that obtains of washing adopts flame filter press to filter, and obtain filtrate, and to adjust filtrate moisture content is 55%, then adds alkali wherein, when adjustment pH value is 5, stand-by;
(6) centrifugation: again by step 5) stand-by material is placed in separating centrifuge and carries out centrifugation 0.5h, and the rotating speed of whizzer is 1000r/min, obtains centrifugate, stand-by;
(7) dry: by step 6) obtain centrifugate spray drying treatment in spray-drier, inlet temperature during spraying dry is 500 DEG C, and temperature out is 40 DEG C, obtains dried powder, stand-by;
(8) thunder covers crushing packing: by step 7) powder that completes of drying is placed in thunder and covers pulverizer and carry out being ground into 130 orders, obtains the finished product humate that dry product contains humic acid 80%, and its specification according to 50kg/ bag is packed.
Described alkali is potassium hydroxide, and concentration is 30%.
It is that 4r3216 thunder covers pulverizer that described thunder covers pulverizer.
The length of described spray-drier is 13m.
Described spray-drier, its inlet temperature and temperature out are successively decreased according to 3 DEG C/unit length, and wherein unit length is after spray-drier length is multiplied by 3 DEG C, then divided by the difference of inlet temperature and temperature out.
Embodiment 2
On the basis of embodiment 1, other are all with embodiment 1, and a kind of method of extracted humic acid from mud coal, comprises the following steps:
(1) mud coal pre-treatment: after excavating out by mud coal, is placed in Indoor Natural environment, deposits 5 days, adjusts and detects mud pit ash and moisture, stand-by;
(2) pulverize: by step 1) adjust and mud coal after detecting, make mud pit ash 19% and moisture 25% time, then peat dust is broken to 42 orders, acquisition coal dust, stand-by;
(3) being oxidized: by step 2) to add concentration be in the salpeter solution of 45% for the coal dust that obtains, wherein the ratio of coal dust and salpeter solution is 2:3, and its proportioning unit is kg/l; Adjustment temperature is 95 DEG C, after reaction 8min, stand-by;
(4) wash: by step 3) reaction terminate after material adopt clear water wash 2 times, obtain suspension, stand-by;
(5) filtering: by step 4) suspension that obtains of washing adopts flame filter press to filter, and obtain filtrate, and to adjust filtrate moisture content is 55%, then adds alkali wherein, when adjustment pH value is 6, stand-by;
(6) centrifugation: again by step 5) stand-by material is placed in separating centrifuge and carries out centrifugation 4h, and the rotating speed of whizzer is 1300r/min, obtains centrifugate, stand-by;
(7) dry: by step 6) obtain centrifugate spray drying treatment in spray-drier, inlet temperature during spraying dry is 600 DEG C, and temperature out is 60 DEG C, obtains dried powder, stand-by;
(8) thunder covers crushing packing: by step 7) powder that completes of drying is placed in thunder and covers pulverizer and carry out being ground into 140 orders, obtains the finished product humate that dry product contains humic acid 80%, and its specification according to 50kg/ bag is packed.
Described alkali is sodium hydroxide, and concentration is 45%.
The length of described spray-drier is 14m.
Embodiment 3
On the basis of embodiment 1, other steps are with embodiment 1, and a kind of method of extracted humic acid from mud coal, comprises the following steps:
(1) mud coal pre-treatment: after excavating out by mud coal, is placed in Indoor Natural environment, deposits, 4 days, adjusts and detects mud pit ash and moisture, stand-by;
(2) pulverize: by step 1) adjust and mud coal after detecting, make mud pit ash 15% and moisture 20% time, then peat dust is broken to 40 orders, acquisition coal dust, stand-by;
(3) being oxidized: by step 2) to add concentration be in the salpeter solution of 43% for the coal dust that obtains, wherein the ratio of coal dust and salpeter solution is 3:5, and its proportioning unit is kg/l; Adjustment temperature is 93 DEG C, after reaction 7min, stand-by;
(4) wash: by step 3) reaction terminate after material adopt clear water wash 1 time, obtain suspension, stand-by;
(5) filtering: by step 4) suspension that obtains of washing adopts flame filter press to filter, and obtain filtrate, and to adjust filtrate moisture content is 55%, then adds alkali wherein, when adjustment pH value is 5.5, stand-by;
(6) centrifugation: again by step 5) stand-by material is placed in separating centrifuge and carries out centrifugation 2h, and the rotating speed of whizzer is 1200r/min, obtains centrifugate, stand-by;
(7) dry: by step 6) obtain centrifugate spray drying treatment in spray-drier, inlet temperature during spraying dry is 550 DEG C, and temperature out is 50 DEG C, obtains dried powder, stand-by;
(8) thunder covers crushing packing: by step 7) powder that completes of drying is placed in thunder and covers pulverizer and carry out being ground into 135 orders, obtains the finished product humate that dry product contains humic acid 80%, and its specification according to 50kg/ bag is packed.
