KR101967061B1 - Fulvic acid extracting method using electro-analysised water - Google Patents

Abstract

The present invention relates to a method for extracting pellic acid from electrolytic water, which comprises sequentially treating the peat among the humic substances contained in the soil with electrolyzed alkaline water and electrolytic acidic water, and using a catalytic material in the treatment, The present invention provides a pelvic acid extraction method using electrolytic water capable of extracting pelvic acid.

Description

FIELD OF THE INVENTION [0001] The present invention relates to a method for extracting pellic acid from an electrolytic water,

The present invention relates to a method for extracting pellic acid from electrolytic water. More specifically, the present invention relates to a method for extracting pellic acid from electrolytic alkaline water and electrolytic acidic water in a humic material in the soil, The present invention relates to a method for extracting pearl vulcanic acid from an electrolytic water.

As is well known, the caustic acid is generally distributed in less than 2% of the soil in the form of a caustic salt, and is distributed in the combustible minerals in an amount of 20 to 80% or more.

The constituent elements of the caustic acid consist of organic carbon content of 45-50%, oxygen content of about 20%, and other hydrogen, nitrogen and sulfur.

Corrosive acids have the effect of improving soil and soil physically and chemically in favor of crop growth. Improvement effect of soil physical property has the function of improving the porosity of the soil structure and increasing the water permeability and retention function of water to improve the plant root environment for growth in growing the crop.

In soil chemistry, soil microorganisms are activated by increasing the soil organic matter content, stabilizing the soil nitrogen state as a plant nutrient, improving the degradation rate of plant residue, improving the effectiveness of plant trace elements in the soil, Promoting degradation, mitigating overgrowth in the soil, promoting the activity of aerobic microorganisms, and inhibiting the activity of anaerobic microorganisms.

In particular, the effect of increasing the oxygen level and mobility in the soil due to the improvement of the soil structure, the mitigation of heavy metal toxicity and the increase of phosphate availability due to buffering action of the acid functional groups are very important in terms of maintenance of soil fertility and stability of soil environment .

In addition, the caustic acid improves plant growth, promotes root development, activates microbial microbes, increases nutrient availability and absorption, and improves utilization of nitrate nitrogen. This increases the chlorophyll content and photosynthetic ability of the plant, thereby contributing to the improvement of crop quality such as increase of crop yield, sugar content, and increase of vitamin content. In addition, it plays a very beneficial role in stabilizing crop cultivation base by performing functions such as alleviation of water stress, increase in water utilization efficiency, reduction in annual production, increase in resistance to plant diseases, and increase in resistance to pests.

In addition, corrosive acids increase the germination rate and germination rate when germinating seeds, and affect the seeds of crops such as seedling growth promotion and improvement of cleavage rate.

Therefore, the corrosive acid is used as a soil conditioner, a plant growth promoter, a carrier of a trace element, a chelating agent, a drilling lubricant, an ink raw material, a mud pack and a beauty agent such as a mud tank.

So far, corrosive acid salts have been extracted and refined with alkaline solutions using flammable minerals such as lignite, peat, or peat or manure distributed in the ground for a long period of time, as raw materials .

However, the conventional method of extracting a corrosive acid salt from combustible minerals has a disadvantage in that an excessive amount of an alkali solution is contained in the solution of the extracted acid salt, or the yield is very low, which is inefficient.

A description of a method for extracting a corrosive acid salt from a combustible mineral conventionally used is as follows.

G.M. According to Volkov (a study on the formation and characterization of corrosive acid salts by the carbonation of lignite, and a study of its extraction process, Moscow, 1959.), high-quality corrosion acid salts can be obtained by heating for 2 to 4 hours for extraction of corrosive acid salts .

However, this method has a problem of waste of energy and a large amount of alkaline solvent remaining due to heating for a long time, and the yield is low, which is inefficient.

