CN102408456A - Preparation method of multifunctional fulvic acid substance - Google Patents

Preparation method of multifunctional fulvic acid substance Download PDF

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CN102408456A
CN102408456A CN201110284354XA CN201110284354A CN102408456A CN 102408456 A CN102408456 A CN 102408456A CN 201110284354X A CN201110284354X A CN 201110284354XA CN 201110284354 A CN201110284354 A CN 201110284354A CN 102408456 A CN102408456 A CN 102408456A
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acid
humic acids
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plant
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张常书
焦家梅
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SHANGHAI TONGWEI BIOLOGICAL SCIENCE & TECHNOLOGY CO LTD
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SHANGHAI TONGWEI BIOLOGICAL SCIENCE & TECHNOLOGY CO LTD
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Abstract

The invention discloses a preparation method of a multifunctional fulvic acid substance. The method comprises the following steps of: crushing a mineral humic acid source until the particle size is less than 60 meshes; adding water of which the amount is 4-6 times that of the crushed mineral humic acid source and 7-8% of alkaline liquid; heating, extracting and performing centrifugal separation to obtain purified humic acid; fetching 60-100% of the total amount of purified humic acid, and adding 0-40% of plant humic acid; adding an accelerant and an oxidant accounting for 1-2% and 3-10% of the total amount of humic acid respectively; performing oxidative degradation at 120-130 DEG C for 3-6 hours; and performing atomization drying to obtain the product fulvic acid. In the invention, a certain amount of biological leaven can also be added into plant humic acid to perform biological fermentation for 7-10 days to obtain biochemical fulvic acid. By combining mineral humic acid and plant humic acid at different proportions or purified by different production technologies, agricultural, livestock, medical and biochemical fulvic acid can be prepared, and obtained fulvic acid has high purity, good water solubility and high bioactivity, resists against acid, calcium and magnesium, and is a novel multifunctional fulvic acid substance.

