CN104448341A - Extraction method of water-soluble humic acid - Google Patents
Extraction method of water-soluble humic acid Download PDFInfo
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- CN104448341A CN104448341A CN201410593571.0A CN201410593571A CN104448341A CN 104448341 A CN104448341 A CN 104448341A CN 201410593571 A CN201410593571 A CN 201410593571A CN 104448341 A CN104448341 A CN 104448341A
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- humic acid
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- fulvo acid
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Abstract
The invention discloses an extraction method of water-soluble humic acid. The method is characterized by comprising the steps of pickling raw humic acid powder to remove humic acid containing calcium ions and magnesium ions; adding sodium hydroxide for alkaline extraction; oxidizing with hydrogen peroxide; and enabling sodium hydroxide and hydrogen peroxide to react for 60 to 90min under a temperature of 80 to 90 DEG C and agitating at the same time until the final solution is at pH of 8 to 10 so as to obtain water-soluble humic acid. After being added with water-soluble humic acid produced by the method, the compound fertilizer is outstanding in color and luster, high in strength, applicable to topdressing of different crops at different seasons, and wide in applicable scope; nutrient elements integrate the functions of quick acting, long lasting and synergia, so that the effects of improving the quality of the crops, inhibiting soil-borne disease, improving stress resistance of the crops and prompting early-maturing of the crops can be realized; the effect of fertilizer on increasing yield is obvious, and the yield per mu is increased by more than 20% on year-on-year basis.
Description
Technical field
The present invention relates to the extraction of fulvo acid in raw coal, especially a kind of extracting method of fulvo acid.
Background technology
At present, acidization, alkalization method and biological fermentation process are mainly taked in the activation of humic acids, the method activated that wherein alkalizes is applied more, the alkaline matter of activation humic acids is mainly potassium hydroxide, salt of wormwood, sodium bicarbonate, saleratus, sodium hydroxide, ammoniacal liquor etc., but it is high, not environmentally to there is cost in these alkaline matters, and there is the shortcomings such as activator is single, fulvo acid extraction yield is low, be unfavorable for realizing suitability for industrialized production.
Summary of the invention
The object of the invention is for overcoming above-mentioned the deficiencies in the prior art, a kind of extracting method of fulvo acid is provided, the fulvo acid extraction yield adopting present method to obtain is high, biological activity is strong, make the utilization ratio of the organic matter of fertilizer high, production method is simple, cost is low, is easy to realize suitability for industrialized production.
For achieving the above object, the present invention adopts following technical proposals:
An extracting method for fulvo acid, first carries out pickling to the former powder of humic acids, the humic acids of removing containing calcium, magnesium ion; First hydro-oxidation sodium carries out alkali and carries, and be then oxidized with hydrogen peroxide, the two reacts 60-90min after adding under 80-90 DEG C of condition, stirs simultaneously, is 8-10, obtains fulvo acid to final solution pH value.
The particle diameter of the former powder of described humic acids is 80 orders.
Described pickling adopts volume fraction to be the sulphuric acid soln of 2%-3%.
What described alkali proposed employing is volume fraction is the sodium hydroxide solution of 4-5%.
The hydrogen peroxide of to be volume fraction the be 30-35% that described oxidation adopts.
The volume ratio of described sodium hydroxide solution and hydrogen peroxide is 3:1.
The speed of described stirring is 500-600r/min.
Preferably, final solution pH value is 8.5-9.5.
The invention has the beneficial effects as follows,
1. the present invention is by activating humic acids, improves the content of fulvo acid in humic acids, and fulvo acid extraction yield can reach more than 90%, adds in composite fertilizer and can improve utilization ratio organic in fertilizer, bring up to about 80% by 50%;
2. after humic acids activation, fulvo acid has the effect improving potential nutrients in utilization rate of fertilizer and activating soil, and can assist potential nutrients in release soil, make the transformation efficiency of Nitrogen In Soils reach 5%-12%, the transformation efficiency of phosphorus, potassium can reach 6%-13% and 9%-15% respectively;
3., on breeding time shorter crop, humic acids adds the alternative chemical fertilizer of Chemical Mixed Fertilizer and carries out single fertilization, reduces production cost, as on soybean and corn, the compound organic and inorganic fertilizer adding humic acids can disposablely apply as base fertilizer, does not need to topdress, both reduced investment outlay, and saved again and throw work;
4. the humic acids that the present invention produces adds that Chemical Mixed Fertilizer color is good, intensity is large, the use of topdressing of Various Seasonal, different crops can be adapted to, suitability is wide, its nutritive element integrates quick-acting, long-acting, synergy, has the effect improving quality of agricultural product, suppress soil-borne disease, strengthen crop anti-adversity, promote crop precocity; Fertilizer effect of increasing production is obvious, on year-on-year basis crop mu volume increase more than 20%;
5. the adjustable liquid-solid ratio of this production method, both directly can add mixed fertile, compound fertilizer system and carry out granulation, again can chelating medium trace element, produced the humic acid liquid fertilizer being rich in medium trace element, was applicable to the leaf dressing of vegetables, fruit tree etc., improve output.
