CN104530447A - Method for extracting biological humic acid from ethanol waste mash - Google Patents
Method for extracting biological humic acid from ethanol waste mash Download PDFInfo
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- CN104530447A CN104530447A CN201510027740.9A CN201510027740A CN104530447A CN 104530447 A CN104530447 A CN 104530447A CN 201510027740 A CN201510027740 A CN 201510027740A CN 104530447 A CN104530447 A CN 104530447A
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Abstract
The invention discloses a method for extracting biological humic acid from ethanol waste mash. The method comprises the following steps of controlling the ethanol waste mash at 80-90 DEG C and adjusting the pH to 5.8-6.3, evaporating, concentrating until the brix degree of a concentrate is 50-55% and carrying out spray drying to obtain granular biological humic acid. By the treatment method of the ethanol waste mash which is developed by the invention, the ethanol waste mash can be completely treated and utilized without addition of any reagent, no any wastewater or exhaust gas is discharged during the preparation process and thus the problems of substandard discharge and secondary pollution are completely avoided. The biological humic acid product obtained by the method has the following parameters that the content of total humic acid reaches 80wt%, wherein the content of fulvic acid reaches 77wt%, the content of dark brown humic acid reaches 3.0wt%, the content of K2O reaches 18.7wt%, the content of P2O reaches 3.5wt% and the content of flavonoid reaches 3.2wt%; and therefore the obtained biological humic acid product belongs to high-quality fulvic acid.
Description
Technical field
The present invention relates to a kind of method extracting biological humic from alcohol waste mash, belong to waste utilization technical field.
Background technology
Century, environment and re-sources problem became the matter of utmost importance affecting human survival and sustainable economic development just day by day.Along with Economic development, the waste that industrial production produces is increasing, and pollution on the environment is more and more serious, also to contain the economic opportunity that waste cycling and reutilization is very large simultaneously.The recycling of waste is the inevitable development direction of current global environmental protection, and the living environment of improving and beautifying mankind itself is extremely urgent.
The alcohol waste mash produced when producing alcohol is a kind of organic waste water of ultrahigh concentration, and COD content is 125000 ~ 170000mg/L, BOD content is 65000 ~ 8500mg/L, and its pollution intensity is more than 240 times of general domestic pollution source.The dissolved solids content of alcohol waste mash is high, dissolved solids content is generally 12 ~ 17BX, in soluble solids, more than 70% is organic, wherein there is sugar, protein, amino acid, vitamine etc., residue 30% is ash content, ash content contain the inorganic salt such as nitrogen, phosphorus, potassium, calcium, magnesium, potassium content up to 0.15 ~ 1.315mg/L.Waste water is in acid, and pH value is 4.8 ~ 5.8.The useless mash often producing one ton of alcohol generation is 12 ~ 14m
3, the pollution load of alcohol waste mash generation is simultaneously very high, often produces 1 ton of alcohol discharge COD about 1.33 tons, BOD about 0.73 ton, SS about 0.62 ton.Its intractability is comparatively large, former treatment process mostly is that method is filled with in liquid agriculture, biochemical process, anaerobic process, anaerobically fermenting are produced in biogas method, oxidation pond process, condensed combustion method, ash flushing water and etc. method.All there is following shortcoming in above administering method: 1. administers the emission standard being difficult to reach country's permission; 2. easily secondary pollution is caused; 3. control investment recovery is more difficult.
Biological humic (xanthohumic acid) be last century the nineties by Chinese research out, the single history extracted from brown coal of xanthohumic acid has been broken in this creation.Biological humic (BFA) take biomass as raw material, be rely on biological fermentation, or from biomass extract obtain compared with mineral humic acids (HA), BFA has higher biological activity, BFA is superior to HA in five: 1. the little penetrating power of molecular weight is strong, easily by bio-absorbable; 2. good water solubility, resistance to hard water is strong, does not flocculate, does not precipitate, easy to use; 3. active gene content is high, and physiologically active is large, strong to metal ion-chelant, fusion faculty; 4. saturation solubility has good intermiscibility greatly, with trace element; 5. not containing heavy metal and other objectionable impurities, be particularly applicable to develop medicinal product.
