CN108395337A - A kind of preparation method of diatom soil matrix anti-caking agent for fertilizer - Google Patents

A kind of preparation method of diatom soil matrix anti-caking agent for fertilizer Download PDF

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Publication number
CN108395337A
CN108395337A CN201810539105.2A CN201810539105A CN108395337A CN 108395337 A CN108395337 A CN 108395337A CN 201810539105 A CN201810539105 A CN 201810539105A CN 108395337 A CN108395337 A CN 108395337A
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fertilizer
caking agent
soil matrix
diatomite
temperature
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CN201810539105.2A
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郭迎庆
林茂梅
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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
    • C05G3/20Mixtures of one or more fertilisers with additives not having a specially fertilising activity for preventing the fertilisers being reduced to powder; Anti-dusting additives
    • 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
    • C05G5/00Fertilisers characterised by their form
    • C05G5/30Layered or coated, e.g. dust-preventing coatings

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

Abstract

The present invention relates to a kind of preparation methods of diatom soil matrix anti-caking agent for fertilizer, belong to anticaking agent preparing technical field.The present invention is using inert powder diatomite as raw material, ultrasonic immersing is blended in itself and ethanol solution, it is freezed again with liquid nitrogen spraying, ball mill grinding obtains pretreatment diatomite powder after freezing, will soybean oil and natto be blended after be put into it is mouldy rancid under conditions of high temperature and humidity, it is sealed by fermentation after again mixing rancid product and pretreatment diatomite powder, finally fermentate and EDTA are blended and carry out high-temperature high-voltage reaction, finally obtained diatom soil matrix anti-caking agent for fertilizer, after anti-caking agent for fertilizer dispersibility produced by the present invention, water proofing property is good, preventing blocking effect is good and function and effect are lasting, it has broad application prospects.

