Summary of the invention
The object of this invention is to provide a kind of processing method utilizing waste cotton seed to produce humic acid.
The present invention includes following steps:
A, fermentation: waste cotton seed and water are added fermentation vat by weight the ratio for 1:1 ~ 1:2.5 are the environment bottom fermentation 10 ~ 40 days of 15 ~ 25 DEG C in temperature;
B, alkalization: after having fermented, according to waste cotton seed and potassium hydroxide solid weight than the ratio for 1:0.04 ~ 1:0.05 add alkalization pond alkalinisation treatment 4 little time more than, be preferably 4 ~ 8 hours, cross leaching solution and namely obtain humic acid solution of the present invention.
Waste cotton seed described in above-mentioned a step can be through lint, and also can be through dressing, can also be the mixing of lint and dressing.
The waste cotton seed of above-mentioned a step is preferably crushed to 0.1mm ~ 0.5mm.
During above-mentioned a step fermentation, the ratio being preferably 1:0.001 ~ 1:0.01 according to waste cotton seed and cellulose-decomposing bacteria weight ratio adds cellulose-decomposing bacteria.
As improvement, after above-mentioned a step fermentation, filtered by the material after fermentation with 1 ~ 3mm filter screen, gained fermented liquid and fermentation slag charge are inserted in alkalization pond A and alkalization pond B respectively.
By leaving the fermented liquid in alkalization pond A in, adding 9 ~ 10g potassium hydroxide according to 1L fermented liquid, alkalizing more than 4 hours under the environment of 15 ~ 25 DEG C, be preferably 4 ~ 8 hours;
Fermentation slag charge in alkalization pond B will be left in, according to adding potassium hydroxide solution 5 ~ 7L that concentration is 0.15 ~ 0.25mol/L in per kilogram fermentation residue (with dry basis), alkalize 4 ~ 8 hours under the environment of 15 ~ 25 DEG C, then the solution in alkalization pond A and alkalization pond B is filtered to obtain humic acid solution.
Above-mentioned humic acid solution is preferably selected the filter screen of 38 ~ 75 μm and is filtered by the mode of negative pressure leaching, can obtain the product of drip irrigation-grade.
As further improvement, after above-mentioned b step alkalinisation treatment, gained humic acid solution carries out acidification: select volume ratio to be that the hydrochloric acid of 5:1 ~ 20:1 and phosphoric acid mixing solutions are as acidizing fluid, acidizing fluid concentration is 15 ~ 18%, acidizing fluid is joined gradually in humic acid solution, stop adding acidizing fluid when pH value reaches 2.0 ~ 3.0, acidification more than 4 hours under the environment of 15 ~ 25 DEG C, be preferably 4 ~ 8 hours, obtain the high first class product of humic acid of the present invention, i.e. xanthohumic acid solution, gained xanthohumic acid solution preferably uses the filter screen of less than 38 μm again, the method of negative pressure leaching is adopted to carry out leaching filtrate, drip irrigation-grade xanthohumic acid solution product can be arrived.
As improvement, the xanthohumic acid solution after above-mentioned acidifying preferably precipitates more than 12 hours under the environment of 15 ~ 25 DEG C, is preferably 12 ~ 24 hours, then gets supernatant liquor under the environment of 102 ~ 110 DEG C and dewaters, can obtain xanthohumic acid solid phase prod further.
Compared with prior art, practicality of the present invention has energy-conserving and environment-protective, does not use brown coal or weathered coal to be raw material, and can by features such as a large amount of waste cotton seed recyclings.
Embodiment
Embodiment 1:
The present invention includes following steps: a, fermentation: waste cotton seed and water are added fermentation vat by weight the ratio for 1:1, is the environment bottom fermentation 20 days of 25 DEG C in temperature; B, alkalization: after having fermented, according to waste cotton seed and potassium hydroxide solid weight than the ratio for 1:0.04 add alkalization pond alkalinisation treatment 4 little time, cross leaching solution and namely obtain humic acid solution of the present invention.
Embodiment 2:
The present invention includes following steps: a, fermentation: add fermentation vat with water by weight for the ratio of 1:2 after waste cotton seed is crushed to 0.5mm, is the environment bottom fermentation 10 days of 15 DEG C in temperature; B, alkalization: after having fermented, according to waste cotton seed and potassium hydroxide solid weight than the ratio for 1:0.05 add alkalization pond alkalinisation treatment 6 little time, cross leaching solution and namely obtain humic acid solution of the present invention.