At agriculturally applying biological humic acids, mainly promote fertilizer efficiency, improve soil, improve crop quality, regulating crop growth and strengthen the resistance of farm crop.Main products has humic acid soil improver, humic acid fertilizer, humic acids agricultural chemicals, humic acids seedling substratum etc.Biological humic soil improvement agent is used for the land remediation of alkaline land improvement and heavy metal contamination, for many-sides such as Desertification drought resisting improvement, also can be made into xanthohumic acid degradable mulch, for aspects such as integrated nursery.At development semiorganic compound fertilizer, foliage fertilizer, the aspects such as liquid sprays fertilizer, humic acids coated fertilizer in China big area advance.Biological humic agricultural chemicals is a kind of brand-new environmental type product.Have the effects such as growth regulator, adverse-resistant agent, sterilant, weedicide, these products are used on farm crop, have improvement soil to promote fertilizer efficiency, regulate crop growth, strengthen the effects such as disease-resistant crops.
If alcohol waste mash is made under the condition of cleaning-less bacteria infection high-quality biological humic to be used, can not only blowdown be reduced, avoid environmental pollution, the unmanageable problem of alcohol waste mash can also be solved, realize resource circulation utilization.
Patent application " alcohol slops harmless treatment and utilisation technology " (201310578657.1), open waste liquid is acidified, oxidation, biochemical, neutralization, flocculation, precipitate and separate reaction treatment obtain mother liquor, containing crop desired nutritionals such as a large amount of microorganism, amino acid, humic acid, organic matters in mother liquor, can be used as the main raw material of organic liquid fertilizer.Patent of invention " utilizing sugar refinery waste residue, waste water to produce the technique of humic acid organic composite fertilizer " (200810219215.7), openly by following processing step: alcohol slops concentrates → quaternization → hybrid reactorization fermentation → pulverizing, sub-sieve, mixed processes and disk balling-up → face powder, drying, sub-sieve and packaging.But these two parts of prior aries all need add reagent in alcohol slops, and through techniques such as biochemical or fermentations, and products therefrom is organic fertilizer raw material containing humic acid or compoiste fertilizer, directly can't utilize alcohol slops acquisition biological humic acid.
Patent of invention " utilizing alcohol waste liquid for sugar refinery to prepare method of activated humic acid liquid and products thereof and purposes " (03112360.0), disclose and alcohol waste liquid for sugar refinery is clarified, make the calcium salt in waste liquid and other insolubless precipitation, obtain supernatant liquor, supernatant liquor is evaporated below as far as possible low temperature, obtain concentrated solution, add in concentrated solution halogen oxide and at room temperature make its in the reactor stir-activating obtain activated humic acid liquid.This activated humic acid liquid can directly use as agronomic crop seed germination, the promotor taken root, uses after also can processing further as the aquatic products medicine of environment-friendly type, agricultural trace element fertilizer, vegetables liquid fertilizer, water body liquid fertilizer, fruit tree solution.This part of prior art need add halogen oxide in preparation process, and this active humic acid liquid is only containing active humic acid >=18%.
Document " preparing humic acids and applied research thereof from the alcohol distillation waste liquid of sweet potato raw material " concentrates sweet potato alcohol slops, solid matter is wherein made to account for about 40%, then enriched material is transferred in enamel reaction still, adjustment temperature of reaction kettle, hydrothermal treatment consists, after 3 hours, filters the suspension product generated, and with hot water wash to not containing sulfate radicals, filter filter cake dry at 105 DEG C, weigh, obtain dun, humus containing humic acids.Document gained is the humus (being as the criterion with butt) containing humic acids 30.21%, can not obtain highly purified humic acid.
Therefore, be necessary to research and develop a kind of method alcohol waste mash directly being made high quality biological humic acid.
Summary of the invention
Because alcohol waste mash is difficult, and existing high quality biological humic only can rely on the unitary system such as biological fermentation or biological extraction Preparation Method, there is raw material and be difficult to the problems such as recycle by limitation, resource, the invention provides a kind of method extracting biological humic from alcohol waste mash, with whole recyclings of the zero release and waste liquid that realize waste liquid, thoroughly eradicate a difficult problem for alcohol industry environmental pollution.
The present invention is realized by following technical proposal: a kind of method extracting biological humic from alcohol waste mash, through following each step:
(1) alcohol waste mash is controlled at 80 ~ 90 DEG C, and adjust ph=5.8 ~ 6.3; When this is due to pH value=5.8 ~ 6.3, the hydroxyl in alcohol waste mash can reach the best demand of human body, is rich in multivitamin, as vitamin A, VITMAIN B1, Lin Suanna Vitamin B2 Sodium Phosphate, vitamin B6, vitamin B12, vitamins C, vitamin F;
(2) it is the concentrated solution of 50 ~ 55% that the alcohol waste mash after step (1) being regulated carries out evaporation concentration to brix;
(3) granular biological humic is obtained by spray-dried for the concentrated solution of step (2).