Description

A kind of preparation method of diatom soil matrix anti-caking agent for fertilizer
Technical field
The present invention relates to a kind of preparation methods of diatom soil matrix anti-caking agent for fertilizer, belong to anticaking agent technology of preparing neck Domain.
Background technology
Fertilizer caking refers to that chemical fertilizer granule is bonded together the phenomenon that forming block.Currently used chemical fertilizer, especially High nutrient chemical fertilizer, generally can all lump.The variation of the case where fertilizer caking extensively generally can be divided into greatly 3 kinds very much:Slight caking, serious knot Block and part are lumpd.The chemical fertilizer slightly to lump can be affranchised flow regime by slight vibration;Serious caking be whole bag or Whole heap chemical fertilizer has formed a bulk when in bulk, and chemical fertilizer is difficult to break into pieces at this time;Part caking is that part chemical fertilizer has formed fritter, this Kind caking is the most unfavorable to mechanical fertilization, because these fritters easily block nozzle and are not easy to be found.It can be seen that fertilizer caking Serious inconvenience can be brought to chemical fertilizer transport, storage and fertilising, also just at the mark of measurement chemical fertilizer products quality whether fertilizer caking One of standard.Fertilizer caking not only carrys out prodigious puzzlement to the storage of chemical fertilizer and conveyer belt, but also can influence fertilising operation and chemical fertilizer Effect.
Inert powder is wrapped in chemical fertilizer granule surface in a manner of physical absorption, reduces the contact between chemical fertilizer granule, weakens Chemical fertilizer plays the role of insulation blocking to the absorption of outside moisture and the volatilization of self component to chemical fertilizer.However, inert powder It itself is easy to reunite and absorb water, uses it as anticaking agent merely, preventing blocking effect is poor and function and effect are not lasting.
Therefore, a kind of good dispersion is invented, is not absorbed water, the novel diatomite base that preventing blocking effect is good and action time is permanent Anti-caking agent for fertilizer has positive meaning.
Invention content
Present invention mainly solves the technical issues of, for current inert powder class anti-caking agent for fertilizer itself be easy reunite simultaneously And absorb water, anticaking agent, preventing blocking effect difference and the unabiding defect of function and effect are used it as merely, provide a kind of silicon The preparation method of diatomaceous earth base anti-caking agent for fertilizer.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is:
A kind of preparation method of diatom soil matrix anti-caking agent for fertilizer, it is characterised in that specifically preparation process is:
(1)It is fitted into sonic oscillation instrument after the ethanol solution of diatomite and mass fraction 50% is mixed, oscillation dipping, dipping knot It is filtered after beam, isolated dipping filter residue, freezes 3~5min with liquid nitrogen spraying immediately;
(2)It after waiting for above-mentioned spray refrigeration, is put into ball grinder, is 20 by ball material mass ratio:1 oxidation is added into ball grinder Zirconium ball milling pearl crosses 200 mesh sieve after grinding 3~5h, and it is to pre-process diatomite powder to collect sieving powder, spare;
(3)It is fitted into stainless steel pallet after soybean oil and natto are mixed, then stainless steel pallet is put into greenhouse, stand acid It loses, obtains rancid product;
(4)It is fitted into fermentation tank, is first stirred with stirring rod anti-after above-mentioned rancid product and spare pretreatment diatomite are mixed After answering 2~3h, sealed fermenter, standing for fermentation obtains fermentate;
(5)It is fitted into high-temperature high-pressure reaction kettle after above-mentioned fermentate and ethylenediamine tetra-acetic acid are mixed, high-temperature high-voltage reaction;
(6)Wait for it is above-mentioned after reaction, take out reaction product filtering, isolated reaction filter cake rinses 3 repeatedly with absolute ethyl alcohol It is put into baking oven after~5 times, discharges to get diatom soil matrix anti-caking agent for fertilizer after dry.
Step(1)Described in diatomite and mass fraction 50% ethanol solution mass ratio be 1:8, vibrate dipping Frequency is 25~30kHz, and the time for vibrating dipping is 5~8h.
Step(3)Described in soybean oil and natto mass ratio be 10:1, the temperature in greenhouse is 35~45 DEG C, air phase It is 60~70% to humidity, it is 10~15 days to stand the rancid time.
Step(4)Described in rancid product and to pre-process diatomaceous mass ratio be 5:1, the temperature of standing for fermentation is 25 ~35 DEG C, the time of standing for fermentation is 7~9 days.
Step(5)Described in fermentate and ethylenediamine tetra-acetic acid mass ratio be 10:1, the pressure of high-temperature high-voltage reaction Temperature for 2.5~3.0MPa, high-temperature high-voltage reaction is 220~250 DEG C, and the time of high-temperature high-voltage reaction is 3~5h.
Step(6)Described in drying temperature be 70~80 DEG C, drying time be 5~8h.
The beneficial effects of the invention are as follows:
Ultrasonic immersing is blended using inert powder diatomite as raw material, by itself and ethanol solution in the present invention, then cold with liquid nitrogen spraying Freeze, after freezing ball mill grinding obtain pretreatment diatomite powder, will soybean oil and natto be blended after be put into the item of high temperature and humidity It is mouldy rancid under part, then be sealed by fermentation after rancid product and pretreatment diatomite powder are mixed, finally by fermentate and EDTA It is blended and carries out high-temperature high-voltage reaction, finally obtained diatom soil matrix anti-caking agent for fertilizer, the present invention is by ethanol solution to diatomite Surface carries out hydroxylating modification, and crushes diatomite using the ice effect of splitting, and then vegetable oil and natto rich in mould are blended, It is rancid under conditions of high temperature and humidity, the rancid product rich in acid, ester is generated, then rancid product and pretreatment diatomite are blended Lipid degradation in product spoiled by rancid oil or fat is generated a large amount of free property ester groups using microorganism, and is introduced into diatom by fermentation Native surface, while esterification occurs using the acid of rancid product and the hydroxyl on diatomite surface, to shield diatomite surface Polar hydroxyl groups, greatly reduce the surface energy of diatomite particle so that diatomite particle is in stable dispersity, keeps away Exempt from the agglomeration using process, the ester group introduced to diatomite surface in esterification and fermentation process can improve Diatomaceous hydrophobicity compensates for the defect that traditional diatomite is easy moisture absorption, finally under the action of high temperature and pressure and EDTA, So that the part metals ion removing on diatomite surface, into the organic phase of rancid product, to be produced on diatomite lattice Raw hole, improves diatomaceous physics and chemism so that final anticaking agent obtained has more excellent anti-caking Performance improves its anti-caking time limit, and anti-caking agent for fertilizer produced by the present invention has good dispersibility and hydrophobicity, can be persistently It is uniformly coated on chemical fertilizer surface, hydrophobic film is formed on chemical fertilizer surface, physically better buffer action is played to chemical fertilizer, is had Have broad application prospects.
