CN104496641A - Zinc humate synergistic fertilizer and preparation method thereof - Google Patents

Zinc humate synergistic fertilizer and preparation method thereof Download PDF

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Publication number
CN104496641A
CN104496641A CN201410700516.7A CN201410700516A CN104496641A CN 104496641 A CN104496641 A CN 104496641A CN 201410700516 A CN201410700516 A CN 201410700516A CN 104496641 A CN104496641 A CN 104496641A
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CN
China
Prior art keywords
humic acids
zinc
preparation
fertilizer
increment
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
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CN201410700516.7A
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Chinese (zh)
Inventor
汤广斌
李丰登
孙长城
桑书梅
李伟萍
韩娟
邓欢
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HENAN HONGKANG ENVIRONMENTAL PROTECTION TECHNOLOGY Co Ltd
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HENAN HONGKANG ENVIRONMENTAL PROTECTION TECHNOLOGY Co Ltd
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Priority to CN201410700516.7A priority Critical patent/CN104496641A/en
Publication of CN104496641A publication Critical patent/CN104496641A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05GMIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
    • C05G3/00Mixtures of one or more fertilisers with additives not having a specially fertilising activity
    • C05G3/80Soil conditioners
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05DINORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
    • C05D9/00Other inorganic fertilisers

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Soil Sciences (AREA)
  • Pest Control & Pesticides (AREA)
  • Fertilizers (AREA)

Abstract

The invention discloses a preparation method of zinc humate synergistic fertilizer. The preparation method comprises the following steps of mixing humic acid and water according to a mass ratio of 1: (4-6), adjusting a pH value to 5.65-5.85 by hydrochloric acid or sulfuric acid with a concentration of 8-12wt%, adding a zinc sulfate heptahydrate solution with a concentration of 10wt% into the mixture, wherein the mass of the zinc sulfate heptahydrate solution is 2.5-3 times that of the water, carrying out a reaction process at a temperature of 70-80 DEG C for 2-3h, carrying out drying at a temperature of 75-85 DEG C and carrying out grinding. The preparation method has simple and easy processes. A method for extraction of humic acid from brown coal by a base-dissolving acidification technology has a high extraction rate and simple processes. The preparation method has good chelating reaction effects and has a chelating rate more than 90%. The zinc humate synergistic fertilizer can be mixed with other common chemical fertilizer according to a certain ratio. An experiment proves that the zinc humate synergistic fertilizer has fertilizer efficiency better than that of the common chemical fertilizer and can improve soil.