Soviet patent No. 220278 discloses a method for producing alkaline-corrosive acid mixed solution and then treating the lignite residue with a 1% solution of ammonia water in order to increase the yield of the corrosion acid salt, followed by oxidation with air at 100 ° C . This method has a weak point that even though a low concentration of an alkali solution is used, an alkaline solvent still remains to cause eutrophication in an ecosystem and the yield of a corrosive acid salt is low.

G.M. Volkov and L.L. According to Khotunstev (dispersion method for the extraction of corrosive acid salts from combustible minerals - corrosive acid fertilizer, Theory and Practice, Vol. 2, Kyiv National Agricultural Publishing House, Ukraine, 1962, p. 534-539), using a 1400 rpm scour mill It is described that the method of putting the fine powdered lignite into the batch type reactor and introducing the alkali solution can extract a greater amount of the corrosive acid salt than the method of administering the preheated lignite into the alkali solution.

According to this method, the concentration of the alkali solution to be used for the extraction of the corrosive acid salt is selected differently depending on the type of the lignite, and the weight ratio of the lignite to the lignite is adjusted to about 20% 1.5%, it was possible to increase the yield up to 50% by developing a new technique to overcharge the alkali solution at a low temperature of 20 ~ 25 ° C, but it still has a weak point that a large amount of alkali solution remains.

Russian Patent No. 1404501 discloses a method for massive extraction of corrosive acid at a high yield of 96% in the form of ammonium hydroxide by treating the lignite with 10% aqueous ammonia solution at a low frequency vibration energy of 15 to 20 Hz . However, this method also has a problem in that effervescence may occur in an ecosystem by using an excessive amount of ammonia water, the design of the manufacturing process is complicated, and the production cost is high, making practical use difficult.

Korean Patent Registration No. 10-0435506 discloses a method of artificially producing active soil using zeolite and peat. The method comprises mixing the zeolite and the peat in a weight ratio of 1 to 1.25, adjusting the water content to 60%, adjusting the pH to 1.5 to 2.5 by injecting sulfuric acid, heating the mixture to 90 to 180 ° C for 4 hours And extracting the corrosive acid by a long process to produce an active humus soil.

However, since active edible soils are mainly used for soil remediation and wastewater treatment, they can not be regarded as a method for mass production of corrosion acid as a raw material.

Korean Patent Registration No. 10-0433372 discloses a method for extracting a corrosive acid and pelubactan from an animal manure biologically treated water. The caustic acid and fulvic acid extracted by the above method can be usefully used in agricultural crops. Korean Patent Registration No. 10-0848669 discloses a powdery feed additive containing a crude extract containing a caustic acid and a vegetable extract, a mixed powder containing a biotite powder and a degreasing steel at a predetermined ratio, . The above method is a method for extracting a corrosive acid salt by using a humus soil. Since the purity of a corrosive acid salt is low and the extraction amount is small, it is used as a means for use in the production of an organic fertilizer. Therefore, the above method is insufficient to secure a large amount of corrosion acid as a raw material.

The conventional method of extracting a corrosive acid salt from a combustible mineral containing alkali metal and ammonium as described so far has an excessive amount of alkali remaining unresponsive to the alkali mixing suspension and can affect the ecosystem and improve the yield There are disadvantages.

In addition, extraction of the corrosive acid salt with the proposed alkali concentration can obtain a high quality corrosion acid salt, but since the concentration of the alkali solution is difficult to control during the extraction process, the alkaline solution remains and the processing cost of the combustible mineral is complicated, .

Therefore, there is a need to develop an improved extraction method of a corrosive acid salt that can increase the yield without remaining excess alkali solution in the corrosive acid salts extracted from the combustible minerals.

SUMMARY OF THE INVENTION The present invention has been made in view of the circumstances of the prior art described above, and it is an object of the present invention to provide a method and apparatus for treating peat in alkaline water and electrolytic acid water in a humic material, The present invention relates to a method for extracting pearl vulcanic acid from an electrolytic water,

In order to achieve the above object, according to a preferred embodiment of the present invention, there is provided a method of manufacturing a flammable mineral containing a humic substance and an alkaline aqueous solution in a weight ratio of 1: 3 to 1:15 in a mixed state for at least 4 hours, Separating; b) extracting the supernatant and separating the acidic aqueous solution into a supernatant and a precipitate by maintaining the mixed state at a weight ratio of 1: 2 to 1: 5 for 8 hours; and c) separating the fulvic acid by centrifuging the mixed suspension of step b).