Specific implementation mode
It is 1 in mass ratio:8 will be fitted into after the mixing of the ethanol solution of diatomite and mass fraction 50% in sonic oscillation instrument, with The hunting of frequency of 25~30kHz impregnates 5~8h, is filtered after dipping, isolated dipping filter residue, uses liquid nitrogen spraying cold immediately Freeze 3~5min;It after waiting for spray refrigeration, is put into ball grinder, is 20 by ball material mass ratio:1 oxidation is added into ball grinder Zirconium ball milling pearl crosses 200 mesh sieve after grinding 3~5h, and it is to pre-process diatomite powder to collect sieving powder, spare;By matter Amount is than being 10:1 will be fitted into after soybean oil and natto mixing in stainless steel pallet, then it is 35~45 that stainless steel pallet, which is put into temperature, DEG C, in the greenhouse that relative air humidity is 60~70%, rancid 10~15 days are stood, rancid product is obtained;By rancid product and standby Pretreatment diatomite is 5 in mass ratio:It is fitted into fermentation tank after 1 mixing, it is close after being first stirred to react 2~3h with stirring rod Seal fermentation tank is left to ferment 7~9 days at being 25~35 DEG C in temperature and obtains fermentate;Fermentate and ethylenediamine tetra-acetic acid are pressed Mass ratio is 10:It is fitted into high-temperature high-pressure reaction kettle after 1 mixing, pressure is to 2.5~3.0MPa in raising reaction kettle, and heats liter Temperature is to 220~250 DEG C, 3~5h of high-temperature high-voltage reaction;It waits for after reaction, taking out reaction product filtering, isolated reaction filter Cake is put into baking oven after rinsing 3~5 times repeatedly with absolute ethyl alcohol, discharges to get diatomite after dry 5~8h at 70~80 DEG C Base anti-caking agent for fertilizer.
It is 1 in mass ratio:8 will be fitted into after the mixing of the ethanol solution of diatomite and mass fraction 50% in sonic oscillation instrument, with The hunting of frequency of 25kHz impregnates 5h, is filtered after dipping, isolated dipping filter residue, freezes 3min with liquid nitrogen spraying immediately; It after waiting for spray refrigeration, is put into ball grinder, is 20 by ball material mass ratio:1 zirconium oxide ball milling pearl is added into ball grinder, grinds It is milled after broken 3h and crosses 200 mesh sieve, it is to pre-process diatomite powder to collect sieving powder, spare;It is 10 in mass ratio:1 will be big It is fitted into stainless steel pallet after soya-bean oil and natto mixing, then it is 35 DEG C that stainless steel pallet, which is put into temperature, relative air humidity is In 60% greenhouse, rancid 10 days are stood, rancid product is obtained;In mass ratio by rancid product and spare pretreatment diatomite It is 5:It is fitted into fermentation tank after 1 mixing, after being first stirred to react 2h with stirring rod, sealed fermenter is stood at being 25 DEG C in temperature Fermentation obtains fermentate in 7 days;It is 10 in mass ratio by fermentate and ethylenediamine tetra-acetic acid:It is packed into high-temperature high-voltage reaction after 1 mixing In kettle, pressure is to 2.5MPa in raising reaction kettle, and is heated to 220 DEG C, high-temperature high-voltage reaction 3h;It waits for after reaction, Reaction product filtering is taken out, isolated reaction filter cake is put into baking oven after rinsing 3 times repeatedly with absolute ethyl alcohol, is done at 70 DEG C Discharging is to get diatom soil matrix anti-caking agent for fertilizer after dry 5h.
It is 1 in mass ratio:8 will be fitted into after the mixing of the ethanol solution of diatomite and mass fraction 50% in sonic oscillation instrument, with The hunting of frequency of 28kHz impregnates 7h, is filtered after dipping, isolated dipping filter residue, freezes 4min with liquid nitrogen spraying immediately; It after waiting for spray refrigeration, is put into ball grinder, is 20 by ball material mass ratio:1 zirconium oxide ball milling pearl is added into ball grinder, grinds It is milled after broken 4h and crosses 200 mesh sieve, it is to pre-process diatomite powder to collect sieving powder, spare;It is 10 in mass ratio:1 will be big It is fitted into stainless steel pallet after soya-bean oil and natto mixing, then it is 40 DEG C that stainless steel pallet, which is put into temperature, relative air humidity is In 65% greenhouse, rancid 13 days are stood, rancid product is obtained;In mass ratio by rancid product and spare pretreatment diatomite It is 5:It is fitted into fermentation tank after 1 mixing, after being first stirred to react 2h with stirring rod, sealed fermenter is stood at being 30 DEG C in temperature Fermentation obtains fermentate in 8 days;It is 10 in mass ratio by fermentate and ethylenediamine tetra-acetic acid:It is packed into high-temperature high-voltage reaction after 1 mixing In kettle, pressure is to 2.8MPa in raising reaction kettle, and is heated to 235 DEG C, high-temperature high-voltage reaction 4h;It waits for after reaction, Reaction product filtering is taken out, isolated reaction filter cake is put into baking oven after rinsing 4 times repeatedly with absolute ethyl alcohol, is done at 75 DEG C Discharging is to get diatom soil matrix anti-caking agent for fertilizer after dry 7h.
It is 1 in mass ratio:8 will be fitted into after the mixing of the ethanol solution of diatomite and mass fraction 50% in sonic oscillation instrument, with The hunting of frequency of 30kHz impregnates 8h, is filtered after dipping, isolated dipping filter residue, freezes 5min with liquid nitrogen spraying immediately; It after waiting for spray refrigeration, is put into ball grinder, is 20 by ball material mass ratio:1 zirconium oxide ball milling pearl is added into ball grinder, grinds It is milled after broken 5h and crosses 200 mesh sieve, it is to pre-process diatomite powder to collect sieving powder, spare;It is 10 in mass ratio:1 will be big It is fitted into stainless steel pallet after soya-bean oil and natto mixing, then it is 45 DEG C that stainless steel pallet, which is put into temperature, relative air humidity is In 70% greenhouse, rancid 15 days are stood, rancid product is obtained;In mass ratio by rancid product and spare pretreatment diatomite It is 5:It is fitted into fermentation tank after 1 mixing, after being first stirred to react 3h with stirring rod, sealed fermenter is stood at being 35 DEG C in temperature Fermentation obtains fermentate in 9 days;It is 10 in mass ratio by fermentate and ethylenediamine tetra-acetic acid:It is packed into high-temperature high-voltage reaction after 1 mixing In kettle, pressure is to 3.0MPa in raising reaction kettle, and is heated to 250 DEG C, high-temperature high-voltage reaction 5h;It waits for after reaction, Reaction product filtering is taken out, isolated reaction filter cake is put into baking oven after rinsing 5 times repeatedly with absolute ethyl alcohol, is done at 80 DEG C Discharging is to get diatom soil matrix anti-caking agent for fertilizer after dry 8h.
The modified hydrotalcite anti-caking agent for fertilizer that reference examples are produced with company of Henan Province example as a contrast
Modified hydrotalcite anti-caking agent for fertilizer in diatom soil matrix anti-caking agent for fertilizer produced by the present invention and reference examples is carried out Performance detection, testing result are as shown in table 1:
1 performance test results of table
It can be seen from detection data in upper table after anti-caking agent for fertilizer dispersibility produced by the present invention, water proofing property is good, anti-caking Effect is good and function and effect are lasting, has broad application prospects.