Description

A kind of zinc humic acids increment is fertile and preparation method thereof
Technical field
The invention belongs to and belong to technical field of fertilizer, be specifically related to the synthetic method that a kind of zinc rotten acid increment is fertile.
Background technology
Scientific agricultural planting shows, be supplied to the various nutrient elements needed for healthy growth of crops, depend on multi-functional, the Composite of fertilizer, the acts and efforts for expediency only in this way effectively could controlling single chemical Term Fertilization increment and the land deterioration trend caused thus.According to domestic and foreign literature, humic acids is a kind of good soil improvement agent, and it is lower as fertilizer efficiency during fertilizer separately, but with chemical fertilizer with the use of time not only can improve chemical fertilizer utilization ratio, strengthen the fertilizer efficiency of chemical fertilizer, can also soil be improved, culture fertility.In addition humic acids or the amendment of medium trace element, sequestrant, have the effect of synergy to micro-fertilizer.Zinc element is also indispensable in crop growthing development process, plays an important role to the various biochemical reaction in plant materials and protein synthesis.Therefore, after humic acids and trace element zinc chelating, the output that greatly can improve farm crop in common fertilizer is added into.
Trace element conventional in current agriculture production is manured into soil mainly with inorganic salt form, very easily deteriorates to indissoluble salt, its utilization ratio is reduced and even all lost efficacy.And humic acids in its chemical structure with a large amount of active groups, and the carboxyl higher with stability and phenolic hydroxyl group are key structural feature, can and metal ion between there is sequestering action, become fulvo acid chelated microelement, thus improve plant to the peanut of trace element.The manufacturer of the rotten sour enhanced fertilizer of synthesis zinc is a lot, but some focus on the diversity of trace element, and focus on humic acids and micro-sequestering action, the absorption rate that result in trace element is low, reduces the effect of fertilizer efficiency.
Summary of the invention
The object of the present invention is to provide a kind of zinc humic acids to rise in value fertile, the preparation method of this increment fertilizer is provided simultaneously.
For achieving the above object, the present invention adopts following technical scheme:
The preparation method that a kind of zinc humic acids increment is fertile, comprise the following steps: by humic acids and water 1:(4-6 in mass ratio) mix after, by the hydrochloric acid of 8-12 wt % or sulfuric acid adjust ph to 5.65-5.85, then the Zinc vitriol solution of the quality 2.5-3 10 wt % doubly of water is added, 70-80 DEG C of reaction 2-3h, 75-85 DEG C of oven dry afterwards, grind after be zinc humic acids finished product.
In aforesaid method, described humic acids utilizes alkali-soluble acid analysis method to extract from brown coal.
Utilize alkali-soluble acid analysis method from brown coal, extract humic acids specifically to comprise the following steps: will the brown coal of 80-100 mesh sieve be crossed after 60-70 DEG C of dry 2-3h, the sulphuric acid soln adding 15 ~ 20wt% soaks 8-12h, filter residue is stayed in filtration, sodium hydroxide solution to the liquid-solid mass ratio adding 1-2 wt % in filter residue is (8-12): 1, then 60-90min is reacted at 60-70 DEG C, carry out centrifugal after being cooled to 20-30 DEG C, the centrifugal 5-10min of 3000-4000r/min, collect supernatant liquor, the sulphur acid for adjusting pH adding 15-20 wt % in supernatant liquor separates out precipitation to 2-3, then carry out suction filtration and obtain filter cake, after using 20-50ml distilled water wash again, 60-70 DEG C of oven dry, obtain humic acids, wherein total humic acid content is greater than 70%, moisture is less than 10%, belong to first grade, the add-on of the sulphuric acid soln of described 15-20wt% flooded brown coal.
Major advantage of the present invention has: method is easy and simple to handle, simple.Utilizing alkali-soluble acid analysis method from brown coal, extract humic acids is a kind of high and fairly simple method of extraction yield.The chelatropic reaction condition optimizing by experiment of the inventive method, the effect of chelatropic reaction is very good, and chelation percent can reach more than 90%.The zinc that utilizes aforesaid method to prepare rotten acid increment fertilizer can add by a certain percentage with other common chemical fertilizer and mixes, better than the fertilizer efficiency of common chemical fertilizer through experimental verification, and has the benefit of improvement soil.