Description

A kind of preparation method of multi-functional xanthohumic acid kind material
Technical field
The present invention relates to a kind of method that adopts mineral resources humic acids and plant-sourced humic acids to prepare multi-functional xanthohumic acid, belong to technological field of biochemistry.
Background technology
Be divided into three kinds of xanthohumic acid, ulmic acid and Ulmic acidss in the common humic acids; Wherein the xanthohumic acid molecular weight is little, and acidic-group is many, and biological activity is high, can passive plant absorbing; Water soluble, antiacid, alkali resistant, anticalcium magnesium, flocculation sediment not in the acidic medium of PH<2.
Middle nineteen seventies; China's Henan chemistry institute has found to contain in the mineral resources humic acids a kind of more low molecular xanthohumic acid; Early eighties begins to be used for wheat hot-dry wind tolerance (drought resistance agent), is widely used in agriculture prodn afterwards and makes foliage fertilizer, liquid fertilizer and medical applications.But, calcium magnesium height few because of China's xanthohumic acid resource reserve produce very difficulty, but people begins to seek new substitute.
The early 1990s, in the xanthohumic acid development and use, adopt plant-sourceds such as biofermentation technique and crop material; Produce a type xanthohumic acid material; " biochemical fulvic acid " promptly named afterwards and " biological humic " etc., alternative mineral resources xanthohumic acid and be widely used in agriculture prodn has been obtained remarkable effect.But biochemical fulvic acid is a kind of polymolecular mixture, contain that lower-molecular substance is many, chemical structure is complicated; The tunning of different resource particularly; Chemical functional group and mineral resources xanthohumic acid gap are bigger; Can not express the character of some useful chemical structure of mineral resources xanthohumic acid and functional group, therefore, people are seeking the new xanthohumic acid kind material that has mineral resources and biochemical two kinds of chemical propertys concurrently.
For a long time, people attempt through various physics and chemical treatment method, solve the suitability for industrialized production problem of xanthohumic acid, but all are difficult to so far realize.Gongxian, the domestic unique mineral resources xanthohumic acid of Hami, because of the high ferro high contents of calcium and magnesium, the extraction process difficulty is big, poor product quality, production cost is high, secular stagnation not before.Therefore, how common very abundant humic acids being changed into the xanthohumic acid kind material, is a great technical barrier, and at present domestic breakthrough does not as yet more have industrial production.
Summary of the invention
For solving the problems of the technologies described above; The present invention provides a kind of preparation method of multi-functional xanthohumic acid kind material; Adopting mineral resources humic acids and plant-sourced humic acids is raw material; Add oxygenant and promotor, and can add bio-fermentation agent according to demand and carry out biological fermentation, can develop agricultural, poultry with the xanthohumic acid of using in, the medical and other field.
The present invention realizes through following technical scheme:
A kind of preparation method of multi-functional xanthohumic acid kind material, be with mineral resources humic acids source be crushed to particle diameter less than 60 orders after, adding its total amount is 4~5 times water and 7~8% alkali lye, the extracting of heating, spinning, the mineral resources humic acids obtains purifying; Get said purification mineral resources humic acids 60~100%; To the plant-sourced humic acids that wherein adds 0~40%; Add the promotor of humic acids total amount 1~2% and 3~10% oxygenant again, oxidative degradation 3~6h under 120~130 ℃ of conditions gets the product xanthohumic acid through atomization drying.
A kind of agricultural xanthohumic acid is by said purification mineral resources humic acids 60~80%, plant-sourced humic acids 20~40%, and 5~10% oxygenant of humic acids total amount, 1~2% promotor are formed.
A kind of poultry is used xanthohumic acid, is by said purification mineral resources humic acids 70~90%, plant-sourced humic acids 10~30%, and 5~10% oxygenant of humic acids total amount, 1~2% promotor are formed.
A kind of medical xanthonumic acid is by said purification mineral resources humic acids 100%, and 3~5% oxygenant of humic acids total amount, 1~2% promotor are formed.
A kind of preparation method of agricultural xanthohumic acid: the mineral resources humic acids is pulverized less than 2mm, added 4~5 times in water, add alkali 7~8%, the extracting of heating, spinning, the humic acids of must purifying; Purification humic acids with 60~80% behind the adding plant-sourced humic acids 20~40%, adds 5~10% oxygenants again, under 120~130 ℃, through oxidative degradation 5~6 hours, after quality product reaches the xanthohumic acid technical indicator, carries out spraying drying, finished product packing again.