Preferably, the combustible mineral is peat, and the method for extracting pellic acid using electrolytic water is provided.

Preferably, the alkali aqueous solution is an electrolysis alkali aqueous solution containing 0.4% by weight of a catalyst selected from the group consisting of sodium hydroxide, potassium carbonate, sodium trisphosphate and sodium silicate.

Preferably, the acidic aqueous solution is an electrolytic acidic aqueous solution using purified sodium chloride.

The method of extracting pellic acid from electrolytic water according to the present invention reduces the input amount of the alkali aqueous solution and the acidic aqueous solution by using a catalyst in the electrolysis for obtaining an aqueous solution and the maximum pellic acid can be obtained even when a small aqueous alkaline solution is added, The efficiency is greatly increased, the production cost can be drastically reduced, and there is an advantage that it is an eco-friendly manufacturing method that minimizes waste of resources.

Hereinafter, the present invention will be described in detail with reference to the drawings.

The method of extracting pellic acid from electrolytic water according to an embodiment of the present invention is characterized in that peat among the humic substances contained in the soil is sequentially treated with electrolytic alkaline water and electrolytic acid water, and a small amount of humic substance It is a method for extracting a large amount of pearlic acid.

More specifically, the method of extracting pellic acid using electrolytic water according to an embodiment of the present invention is performed through an alkali aqueous solution treatment and an acidic aqueous solution treatment step, wherein a) a combustible mineral containing a humic substance and an alkali aqueous solution are mixed at a ratio of 1: To 1: 15 weight ratio for at least 4 hours to separate the supernatant; b) extracting the supernatant and separating the acidic aqueous solution into a supernatant and a precipitate by maintaining the mixed state at a weight ratio of 1: 2 to 1: 5 for 8 hours.

The present invention also includes a step c) separating the pivalic acid by centrifuging the mixed suspension of step b).

At this time, the combustible mineral may be lignite, bituminous coal, and anthracite, but is preferably a peat.

The alkali aqueous solution may be any one of an aqueous solution of sodium hydroxide, an aqueous solution of potassium hydroxide, an aqueous solution of ammonia, an aqueous solution of sodium phosphate, and an aqueous solution of sodium carbonate. Decomposed alkali aqueous solution.

In order to increase the extraction yield of pelubactic acid from combustible minerals, the alkali solution should be heated to the optimum temperature.

The acidic aqueous solution is an electrolytic acidic aqueous solution using purified sodium chloride.

In the extraction method according to the present invention, the mixing ratio of the combustible mineral and the alkali aqueous solution is adjusted to determine the amount of the alkali to be added. More preferably, the alkaline reaction is maximized by using the catalytic material to obtain the same amount of pearlic acid It is possible to effectively reduce the amount of alkali, thereby minimizing the alkali residues present in the pelubactic acid and maximally reducing the extraction loss of pelubactic acid, thereby maximizing the yield of pelubactic acid.

That is, the use of electrolytic water increases the oxidation-reduction potential (oxidation-reduction potential difference) of the ORP value, so that even if a small amount of catalyst is used, the electrolytic water is extracted more and the cost is also reduced.

Hereinafter, preferred embodiments of the present invention will be described in order to facilitate understanding of the present invention. However, the following examples are provided only for the purpose of easier understanding of the present invention, and the present invention is not limited by the examples.

Example 1 : Pelvactic acid extraction from peat

First, 0.4% by weight of any one of sodium hydroxide, potassium carbonate, sodium trisphosphate and sodium silicate, which is a catalytic substance, is added to 150 ml of 1 to 5 mol of sodium hydroxide (NaOH) solution and 150 ml of hot water Mix and electrolysis.