Accompanying drawing explanation
Fig. 1 is schematic flow sheet of the present invention.
Embodiment
Below in conjunction with drawings and Examples, the present invention is further described.
Embodiment 1:
An extracting method for fulvo acid, as shown in Figure 1, adds in reactor by former for humic acids powder, utilize volume fraction be 2% sulphuric acid soln carry out pickling, removing calcium ions and magnesium ions; Add the sodium hydroxide solution that volume fraction is 4%, slowly add the hydrogen peroxide that volume fraction is 30%, carry out being oxidized and alkali is carried, under 80 DEG C of conditions, react 60min, stir simultaneously, rotating speed is 500r/min, be 8 to final solution pH value, obtain fulvo acid.
Embodiment 2:
An extracting method for fulvo acid, as shown in Figure 1, adds in reactor by former for humic acids powder, utilize volume fraction be 3% sulphuric acid soln carry out pickling, removing calcium ions and magnesium ions; Add the sodium hydroxide solution that volume fraction is 5%, and then slowly add the hydrogen peroxide that volume fraction is 35%, carry out being oxidized and alkali is carried, under 90 DEG C of conditions, react 90min, stir simultaneously, rotating speed is 600r/min, be 10 to final solution pH value, obtain fulvo acid.
Embodiment 3:
An extracting method for fulvo acid, as shown in Figure 1, adds in reactor by former for humic acids powder, utilize volume fraction be 2.5% sulphuric acid soln carry out pickling, removing calcium ions and magnesium ions; Add the sodium hydroxide solution that volume fraction is 4.5%, and then slowly add the hydrogen peroxide that volume fraction is 32%, carry out being oxidized and alkali is carried, under 85 DEG C of conditions, react 75min, stir simultaneously, rotating speed is 550r/min, be 9 to final solution pH value, obtain fulvo acid.
(1) weathered coal activates the mensuration of solubility humic acids content in filtrate
The mensuration of humic acids must under strongly acidic conditions, and the oxidation of coal in humic acids could be carbonic acid gas by potassium bichromate, and then could analyze and measure out.What get when adopting HG/T 3278-2011 Sodium salts humic acids rower to measure is solid powdery sample, take the water-soluble humic acid that 0.2 gram of the present embodiment 3 obtains, add the 15ml vitriol oil, obtain filtrate, and the filtrate after activation, stronger owing to presenting alkalescence, the 15ml sulfuric acid added is not enough to provide strongly-acid, so filtrate need be diluted when analyzing activated, namely filtrate 5ml is drawn, be settled in 100ml volumetric flask with distilled water, draw the filtrate after 5ml constant volume again, according to 5.2.4.1 in Sodium salts humic acids rower HG/T 3278-2011, add 70ml water, analyze, determine that the formula calculating solubility humic acids content is as follows simultaneously:
V
0: blank test consumes the numerical value of ferrous ammonium sulphate standard titration solution volume, and unit is milliliter (ml)
V
1: titration test solution consumes the numerical value of ferrous ammonium sulphate standard titration solution volume, and unit is milliliter (ml)
C: the numerical value of ferrous ammonium sulphate concentration of standard solution, unit is mole often liter (mol/L).
0.003: the numerical value of the carbonaceous amount suitable with 1.00ml1.000mol/L l ferrous ammonium sulfate solution, unit is gram every mmole (g/mmol)
0.64: the pure humic acids carbon ratio of Coal rank, weathered coal is 0.64.
Described weathered coal analytical results:
(2) calculating of weathered coal extraction yield
Determine in this activating process as follows with the weathered coal extraction yield calculation formula of weathered coal raw material extraction solubility humic acids:
As calculated, the embodiment of the present invention 3 weathered coal extraction yield is 88.91%.