Claims (6)

1. a kind of preparation method of diatom soil matrix anti-caking agent for fertilizer, it is characterised in that specifically preparation process is:
(1)It is fitted into sonic oscillation instrument after the ethanol solution of diatomite and mass fraction 50% is mixed, oscillation dipping, dipping knot It is filtered after beam, isolated dipping filter residue, freezes 3~5min with liquid nitrogen spraying immediately;
(2)It after waiting for above-mentioned spray refrigeration, is put into ball grinder, is 20 by ball material mass ratio:1 oxidation is added into ball grinder Zirconium ball milling pearl crosses 200 mesh sieve after grinding 3~5h, and it is to pre-process diatomite powder to collect sieving powder, spare;
(3)It is fitted into stainless steel pallet after soybean oil and natto are mixed, then stainless steel pallet is put into greenhouse, stand acid It loses, obtains rancid product;
(4)It is fitted into fermentation tank, is first stirred with stirring rod anti-after above-mentioned rancid product and spare pretreatment diatomite are mixed After answering 2~3h, sealed fermenter, standing for fermentation obtains fermentate;
(5)It is fitted into high-temperature high-pressure reaction kettle after above-mentioned fermentate and ethylenediamine tetra-acetic acid are mixed, high-temperature high-voltage reaction;
(6)Wait for it is above-mentioned after reaction, take out reaction product filtering, isolated reaction filter cake rinses 3 repeatedly with absolute ethyl alcohol It is put into baking oven after~5 times, discharges to get diatom soil matrix anti-caking agent for fertilizer after dry.
2. a kind of preparation method of diatom soil matrix anti-caking agent for fertilizer according to claim 1, it is characterised in that:Step (1)Described in diatomite and mass fraction 50% ethanol solution mass ratio be 1:8, vibrate dipping frequency be 25~ 30kHz, the time for vibrating dipping are 5~8h.
3. a kind of preparation method of diatom soil matrix anti-caking agent for fertilizer according to claim 1, it is characterised in that:Step (3)Described in soybean oil and natto mass ratio be 10:1, the temperature in greenhouse is 35~45 DEG C, relative air humidity is 60~ 70%, it is 10~15 days to stand the rancid time.
4. a kind of preparation method of diatom soil matrix anti-caking agent for fertilizer according to claim 1, it is characterised in that:Step (4)Described in rancid product and to pre-process diatomaceous mass ratio be 5:1, the temperature of standing for fermentation is 25~35 DEG C, is stood The time of fermentation is 7~9 days.
5. a kind of preparation method of diatom soil matrix anti-caking agent for fertilizer according to claim 1, it is characterised in that:Step (5)Described in fermentate and ethylenediamine tetra-acetic acid mass ratio be 10:1, the pressure of high-temperature high-voltage reaction is 2.5~ The temperature of 3.0MPa, high-temperature high-voltage reaction are 220~250 DEG C, and the time of high-temperature high-voltage reaction is 3~5h.
6. a kind of preparation method of diatom soil matrix anti-caking agent for fertilizer according to claim 1, it is characterised in that:Step (6)Described in drying temperature be 70~80 DEG C, drying time be 5~8h.
CN201810539105.2A 2018-05-30 2018-05-30 A kind of preparation method of diatom soil matrix anti-caking agent for fertilizer Pending CN108395337A (en)