Embodiment 3:
The present invention includes following steps: a, fermentation: after waste cotton seed is crushed to 0.2mm, add fermentation vat with water by weight the ratio for 1:2.5, at the environment bottom fermentation 40 days that temperature is 20 DEG C, and add cellulose-decomposing bacteria according to the ratio that waste cotton seed and cellulose-decomposing bacteria weight ratio are 1:0.01; B, alkalization: after having fermented, according to waste cotton seed and potassium hydroxide solid weight than the ratio for 1:0.04 add alkalization pond alkalinisation treatment 8 little time, cross leaching solution and namely obtain humic acid solution of the present invention.
Embodiment 4:
The present invention includes following steps: a, fermentation: waste cotton seed and water are added fermentation vat by weight the ratio for 1:1.5, is the environment bottom fermentation 30 days of 18 DEG C in temperature; After fermentation, filtered by the material 2mm filter screen after fermentation, gained fermented liquid and fermentation slag charge are inserted in alkalization pond A and alkalization pond B respectively; B, alkalization: by leaving the fermented liquid in alkalization pond A in, adding 10g potassium hydroxide according to 1L fermented liquid, alkalizing 5 hours under the environment of 25 DEG C; Fermentation slag charge in alkalization pond B will be left in, according to adding the potassium hydroxide solution 7L that concentration is 0.25mol/L in per kilogram fermentation residue (with dry basis), alkalize 4 hours under the environment of 15 DEG C, then the solution in alkalization pond A and alkalization pond B is filtered to obtain humic acid solution.
Embodiment 5:
The present invention includes following steps: a, fermentation: add fermentation vat with water by weight for the ratio of 1:1.2 after waste cotton seed is crushed to 0.4mm, is the environment bottom fermentation 25 days of 22 DEG C in temperature; After fermentation, filtered by the material 1mm filter screen after fermentation, gained fermented liquid and fermentation slag charge are inserted in alkalization pond A and alkalization pond B respectively; B, alkalization: by leaving the fermented liquid in alkalization pond A in, adding 9g potassium hydroxide according to 1L fermented liquid, alkalizing 10 hours under the environment of 15 DEG C; Fermentation slag charge in alkalization pond B will be left in, according to adding the potassium hydroxide solution 6L that concentration is 0.15mol/L in per kilogram fermentation residue (with dry basis), alkalize 6 hours under the environment of 20 DEG C, then the solution in alkalization pond A and alkalization pond B is filtered to obtain humic acid solution.
Embodiment 6:
The present invention includes following steps: a, fermentation: after waste cotton seed is crushed to 0.3mm, add fermentation vat with water by weight the ratio for 1:2.3, at the environment bottom fermentation 35 days that temperature is 15 DEG C, and add cellulose-decomposing bacteria according to the ratio that waste cotton seed and cellulose-decomposing bacteria weight ratio are 1:0.006; After fermentation, filtered by the material 3mm filter screen after fermentation, gained fermented liquid and fermentation slag charge are inserted in alkalization pond A and alkalization pond B respectively; B, alkalization: by leaving the fermented liquid in alkalization pond A in, adding 10g potassium hydroxide according to 1L fermented liquid, alkalizing 9 hours under the environment of 20 DEG C; Fermentation slag charge in alkalization pond B will be left in, according to adding the potassium hydroxide solution 5L that concentration is 0.2mol/L in per kilogram fermentation residue (with dry basis), alkalize 10 hours under the environment of 25 DEG C, then the solution in alkalization pond A and alkalization pond B is filtered to obtain humic acid solution.
Embodiment 7:
The present invention includes following steps: a, fermentation: after waste cotton seed is crushed to 0.1mm, add fermentation vat with water by weight the ratio for 1:1.8, at the environment bottom fermentation 25 days that temperature is 25 DEG C, and add cellulose-decomposing bacteria according to the ratio that waste cotton seed and cellulose-decomposing bacteria weight ratio are 1:0.003; After fermentation, filtered by the material 1.5mm filter screen after fermentation, gained fermented liquid and fermentation slag charge are inserted in alkalization pond A and alkalization pond B respectively; B, alkalization: by leaving the fermented liquid in alkalization pond A in, adding 9g potassium hydroxide according to 1L fermented liquid, alkalizing 6 hours under the environment of 15 DEG C; Fermentation slag charge in alkalization pond B will be left in, according to adding the potassium hydroxide solution 7L that concentration is 0.15mol/L in per kilogram fermentation residue (with dry basis), alkalize 7 hours under the environment of 25 DEG C, again the solution in alkalization pond A and alkalization pond B is filtered to obtain humic acid solution, obtained humic acid solution selected the filter screen of 75 μm and filter by the mode of negative pressure leaching, the product of drip irrigation-grade can be obtained.