Described alkali is potassium hydroxide, and concentration is 40%.
The length of described spray-drier is 13.5m.
Embodiment 4
On the basis of embodiment 1, other are all with embodiment 1, and a kind of method of extracted humic acid from mud coal, comprises the following steps:
(1) mud coal pre-treatment: after excavating out by mud coal, is placed in Indoor Natural environment, deposits 5 days, adjusts and detects mud pit ash and moisture, stand-by;
(2) pulverize: by step 1) adjust and mud coal after detecting, make mud pit ash 18% and moisture 22% time, then peat dust is broken to 39 orders, acquisition coal dust, stand-by;
(3) being oxidized: by step 2) to add concentration be in the salpeter solution of 44% for the coal dust that obtains, wherein the ratio of coal dust and salpeter solution is 1.6:2.5, and its proportioning unit is kg/l; Adjustment temperature is 91 DEG C, after reaction 6min, stand-by;
(4) wash: by step 3) reaction terminate after material adopt clear water wash 2 times, obtain suspension, stand-by;
(5) filtering: by step 4) suspension that obtains of washing adopts flame filter press to filter, and obtain filtrate, and to adjust filtrate moisture content is 55%, then adds alkali wherein, when adjustment pH value is 6, stand-by;
(6) centrifugation: again by step 5) stand-by material is placed in separating centrifuge and carries out centrifugation 3h, and the rotating speed of whizzer is 1100r/min, obtains centrifugate, stand-by;
(7) dry: by step 6) obtain centrifugate spray drying treatment in spray-drier, inlet temperature during spraying dry is 580 DEG C, and temperature out is 42 DEG C, obtains dried powder, stand-by;
(8) thunder covers crushing packing: by step 7) powder that completes of drying is placed in thunder and covers pulverizer and carry out being ground into 135 orders, obtains the finished product humate that dry product contains humic acid 80%, and its specification according to 50kg/ bag is packed.
Described alkali is sodium hydroxide, and concentration is 30-45%.
Test example:
Experimental group, adopt the method for extracted humic acid from mud coal of the embodiment of the present invention 1, embodiment 2, embodiment 3, embodiment 4 to carry out the extraction experiment of humic acid, and measure the acquisition cycle of the humic acid purity in record mud coal in the recovery rate of humic acid, finished product humate product, every t product.
Comparative group, utilize sodium hydroxide and potassium hydroxide neutralization reaction, then Precipitation, the method for last artificial airing carries out the extraction experiment of mud coal humic acid, and measures the acquisition cycle of the humic acid purity in the recovery rate of humic acid in record mud coal, finished product humate product, every t product.
Concrete experimental result is shown in Table 1:
Table 1
Shown by upper table 1 experimental data, the method of extracted humic acid from mud coal of the present invention at least improves 8-13 percentage point than the recovery rate of traditional humic acid production method, the purity of humic acid in finished product product also at least improves 10-13 percentage point, 1 ton of product obtains more than the one times time of cycle time, and then has significant progress.
It is important to point out at this; above embodiment and test example are only limitted to the technique effect that can reach technical scheme of the present invention and concrete operations mode of the present invention is further elaborated and illustrates; so that the understanding of present specification; be not to further restriction of the present invention; the essential characteristics of the non-protruding that those skilled in the art make on this basis and the improvement of non-significant progress, all belong to protection category of the present invention.