A kind of preparation method who raises with xanthohumic acid: with mineral resources peat composed of rotten mosses humic acids 70~90%, be crushed to 2~4mm, add 7~8% alkali extracting; Spinning, the humic acids of must purifying adds 10~30% plant humic acids in proportion; Add 5~10% oxygenant and 1~2% promotor again, under 120~130 ℃, behind oxidative degradation 3~4h; Product quality indicator is carried out spraying drying, finished product packing after reaching the standard of poultry with xanthohumic acid again.
A kind of preparation method of medical xanthonumic acid: the mineral resources humic acids is pulverized less than 60 orders; Add 4~5 times in water; Add 7~8% alkali PH=7~8 that neutralize, oxidizer 3~5% and promotor 1% again were 130 ℃ of following oxidative degradations 4~6 hours; After reaching the technical indicator of medical xanthonumic acid, carry out spraying drying, finished product packing again.
The present invention also provides a kind of preparation method of biochemical fulvic acid: adopt said plant humic acids; Add the ammoniation agent of its total amount 5~10%, 1% promotor, 0.1~0.3% bio-fermentation agent; At normal temperatures, carry out the biology aerobic solid fermentation after 10~15 days, changed the anaerobism liquid fermenting again over to 7~10 days; Reach the technical indicator of biochemical fulvic acid when quality product after, again through extracting filtration, spraying drying, finished product packing.
Beneficial effect of the present invention is: a kind of material that has biochemical and mineral resources xanthohumic acid dual-use function concurrently has solved the suitability for industrialized production problem of agricultural xanthohumic acid, medical xanthonumic acid and biochemical fulvic acid class material; Adopting mineral resources humic acids and extraordinary plant resources, utilize Measurement for Biochemistry, is xanthohumic acid and biological acid with common humic acids and organic matter transformation.These article purity height, good water solubility, ash content is low, impurity is few, activity is high, effective, can produce agricultural xanthohumic acid, medical xanthonumic acid, poultry with series product such as xanthohumic acid and biochemical fulvic acids.
Embodiment
Below in conjunction with embodiment, the present invention is further specified.
Embodiment 1
The preparation of agricultural xanthohumic acid: 150 parts of mineral resources humic acidss are pulverized particle diameter less than 2mm, add 650 parts in water, 10.5 parts in hydro-oxidation sodium, 50~60 ℃ of extractings of heating, spinning, the humic acids of must purifying; With 80 parts purification humic acids, add 20 parts of plant-sourced humic acidss after, add 5 parts of oxygenants again, under 120~130 ℃,, after quality product reaches the xanthohumic acid technical indicator, carry out spraying drying, finished product packing again through oxidative degradation 5~6 hours.
Embodiment 2
Raise preparation method: 100 parts of mineral resources peat composed of rotten mosses humic acidss are pulverized 2~4mm, add 8 parts of sodium hydroxide extractings, spinning with xanthohumic acid; The humic acids of must purifying is got 85 parts of mineral resources peat composed of rotten mosses humic acidss after the purification, adds 15 parts plant humic acids in proportion; Add oxygenant and 2 parts of promotor of 10 parts again, under 120~130 ℃, behind oxidative degradation 3~4h; Product quality indicator is carried out spraying drying, finished product packing after reaching the standard of poultry with xanthohumic acid again.
Embodiment 3
The preparation method of medical xanthonumic acid: 100 parts of mineral resources humic acidss are pulverized less than 60mm; Add 500 parts in water, add 7.5 parts of sodium hydroxide, the PH=7 that neutralizes~8; 3 parts of oxidizer and promotor 1% again; 130 ℃ of following oxidative degradations 4~6 hours, reach the technical indicator of medical xanthonumic acid after, carry out spraying drying, finished product packing again.
Embodiment 4
The preparation method of biochemical fulvic acid: adopt 100 parts of said plant humic acidss; Add the ammoniation agent of its total amount 5~10%, 1% promotor, 0.1~0.3% bio-fermentation agent; At normal temperatures, carry out the biology aerobic solid fermentation after 10~15 days, changed the anaerobism liquid fermenting again over to 7~10 days; Reach the technical indicator of biochemical fulvic acid when quality product after, again through extracting filtration, spraying drying, finished product packing.
Adopt the foregoing description method to feed intake in proportion, obtain all kinds of xanthohumic acid kind material physicochemical characteristicses and technical indicator such as table 1.
Table 1
Figure BSA00000579206100051
Figure BSA00000579206100061
The xanthohumic acid product that working method of the present invention is produced can reach the xanthohumic acid technical indicator and the physico-chemical property of domestic present general requirement, its product purity height, good water solubility, ash content is low, impurity is few, activity is high, effective.