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Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101450878A (en) * 2007-11-29 2009-06-10 襄樊隆福矿业有限公司 Anti-caking agent for mineral composite fertilizer and production method and use thereof
FR2938261A1 (en) * 2008-11-13 2010-05-14 Arkema France MANUFACTURE OF CARBOXYLIC ACID VINYL ETHYLENE / ESTER COPOLYMERS FROM RENEWABLE MATERIALS, COPOLYMERS OBTAINED AND USES THEREOF
CN101745347A (en) * 2010-01-12 2010-06-23 湖北富邦化工科技有限公司 Method for surface modification of kieselguhr powder
CN105294313A (en) * 2015-12-02 2016-02-03 中国地质科学院郑州矿产综合利用研究所 Low-grade talc fertilizer anti-caking agent and preparation method and application thereof
CN105409946A (en) * 2015-12-01 2016-03-23 雷春生 Method for preparing pesticide auxiliary by use of spent bleaching clay
CN105503380A (en) * 2015-12-12 2016-04-20 常州大学 Preparation method of degradable fertilizer anti-caking agent
CN106478250A (en) * 2016-10-11 2017-03-08 常州市鼎日环保科技有限公司 A kind of preparation method of degradable anti-caking agent for fertilizer
CN106492750A (en) * 2016-10-21 2017-03-15 常州市鼎升环保科技有限公司 A kind of preparation method of mesoporous cattle manure charcoal heavy-metal adsorption material
CN108084805A (en) * 2017-12-06 2018-05-29 田秋珍 A kind of preparation method of water proof type diatom ooze coating

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101450878A (en) * 2007-11-29 2009-06-10 襄樊隆福矿业有限公司 Anti-caking agent for mineral composite fertilizer and production method and use thereof
FR2938261A1 (en) * 2008-11-13 2010-05-14 Arkema France MANUFACTURE OF CARBOXYLIC ACID VINYL ETHYLENE / ESTER COPOLYMERS FROM RENEWABLE MATERIALS, COPOLYMERS OBTAINED AND USES THEREOF
CN101745347A (en) * 2010-01-12 2010-06-23 湖北富邦化工科技有限公司 Method for surface modification of kieselguhr powder
CN105409946A (en) * 2015-12-01 2016-03-23 雷春生 Method for preparing pesticide auxiliary by use of spent bleaching clay
CN105294313A (en) * 2015-12-02 2016-02-03 中国地质科学院郑州矿产综合利用研究所 Low-grade talc fertilizer anti-caking agent and preparation method and application thereof
CN105503380A (en) * 2015-12-12 2016-04-20 常州大学 Preparation method of degradable fertilizer anti-caking agent
CN106478250A (en) * 2016-10-11 2017-03-08 常州市鼎日环保科技有限公司 A kind of preparation method of degradable anti-caking agent for fertilizer
CN106492750A (en) * 2016-10-21 2017-03-15 常州市鼎升环保科技有限公司 A kind of preparation method of mesoporous cattle manure charcoal heavy-metal adsorption material
CN108084805A (en) * 2017-12-06 2018-05-29 田秋珍 A kind of preparation method of water proof type diatom ooze coating

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Application publication date: 20180814