Embodiment
Below in conjunction with embodiment, the present invention is described further, but protection scope of the present invention is not limited in this.
embodiment 1
By humic acids and water in mass ratio 1:4 mix, after stirring, with the salt acid for adjusting pH value to 5.65 of 10wt%, the past Zinc vitriol solution wherein adding the 10wt% of the quality 2.7 times of water, then 75 DEG C of stirred in water bath react 2 hours, put 80 DEG C of oven dry in loft drier after reaction terminates, obtain zinc humic acids finished product after grinding, the chelation percent of humic acids and zinc is 93% after testing.
embodiment 2
(1) brown coal of 90 mesh sieves will be crossed after 70 DEG C of dry 2h, the sulphuric acid soln adding the 15wt% not having brown coal soaks 10h, filter residue is stayed in filtration, sodium hydroxide solution to the liquid-solid mass ratio adding 1 wt % in filter residue is 10:1, then 75min is reacted at 65 DEG C, carry out centrifugal after being cooled to 25 DEG C, the centrifugal 5min of 4000r/min, collect supernatant liquor, the sulphuric acid soln adding 17wt % in supernatant liquor regulates pH to 2.5 to separate out precipitation, then carry out suction filtration and obtain filter cake, after using 30ml distilled water wash again, 65 DEG C of oven dry, obtain humic acids, wherein total humic acid content is greater than 70%, moisture is less than 10%, belong to first grade,
(2) humic acids step (1) obtained and water in mass ratio 1:6 mix, after stirring, with the salt acid for adjusting pH value to 5.70 of 12wt%, the past Zinc vitriol solution wherein adding the 10wt% of 3 times of quality, then 80 DEG C of stirred in water bath react 3 hours, put 85 DEG C of oven dry in loft drier after reaction terminates, obtain zinc humic acids finished product after grinding, the chelation percent of humic acids and zinc is 95% after testing.
Embodiment 3
(1) brown coal of 100 mesh sieves will be crossed after 65 DEG C of dry 2.5h, the sulphuric acid soln adding the 20wt% not having brown coal soaks 12h, filter residue is stayed in filtration, sodium hydroxide solution to the liquid-solid mass ratio adding 2wt % in filter residue is 12:1, then 90min is reacted at 70 DEG C, carry out centrifugal after being cooled to 30 DEG C, the centrifugal 10min of 3000r/min, collect supernatant liquor, the sulphuric acid soln adding 20wt % in supernatant liquor regulates pH to 3 to separate out precipitation, then carry out suction filtration and obtain filter cake, after using 30ml distilled water wash again, 70 DEG C of oven dry, obtain humic acids, wherein total humic acid content is greater than 70%, moisture is less than 10%, belong to first grade,
(2) humic acids step (1) obtained and water in mass ratio 1:5 mix, after stirring, with the salt acid for adjusting pH value to 5.75 of 10wt%, the past Zinc vitriol solution wherein adding the 10wt% of 2.5 times of quality, then 70 DEG C of stirred in water bath react 2 hours, put 75 DEG C of oven dry in loft drier after reaction terminates, obtain zinc humic acids finished product after grinding, the chelation percent of humic acids and zinc is 94% after testing.
Embodiment 4
(1) brown coal of 80 mesh sieves will be crossed after 70 DEG C of dry 3h, the sulphuric acid soln adding the 15wt% not having brown coal soaks 8h, filter residue is stayed in filtration, sodium hydroxide solution to the liquid-solid mass ratio adding 1wt % in filter residue is 8:1, then 60min is reacted at 60 DEG C, carry out centrifugal after being cooled to 30 DEG C, the centrifugal 8min of 3500r/min, collect supernatant liquor, the sulphuric acid soln adding 15wt % in supernatant liquor regulates pH to 2 to separate out precipitation, then carry out suction filtration and obtain filter cake, after using 30ml distilled water wash again, 60 DEG C of oven dry, obtain humic acids, wherein total humic acid content is greater than 70%, moisture is less than 10%, belong to first grade,
(2) humic acids step (1) obtained and water in mass ratio 1:4 mix, after stirring, by the sulfuric acid adjust ph to 5.85 of 10wt%, the past Zinc vitriol solution wherein adding the 10wt% of 3 times of quality, then 70 DEG C of stirred in water bath react 3 hours, put 80 DEG C of oven dry in loft drier after reaction terminates, obtain zinc humic acids finished product after grinding, the chelation percent of humic acids and zinc is 90% after testing.