Embodiment 8:
The present invention includes following steps: a, fermentation: waste cotton seed and water are added fermentation vat by weight the ratio for 1:1.1, is the environment bottom fermentation 15 days of 22 DEG C in temperature; B, alkalization: after having fermented, according to waste cotton seed and potassium hydroxide solid weight than the ratio for 1:0.05 add alkalization pond alkalinisation treatment 7 little time, cross leaching solution and namely obtain humic acid solution of the present invention; C, acidifying: after having alkalized, volume ratio is selected to be that the hydrochloric acid of 15:1 and phosphoric acid mixing solutions are as acidizing fluid, acidizing fluid concentration is 15%, acidizing fluid is joined gradually in humic acid solution, stop adding acidizing fluid when pH value reaches 2.0, acidification 7 hours under the environment of 18 DEG C, obtain the high first class product of humic acid of the present invention, i.e. xanthohumic acid solution, gained xanthohumic acid solution preferably uses the filter screen of 50 μm again, adopt the method for negative pressure leaching to carry out leaching filtrate, drip irrigation-grade xanthohumic acid solution product can be obtained.
As improvement, the xanthohumic acid solution after above-mentioned acidifying precipitates 12 hours under the environment of 15 DEG C, then gets supernatant liquor under the environment of 108 DEG C to dewater, and can obtain xanthohumic acid solid phase prod further.
Embodiment 9:
The present invention includes following steps: a, fermentation: waste cotton seed and water are added fermentation vat by weight the ratio for 1:2, is the environment bottom fermentation 15 days of 18 DEG C in temperature; B, alkalization: after having fermented, according to waste cotton seed and potassium hydroxide solid weight than the ratio for 1:0.04 add alkalization pond alkalinisation treatment 10 little time, cross leaching solution and namely obtain humic acid solution of the present invention; C, acidifying: after having alkalized, volume ratio is selected to be that the hydrochloric acid of 20:1 and phosphoric acid mixing solutions are as acidizing fluid, acidizing fluid concentration is 15%, acidizing fluid is joined gradually in humic acid solution, stop adding acidizing fluid when pH value reaches 2.7, acidification 7 hours under the environment of 16 DEG C, obtain the high first class product of humic acid of the present invention, i.e. xanthohumic acid solution, gained xanthohumic acid solution preferably uses the filter screen of 38 μm again, adopt the method for negative pressure leaching to carry out leaching filtrate, drip irrigation-grade xanthohumic acid solution product can be obtained.
As improvement, the xanthohumic acid solution after above-mentioned acidifying precipitates 15 hours under the environment of 20 DEG C, then gets supernatant liquor under the environment of 103 DEG C to dewater, and can obtain xanthohumic acid solid phase prod further.
Embodiment 10:
The present invention includes following steps: a, fermentation: after waste cotton seed is crushed to 0.2mm, add fermentation vat with water by weight the ratio for 1:1.5, at the environment bottom fermentation 10 days that temperature is 15 DEG C, and add cellulose-decomposing bacteria according to the ratio that waste cotton seed and cellulose-decomposing bacteria weight ratio are 1:0.004; B, alkalization: after having fermented, according to waste cotton seed and potassium hydroxide solid weight than the ratio for 1:0.04 add alkalization pond alkalinisation treatment 8 little time, cross leaching solution and namely obtain humic acid solution of the present invention; C, acidifying: after having alkalized, volume ratio is selected to be that the hydrochloric acid of 10:1 and phosphoric acid mixing solutions are as acidizing fluid, acidizing fluid concentration is 18%, acidizing fluid is joined gradually in humic acid solution, stop adding acidizing fluid when pH value reaches 2.2, acidification 4 hours under the environment of 22 DEG C, obtain the high first class product of humic acid of the present invention, i.e. xanthohumic acid solution, gained xanthohumic acid solution preferably uses the filter screen of 80 μm again, adopt the method for negative pressure leaching to carry out leaching filtrate, drip irrigation-grade xanthohumic acid solution product can be obtained.
As improvement, the xanthohumic acid solution after above-mentioned acidifying precipitates 20 hours under the environment of 18 DEG C, then gets supernatant liquor under the environment of 104 DEG C to dewater, and can obtain xanthohumic acid solid phase prod further.