Claims (8)
1. an extracting method for fulvo acid, is characterized in that, first carries out pickling to the former powder of humic acids, the humic acids of removing containing calcium, magnesium ion; First hydro-oxidation sodium carries out alkali and carries, and be then oxidized with hydrogen peroxide, the two reacts 60-90min after adding under 80-90 DEG C of condition, stirs simultaneously, is 8-10, obtains fulvo acid to final solution pH value.
2. the extracting method of a kind of fulvo acid as claimed in claim 1, is characterized in that, the particle diameter of the former powder of described humic acids is 80 orders.
3. the extracting method of a kind of fulvo acid as claimed in claim 1, is characterized in that, described pickling adopts volume fraction to be the sulphuric acid soln of 2-3%.
4. the extracting method of a kind of fulvo acid as claimed in claim 1, is characterized in that, what described alkali proposed employing is volume fraction is the sodium hydroxide solution of 4-5%.
5. the extracting method of a kind of fulvo acid as claimed in claim 1, is characterized in that, the hydrogen peroxide of to be volume fraction the be 30-35% that described oxidation adopts.
6. the extracting method of a kind of fulvo acid as claimed in claim 1, is characterized in that, the volume ratio of described sodium hydroxide solution and hydrogen peroxide is 3:1.
7. the extracting method of a kind of fulvo acid as claimed in claim 1, is characterized in that, the speed of described stirring is 500-600r/min.
8. the extracting method of a kind of fulvo acid as claimed in claim 1, is characterized in that, final solution pH value is 8.5-9.5.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104861173A (en) * | 2015-06-02 | 2015-08-26 | 福建师范大学福清分校 | Method for extracting fulvic acid |
| CN105037748A (en) * | 2015-09-16 | 2015-11-11 | 中国环境科学研究院 | Grading extraction method of humic acid in frond |
| CN105111463A (en) * | 2015-08-23 | 2015-12-02 | 唐山炬能节能科技有限公司 | Method for producing humic acid by treating biomass before steam explosion |
| CN105111464A (en) * | 2015-09-16 | 2015-12-02 | 中国环境科学研究院 | Method for graded extraction of humic acid in soil |
| CN106279717A (en) * | 2016-11-09 | 2017-01-04 | 泸天化（集团）有限责任公司 | The preparation method of humic acid high extraction in a kind of low-order coal |
| CN109400349A (en) * | 2018-11-09 | 2019-03-01 | 中国农业科学院农业资源与农业区划研究所 | A kind of preparation method of the Humic acid synergistic carrier of the urea suitable for rice top dressing |
| 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 |
| CN112011066A (en) * | 2019-05-29 | 2020-12-01 | 三通生物工程（潍坊）有限公司 | Production process of high-purity humic acid |
-
2014
- 2014-10-29 CN CN201410593571.0A patent/CN104448341A/en not_active Withdrawn
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104861173A (en) * | 2015-06-02 | 2015-08-26 | 福建师范大学福清分校 | Method for extracting fulvic acid |
| CN105111463A (en) * | 2015-08-23 | 2015-12-02 | 唐山炬能节能科技有限公司 | Method for producing humic acid by treating biomass before steam explosion |
| CN105037748A (en) * | 2015-09-16 | 2015-11-11 | 中国环境科学研究院 | Grading extraction method of humic acid in frond |
| CN105111464A (en) * | 2015-09-16 | 2015-12-02 | 中国环境科学研究院 | Method for graded extraction of humic acid in soil |
| CN106279717A (en) * | 2016-11-09 | 2017-01-04 | 泸天化（集团）有限责任公司 | The preparation method of humic acid high extraction in a kind of low-order coal |
| CN109400349A (en) * | 2018-11-09 | 2019-03-01 | 中国农业科学院农业资源与农业区划研究所 | A kind of preparation method of the Humic acid synergistic carrier of the urea suitable for rice top dressing |
| CN112011066A (en) * | 2019-05-29 | 2020-12-01 | 三通生物工程（潍坊）有限公司 | Production process of high-purity humic acid |
| CN112011066B (en) * | 2019-05-29 | 2022-04-01 | 三通生物工程（潍坊）有限公司 | Production process of high-purity humic acid |
| 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 |
| CN110358110B (en) * | 2019-07-24 | 2021-07-27 | 西安集佰侬生物科技有限公司 | Preparation method of mineral source potassium fulvate |
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Application publication date: 20150325 |