Claims (4)

1. the preparation method that a zinc humic acids increment is fertile, it is characterized in that, comprise the following steps: by humic acids and water 1:(4-6 in mass ratio) mix after, by the hydrochloric acid of 8-12 wt % or sulfuric acid adjust ph to 5.65-5.85, then the Zinc vitriol solution of the quality 2.5-3 10 wt % doubly of water is added, 70-80 DEG C of reaction 2-3h, 75-85 DEG C of oven dry afterwards, grind after and get final product.
2. the preparation method that zinc humic acids increment as claimed in claim 1 is fertile, it is characterized in that, described humic acids utilizes alkali-soluble acid analysis method to extract from brown coal.
3. the preparation method that zinc humic acids increment as claimed in claim 2 is fertile, it is characterized in that, utilize alkali-soluble acid analysis method from brown coal, extract humic acids specifically to comprise the following steps: will the brown coal of 80-100 mesh sieve be crossed after 60-70 DEG C of dry 2-3h, the sulphuric acid soln adding 15 ~ 20wt% soaks 8-12h, filter residue is stayed in filtration, sodium hydroxide solution to the liquid-solid mass ratio adding 1-2 wt % in filter residue is (8-12): 1, then 60-90min is reacted at 60-70 DEG C, carry out centrifugal after being cooled to 20-30 DEG C, centrifugal 5 ~ the 10min of 3000 ~ 4000r/min, collect supernatant liquor, the sulphur acid for adjusting pH adding 15-20 wt % in supernatant liquor separates out precipitation to 2-3, then carry out suction filtration and obtain filter cake, after using 20-50ml distilled water wash again, 60-70 DEG C of oven dry, obtain humic acids.
4. utilize zinc humic acids prepared by the fertile preparation method of claim 1-3 arbitrary described zinc humic acids increment.
CN201410700516.7A 2014-11-28 2014-11-28 Zinc humate synergistic fertilizer and preparation method thereof Pending CN104496641A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107473860A (en) * 2017-09-22 2017-12-15 吴洪生 Method and application of the Synchronos method using zinc gray cadmia production organic zinc/iron fertilizer
CN108558583A (en) * 2018-05-16 2018-09-21 安徽中元化肥股份有限公司 Rotten sour durable composite fertilizer of a kind of zinc and preparation method thereof
CN109400347A (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 It is a kind of suitable for winter wheat or the phosphorus ammonium Humic acid synergistic support preparation method of spring maize base manure
CN110483216A (en) * 2019-08-07 2019-11-22 中海石油化学股份有限公司 A kind of special fertilizer for sugar cane and its application method

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CN1075312A (en) * 1992-02-14 1993-08-18 于国源 The production method of humic acid liquid compound fertilizer
CN1401616A (en) * 2002-07-24 2003-03-12 通辽绿阳科技开发有限公司 Liquid multi-nutrient element humic acid fertilizer and preparing process thereof
CN101768031A (en) * 2009-12-30 2010-07-07 马增禄 Preparation method of humic acid organic fertilizer
CN103936520A (en) * 2014-04-28 2014-07-23 白银市桔瑞生物科技有限公司 Ecological slow release fertilizer and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN1075312A (en) * 1992-02-14 1993-08-18 于国源 The production method of humic acid liquid compound fertilizer
CN1401616A (en) * 2002-07-24 2003-03-12 通辽绿阳科技开发有限公司 Liquid multi-nutrient element humic acid fertilizer and preparing process thereof
CN101768031A (en) * 2009-12-30 2010-07-07 马增禄 Preparation method of humic acid organic fertilizer
CN103936520A (en) * 2014-04-28 2014-07-23 白银市桔瑞生物科技有限公司 Ecological slow release fertilizer and preparation method thereof

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107473860A (en) * 2017-09-22 2017-12-15 吴洪生 Method and application of the Synchronos method using zinc gray cadmia production organic zinc/iron fertilizer
CN108558583A (en) * 2018-05-16 2018-09-21 安徽中元化肥股份有限公司 Rotten sour durable composite fertilizer of a kind of zinc and preparation method thereof
CN109400347A (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 It is a kind of suitable for winter wheat or the phosphorus ammonium Humic acid synergistic support preparation method of spring maize base manure
CN110483216A (en) * 2019-08-07 2019-11-22 中海石油化学股份有限公司 A kind of special fertilizer for sugar cane and its application method
CN110483216B (en) * 2019-08-07 2021-07-30 中海石油化学股份有限公司 Special fertilizer for sugarcane and application method thereof

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Application publication date: 20150408