Claims (5)

1. the preparation method of a multi-functional xanthohumic acid kind material, it is characterized in that be with mineral resources humic acids source be crushed to particle diameter less than 60 orders after, adding its total amount is 4~5 times water and 7~8% alkali lye, the extracting of heating, spinning, the mineral resources humic acids obtains purifying; Get said purification mineral resources humic acids 60~100%; To the plant-sourced humic acids that wherein adds 0~40%; Add the promotor of humic acids total amount 1~2% and 3~10% oxygenant again, oxidative degradation 3~6h under 120~130 ℃ of conditions gets the product xanthohumic acid through atomization drying.
2. the preparation method of an agricultural xanthohumic acid is characterized in that the mineral resources humic acids is pulverized less than 2mm, adds 4~5 times in water, adds alkali 7~8%, the extracting of heating, spinning, the humic acids of must purifying; Purification humic acids with 60~80% behind the adding plant-sourced humic acids 20~40%, adds 5~10% oxygenants again, under 120~130 ℃, through oxidative degradation 5~6 hours, after quality product reaches the xanthohumic acid technical indicator, carries out spraying drying, finished product packing again.
3. a preparation method who raises with xanthohumic acid is characterized in that mineral resources humic acids 70~90% is crushed to 2~4mm; Add 7~8% alkali extracting, spinning, the humic acids of must purifying; Add 10~30% plant humic acids in proportion, add 5~10% oxygenant and 1~2% promotor again, under 120~130 ℃; Behind oxidative degradation 3~4h, product quality indicator is carried out spraying drying, finished product packing after reaching the standard of poultry with xanthohumic acid again.
4. the preparation method of a medical xanthonumic acid; It is characterized in that the mineral resources humic acids is pulverized less than 60 orders, add 4~5 times in water, add 7~8% alkali PH=7~8 that neutralize; Oxidizer 3~5% and promotor 1% again; 130 ℃ of following oxidative degradations 4~6 hours, reach the technical indicator of medical xanthonumic acid after, carry out spraying drying, finished product packing again.
5. the preparation method of a biochemical fulvic acid; It is characterized in that adopting said plant humic acids, add the ammoniation agent of its total amount 5~10%, 1% promotor, 0.1~0.3% bio-fermentation agent, at normal temperatures; Carry out the biology aerobic solid fermentation after 10~15 days; Changed the anaerobism liquid fermenting again over to 7~10 days, reach the technical indicator of biochemical fulvic acid when quality product after, again through extracting filtration, spraying drying, finished product packing.
CN201110284354XA 2011-09-23 2011-09-23 Preparation method of multifunctional fulvic acid substance Pending CN102408456A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103342589A (en) * 2013-07-08 2013-10-09 山东创新腐植酸科技股份有限公司 Process method for preparing high-solubility potassium fulvate dry powder
CN106432368A (en) * 2016-09-23 2017-02-22 山东农业大学 Method of efficiently extracting fulvic acid from papermaking black liquid

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20030066024A (en) * 2002-02-04 2003-08-09 주식회사 환경비젼이십일 The extraction method of humic acid and fulvic acid from outflow of biological treatment system of livestock manure waste
CN1456539A (en) * 2003-04-01 2003-11-19 刘泉 Prepartion of xanthonumic acid for agriculture
CN101423536A (en) * 2008-12-02 2009-05-06 昆明理工大学 Method for preparing humic acid and salt thereof by oxidation and degradation of brown coal
US20100010089A1 (en) * 2008-07-09 2010-01-14 Don Calvin Van Dyke System and method for production and use of fulvic acid
CN101684132A (en) * 2008-09-25 2010-03-31 唐毅 Production method and application of humic acid and fulvic acid extracted from humus and organic salts of mineral compounds thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20030066024A (en) * 2002-02-04 2003-08-09 주식회사 환경비젼이십일 The extraction method of humic acid and fulvic acid from outflow of biological treatment system of livestock manure waste
CN1456539A (en) * 2003-04-01 2003-11-19 刘泉 Prepartion of xanthonumic acid for agriculture
US20100010089A1 (en) * 2008-07-09 2010-01-14 Don Calvin Van Dyke System and method for production and use of fulvic acid
CN101684132A (en) * 2008-09-25 2010-03-31 唐毅 Production method and application of humic acid and fulvic acid extracted from humus and organic salts of mineral compounds thereof
CN101423536A (en) * 2008-12-02 2009-05-06 昆明理工大学 Method for preparing humic acid and salt thereof by oxidation and degradation of brown coal

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Title
张常书等: ""生化黄腐酸的生物活性和激素作用研究"", 《2010年中国腐植酸行业低碳经济交流大会暨第九届全国绿色环保肥料(农药)新技术、新产品交流会论文集》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103342589A (en) * 2013-07-08 2013-10-09 山东创新腐植酸科技股份有限公司 Process method for preparing high-solubility potassium fulvate dry powder
CN103342589B (en) * 2013-07-08 2014-11-12 山东创新腐植酸科技股份有限公司 Process method for preparing high-solubility potassium fulvate dry powder
CN106432368A (en) * 2016-09-23 2017-02-22 山东农业大学 Method of efficiently extracting fulvic acid from papermaking black liquid

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Application publication date: 20120411