The adjust ph of described step (1) regulates with alkali lye.
Described alkali lye is the aqua calcis of any concentration.
The evaporation concentration of described step (2) is carried out in quadruple effect falling film evaporation mode: alcohol waste mash is with 80 ~ 90 DEG C of chargings, and the pressure that passes into of saturation steam is 0.4 ~ 0.8Mpa.
The moisture that in described step (2), evaporation concentration is collected is soft water, can be directly used in boiler feed water.
The temperature controlling concentrated solution in described step (3) during spraying dry is 170 ~ 190 DEG C and sprays.This is because the nutrition mass-energy in concentrated solution at 170 ~ 190 DEG C is preserved completely, can not lose nutritive ingredient because of spraying dry.
In described step (3), spraying dry is the particle making concentrated solution form 0.35mm granularity under the sinking speed of 300 ~ 400mm/s.The undersized of particle, can be easily sticky glutinous.
Aforesaid method is applicable to the alcohol waste mash process produced from raw materials such as sweet potato, sugarcane, beets.
Advantage of the present invention and effect: the alcohol residue liquid processing method of the present invention's research and development can by complete for alcohol waste mash processing and utilizing, and do not need to add any reagent, also without any waste water and exhaust gas emission in preparation process, completely avoid the problem of the not up to standard and secondary pollution of discharge.The parameter of gained biological humic product of the present invention is as follows: total humic acid reaches that 80wt%, wherein xanthohumic acid reach 77wt%, dark brown humic acids reaches 3.0wt%, K
2o reaches 18.7wt%, P
2o reaches 3.5wt%, flavones reaches 3.2wt%, belongs to high-quality xanthohumic acid.Gained biological humic is the best raw material of fertilizer, it is again farm crop high-grade nutrient element, low-carbon (LC) fertilizer, soil-repairing agent, biological pesticide, farm-oriented mulch, fodder additives, livestock and poultry and aquatic feeds etc. can be produced, also can be used for pharmaceutical industries, through the purifying of xanthohumic acid, the extraction of superclass melanocyte and prepare in order to develop multiple specific medicament and healthcare products with other drug.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention;
Fig. 2 is the structural representation that embodiment uses quadruple effect falling-film evaporator;
Fig. 3 is the structural representation that embodiment uses spray-dryer.
Embodiment
Below by embodiment, the present invention will be further described.
Embodiment 1
(1) sugarcane raw material gained alcohol waste mash is controlled at 80 DEG C, and with aqua calcis adjust ph=6 of any concentration;
(2) alcohol waste mash after step (1) being regulated carries out evaporation concentration in quadruple effect falling-film evaporator, and its alcohol waste mash is with 80 DEG C of chargings, and the pressure that passes into of saturation steam is 0.4Mpa, and evaporation concentration is until obtain the concentrated solution that brix is 55%; The moisture that period collects is soft water, and can be directly used in boiler feed water, obtained steam is the recycle of evaporation concentration link again;
(3) be 180 DEG C of granular biological humics carrying out in spray-dryer that under the sinking speed of 400mm/s spraying dry obtains 0.35mm granularity by the concentrated solution of step (2) with temperature.
In gained biological humic, total humic acid is that wherein xanthohumic acid is 71.22wt% to 74.22wt%(, dark brown humic acids is 3wt%), K
2o is 16.08wt%, P
2o is 3.5wt%, flavones is 3.2wt%.
Embodiment 2
(1) sugarcane raw material gained alcohol waste mash is controlled at 85 DEG C, and with aqua calcis adjust ph=6.3 of any concentration;
(2) alcohol waste mash after step (1) being regulated carries out evaporation concentration in quadruple effect falling film evaporation mode, and its alcohol waste mash is with 85 DEG C of chargings, and the pressure that passes into of saturation steam is 0.6Mpa, and evaporation concentration is until obtain the concentrated solution that brix is 52%; The moisture that period collects is soft water, and can be directly used in boiler feed water, obtained steam is the recycle of evaporation concentration link again;
(3) be 190 DEG C of granular biological humics carrying out that under the sinking speed of 350mm/s spraying dry obtains 0.35mm granularity by the concentrated solution of step (2) with temperature.
In gained biological humic, total humic acid is that wherein xanthohumic acid is 77wt% to 80wt%(, dark brown humic acids is 3wt%), K
2o is 15wt%, P
2o is 2wt%, flavones is 3wt%.