Claims (6)
1. the method for extracted humic acid from mud coal, is characterized in that, comprise the following steps:
(1) mud coal pre-treatment: after excavating out by mud coal, is placed in Indoor Natural environment, deposits 3-5 days, adjusts and detects mud pit ash and moisture, stand-by;
(2) pulverize: by step 1) adjust and mud coal after detecting, make mud pit ash <20% and moisture <30% time, then peat dust is broken to 38-42 order, acquisition coal dust, stand-by;
(3) being oxidized: by step 2) to add concentration be in the salpeter solution of 40-45% for the coal dust that obtains, wherein the ratio of coal dust and salpeter solution is (1-2): (2-3), and its proportioning unit is kg/l; Adjustment temperature is 90-95 DEG C, after reaction 5-8min, stand-by;
(4) wash: by step 3) reaction terminate after material adopt clear water wash 1-2 time, acquisition suspension, stand-by;
(5) filtering: by step 4) suspension that obtains of washing adopts flame filter press to filter, and obtain filtrate, and to adjust filtrate moisture content is 55%, then adds alkali wherein, when adjustment pH value is 5-6, stand-by;
(6) centrifugation: again by step 5) stand-by material is placed in separating centrifuge and carries out centrifugation 0.5-4h, and the rotating speed of whizzer is 1000-1300r/min, obtains centrifugate, stand-by;
(7) dry: by step 6) obtain centrifugate spray drying treatment in spray-drier, inlet temperature during spraying dry is 500-600 DEG C, and temperature out is 40-60 DEG C, obtains dried powder, stand-by;
(8) thunder covers crushing packing: by step 7) powder that completes of drying is placed in thunder and covers pulverizer and carry out being ground into 130-140 order, obtain the finished product humate that dry product contains humic acid 80%, and its specification of wrapping according to 50kg/ is packed.
2. the method for extracted humic acid from mud coal as claimed in claim 1, it is characterized in that, described alkali is the one in potassium hydroxide, sodium hydroxide.
3. the method for extracted humic acid from mud coal as claimed in claim 1, it is characterized in that, described paper mill wastewater is 30-45%.
4. the method for extracted humic acid from mud coal as claimed in claim 1, is characterized in that, it is that 4r3216 thunder covers pulverizer that described thunder covers pulverizer.
5. the method for extracted humic acid from mud coal as claimed in claim 1, it is characterized in that, the length of described spray-drier is 13-14m.
6. the method for extracted humic acid from mud coal as claimed in claim 1, it is characterized in that, described spray-drier, its inlet temperature and temperature out are successively decreased according to 3 DEG C/unit length, wherein unit length is after spray-drier length is multiplied by 3 DEG C, then divided by the difference of inlet temperature and temperature out.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105542115A (en) * | 2016-01-22 | 2016-05-04 | 江苏大学 | Preparation method of coal-based humic acid modified waterborne polyurethane composite |
| CN107312183A (en) * | 2017-08-03 | 2017-11-03 | 山西绿能新动力环保科技有限公司 | A kind of environment-friendly production process of nitro humus acid potassium |
| CN107353415A (en) * | 2017-06-27 | 2017-11-17 | 界首市沃土生物科技有限公司 | A kind of method of river silt detritus acid high efficiency extraction |
| CN109627456A (en) * | 2018-12-18 | 2019-04-16 | 大连理工大学 | A kind of method of fulvic acid content in raising lignite |
| CN111171334A (en) * | 2020-01-21 | 2020-05-19 | 广西大学 | Method for preparing sodium humate from high-calcium magnesium ore source |
| CN115819795A (en) * | 2022-12-21 | 2023-03-21 | 神华准能资源综合开发有限公司 | Method for extracting humic acid from residue of acid leaching and aluminum extraction of coal gangue |
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2014
- 2014-09-12 CN CN201410464584.8A patent/CN104231279A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105542115A (en) * | 2016-01-22 | 2016-05-04 | 江苏大学 | Preparation method of coal-based humic acid modified waterborne polyurethane composite |
| CN105542115B (en) * | 2016-01-22 | 2018-01-16 | 江苏大学 | A kind of preparation method of the humic acid modified Waterborne PU Composite of coal base |
| CN107353415A (en) * | 2017-06-27 | 2017-11-17 | 界首市沃土生物科技有限公司 | A kind of method of river silt detritus acid high efficiency extraction |
| CN107312183A (en) * | 2017-08-03 | 2017-11-03 | 山西绿能新动力环保科技有限公司 | A kind of environment-friendly production process of nitro humus acid potassium |
| CN109627456A (en) * | 2018-12-18 | 2019-04-16 | 大连理工大学 | A kind of method of fulvic acid content in raising lignite |
| CN111171334A (en) * | 2020-01-21 | 2020-05-19 | 广西大学 | Method for preparing sodium humate from high-calcium magnesium ore source |
| CN115819795A (en) * | 2022-12-21 | 2023-03-21 | 神华准能资源综合开发有限公司 | Method for extracting humic acid from residue of acid leaching and aluminum extraction of coal gangue |
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