Embodiment 11:
The present invention includes following steps: a, fermentation: after waste cotton seed is crushed to 0.2mm, add fermentation vat with water by weight the ratio for 1:2.5, at the environment bottom fermentation 10 days that temperature is 18 DEG C, and add cellulose-decomposing bacteria according to the ratio that waste cotton seed and cellulose-decomposing bacteria weight ratio are 1:0.005; B, alkalization: after having fermented, according to waste cotton seed and potassium hydroxide solid weight than the ratio for 1:0.04 add alkalization pond alkalinisation treatment 8 little time, cross leaching solution and namely obtain humic acid solution of the present invention; C, acidifying: after having alkalized, volume ratio is selected to be that the hydrochloric acid of 8:1 and phosphoric acid mixing solutions are as acidizing fluid, acidizing fluid concentration is 17%, acidizing fluid is joined gradually in humic acid solution, stop adding acidizing fluid when pH value reaches 2.4, acidification 4 hours under the environment of 22 DEG C, obtain the high first class product of humic acid of the present invention, i.e. xanthohumic acid solution, gained xanthohumic acid solution preferably uses the filter screen of less than 48 μm again, adopt the method for negative pressure leaching to carry out leaching filtrate, drip irrigation-grade xanthohumic acid solution product can be obtained.
As improvement, the xanthohumic acid solution after above-mentioned acidifying precipitates 24 hours under the environment of 15 DEG C, then gets supernatant liquor under the environment of 102 DEG C to dewater, and can obtain xanthohumic acid solid phase prod further.
Embodiment 12:
The present invention includes following steps: a, fermentation: after waste cotton seed is crushed to 0.4mm, add fermentation vat with water by weight the ratio for 1:1.8, at the environment bottom fermentation 25 days that temperature is 23 DEG C, and add cellulose-decomposing bacteria according to the ratio that waste cotton seed and cellulose-decomposing bacteria weight ratio are 1:0.004; B, alkalization: after having fermented, according to waste cotton seed and potassium hydroxide solid weight than the ratio for 1:0.05 add alkalization pond alkalinisation treatment 6 little time, cross leaching solution and namely obtain humic acid solution of the present invention; C, acidifying: after having alkalized, volume ratio is selected to be that the hydrochloric acid of 13:1 and phosphoric acid mixing solutions are as acidizing fluid, acidizing fluid concentration is 18%, acidizing fluid is joined gradually in humic acid solution, stop adding acidizing fluid when pH value reaches 2.5, acidification 8 hours under the environment of 20 DEG C, obtain the high first class product of humic acid of the present invention, i.e. xanthohumic acid solution, gained xanthohumic acid solution preferably uses the filter screen of less than 75 μm again, adopt the method for negative pressure leaching to carry out leaching filtrate, drip irrigation-grade xanthohumic acid solution product can be obtained.
As improvement, the xanthohumic acid solution after above-mentioned acidifying precipitates 18 hours under the environment of 20 DEG C, then gets supernatant liquor under the environment of 107 DEG C to dewater, and can obtain xanthohumic acid solid phase prod further.
Embodiment 13:
The present invention includes following steps: a, fermentation: after waste cotton seed is crushed to 0.4mm, add fermentation vat with water by weight the ratio for 1:2.2, at the environment bottom fermentation 25 days that temperature is 17 DEG C, and add cellulose-decomposing bacteria according to the ratio that waste cotton seed and cellulose-decomposing bacteria weight ratio are 1:0.005; B, alkalization: after having fermented, according to waste cotton seed and potassium hydroxide solid weight than the ratio for 1:0.05 add alkalization pond alkalinisation treatment 6 little time, cross leaching solution and namely obtain humic acid solution of the present invention; C, acidifying: after having alkalized, volume ratio is selected to be that the hydrochloric acid of 22:1 and phosphoric acid mixing solutions are as acidizing fluid, acidizing fluid concentration is 16%, acidizing fluid is joined gradually in humic acid solution, stop adding acidizing fluid when pH value reaches 2.7, acidification 8 hours under the environment of 20 DEG C, obtain the high first class product of humic acid of the present invention, i.e. xanthohumic acid solution, gained xanthohumic acid solution preferably uses the filter screen of less than 40 μm again, adopt the method for negative pressure leaching to carry out leaching filtrate, drip irrigation-grade xanthohumic acid solution product can be obtained.
As improvement, the xanthohumic acid solution after above-mentioned acidifying precipitates 20 hours under the environment of 25 DEG C, then gets supernatant liquor under the environment of 110 DEG C to dewater, and can obtain xanthohumic acid solid phase prod further.