The electrolytic bath used for electrolysis may include a diaphragm for separating the regions of the anode portion, the cathode portion and the both electrode portions. The diaphragm may be made of polyvinylidene difluoride (PVDF), polytetrafluoroethylene (PTFE), polyether sulfone ) And polycarbonate. In this embodiment, PVDF (polyvinylidene difluoride) is used. The pores of the diaphragm are 1 to 10 mu m.

The electrodes of the anode and the cathode may be Ti / IrO2 or Ti / RuO2, but Ti / IrO2 is used in the present embodiment.

Further, the alkali aqueous solution is obtained by electrolysis in a current density range of 50 to 200 mA / cm 2, and the inflow rate of the electrolytic bath is 5 to 30 ml / min.

In this state, 100 g of the peat excavated in the domestic Gangwon-do clean area and 300 ml of the electrolyzed alkaline aqueous solution are kept mixed for 4 hours.

Then, the mixed suspension is separated into a supernatant and a precipitate. Only the supernatant is separated and extracted.

Then, 100 ml of the extracted supernatant is separated into a supernatant and a precipitate by maintaining the mixed state at a weight ratio of 200 ml of the acidic aqueous solution for 8 hours. The acidic aqueous solution used herein is an aqueous solution obtained by electrolysis of purified sodium chloride (NaCl) The acidic aqueous solution is also obtained by electrolysis in the current density range of 50 to 200 mA / cm 2 in the same manner as the aqueous alkaline solution, and the flow rate of the electrolysis bath is 5 to 30 ml / min.

At this time, PH is 0 to 2.0.

Then, the mixed suspension obtained by mixing the acidic aqueous solution was centrifuged to separate the pivalic acid, and the amount of the obtained pivalic acid was measured.

Comparative Example : Corrosion acid extraction from peat

Under the conditions shown in Table 1 below. Volkov and L.L. According to the method of Khotunstev (a dispersion method for the extraction of corrosive acid salts from combustible minerals - Corrosive acid fertilizer, Theory and Practice, Vol. 2, Kyiv National Agricultural Press, Ukraine, 1962, p. 534-539) The salt was extracted. In Comparative Example 1, soybean lignite was used.

Conditions and yields of pelubactic acid and corrosive acid extracted from the combustible minerals of Example 1 and Comparative Example 1 are shown in Table 1.

Humidity(%) Peat / Lignite content (%) Mixing suspension temperature (캜) Alkali aqueous solution (ml) The amount of catalyst (g) Acidic aqueous solution (ml) Pelvic acid / Corrosive acid yield (g) Example 5 96 96 300 0.1 200 96.3 Comparative Example 36 96 45 300 0 0 61.7

As shown in Table 1, according to the extraction method of the present invention, as a method of sequentially using an electrolytic alkali aqueous solution and an electrolytic acidic aqueous solution obtained by electrolytic treatment using a flammable mineral, that is, peat and alkali aqueous solution, The amount of alkaline aqueous solution and acidic aqueous solution required to obtain the same amount of pearlbic acid can be reduced and most of the pearlic acid obtained from the combustible mineral can be obtained.

Meanwhile, the method of extracting pellic acid using electrolytic water according to an embodiment of the present invention is not limited to the above-described embodiment, but various modifications can be made without departing from the technical gist.

Claims (4)

a) separating the supernatant liquid by maintaining a mixed state of the combustible mineral containing the humic substance and the aqueous alkali solution at a weight ratio of 1: 3 to 1:15 for at least 4 hours;
b) extracting the supernatant and separating the aqueous electrolytic acid solution using purified sodium chloride into a supernatant and a precipitate by maintaining the mixed state at a weight ratio of 1: 2 to 1: 5 for 8 hours;
c) separating the fulvic acid by centrifuging the mixed suspension of step b). The method according to claim 1,
Wherein the combustible mineral is peat. The method according to claim 1,
Wherein the alkali aqueous solution is an electrolysis alkali aqueous solution containing 0.4% by weight of a catalyst selected from the group consisting of sodium hydroxide, potassium carbonate, sodium trisphosphate and sodium silicate. delete