Embodiment 3
(1) sugarcane raw material gained alcohol waste mash is controlled at 90 DEG C, and with aqua calcis adjust ph=5.8 of any concentration;
(2) alcohol waste mash after step (1) being regulated carries out evaporation concentration in quadruple effect falling film evaporation mode, and its alcohol waste mash is with 90 DEG C of chargings, and the pressure that passes into of saturation steam is 0.8Mpa, and evaporation concentration is until obtain the concentrated solution that brix is 50; The moisture that period collects is soft water, and can be directly used in boiler feed water, obtained steam is the recycle of evaporation concentration link again;
(3) be 170 DEG C of granular biological humics carrying out that under the sinking speed of 300mm/s spraying dry obtains 0.35mm granularity by the concentrated solution of step (2) with temperature.
In gained biological humic, total humic acid is that wherein xanthohumic acid is 76wt% to 78wt%(, dark brown humic acids is 2wt%), K
2o is 15.5wt%, P
2o is 3.4wt%, flavones is 3.1wt%.
Claims (7)
1. from alcohol waste mash, extract a method for biological humic, it is characterized in that through following each step:
(1) alcohol waste mash is controlled at 80 ~ 90 DEG C, and adjust ph=5.8 ~ 6.3;
(2) it is the concentrated solution of 50 ~ 55% that the alcohol waste mash after step (1) being regulated carries out evaporation concentration to brix;
(3) granular biological humic is obtained by spray-dried for the concentrated solution of step (2).
2. method according to claim 1, is characterized in that: the adjust ph of described step (1) regulates with alkali lye.
3. method according to claim 2, is characterized in that: described alkali lye is the aqua calcis of any concentration.
4. method according to claim 1, is characterized in that: the evaporation concentration of described step (2) is carried out in quadruple effect falling film evaporation mode: alcohol waste mash is with 80 ~ 90 DEG C of chargings, and the pressure that passes into of saturation steam is 0.4 ~ 0.8Mpa.
5. method according to claim 1, is characterized in that: the moisture that in described step (2), evaporation concentration is collected is soft water, can be directly used in boiler feed water.
6. method according to claim 1, is characterized in that: the temperature controlling concentrated solution in described step (3) during spraying dry is 170 ~ 190 DEG C and sprays.
7. method according to claim 1, is characterized in that: in described step (3), spraying dry is the particle making concentrated solution form 0.35mm granularity under the sinking speed of 300 ~ 400mm/s.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109260225A (en) * | 2018-11-26 | 2019-01-25 | 萍乡市乐乐腐植酸厂 | A method of utilizing Flavonoid substances in ultrasonic wave extraction fulvic acid |
| CN109574759A (en) * | 2019-01-31 | 2019-04-05 | 安徽顺利生物有限公司 | A kind of preparation method of L-Ascorbic Acid L-O-Phosphate composite water conservation slow-release fertilizer |
| CN112657220A (en) * | 2020-12-25 | 2021-04-16 | 新疆冠农果茸股份有限公司 | Method for preparing fulvic acid dry powder from waste mash of alcohol |
| CN113319110A (en) * | 2021-05-18 | 2021-08-31 | 昆明理工大学 | Method for restoring heavy metal contaminated soil and increasing fertilizer by spraying waste mash of alcohol |
| CN113372571A (en) * | 2021-07-05 | 2021-09-10 | 云南紫辰集团生物科技有限公司 | Production process of potassium fulvate dry powder |
-
2015
- 2015-01-21 CN CN201510027740.9A patent/CN104530447A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109260225A (en) * | 2018-11-26 | 2019-01-25 | 萍乡市乐乐腐植酸厂 | A method of utilizing Flavonoid substances in ultrasonic wave extraction fulvic acid |
| CN109574759A (en) * | 2019-01-31 | 2019-04-05 | 安徽顺利生物有限公司 | A kind of preparation method of L-Ascorbic Acid L-O-Phosphate composite water conservation slow-release fertilizer |
| CN112657220A (en) * | 2020-12-25 | 2021-04-16 | 新疆冠农果茸股份有限公司 | Method for preparing fulvic acid dry powder from waste mash of alcohol |
| CN113319110A (en) * | 2021-05-18 | 2021-08-31 | 昆明理工大学 | Method for restoring heavy metal contaminated soil and increasing fertilizer by spraying waste mash of alcohol |
| CN113319110B (en) * | 2021-05-18 | 2023-01-24 | 昆明理工大学 | Method for restoring heavy metal contaminated soil and increasing fertilizer by spraying waste mash of alcohol |
| CN113372571A (en) * | 2021-07-05 | 2021-09-10 | 云南紫辰集团生物科技有限公司 | Production process of potassium fulvate dry powder |
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Application publication date: 20150422 |
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