CN109574759A - A kind of preparation method of L-Ascorbic Acid L-O-Phosphate composite water conservation slow-release fertilizer - Google Patents
A kind of preparation method of L-Ascorbic Acid L-O-Phosphate composite water conservation slow-release fertilizer Download PDFInfo
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- CN109574759A CN109574759A CN201910099003.8A CN201910099003A CN109574759A CN 109574759 A CN109574759 A CN 109574759A CN 201910099003 A CN201910099003 A CN 201910099003A CN 109574759 A CN109574759 A CN 109574759A
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES 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
- C05G5/00—Fertilisers characterised by their form
- C05G5/30—Layered or coated, e.g. dust-preventing coatings
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B17/00—Other phosphatic fertilisers, e.g. soft rock phosphates, bone meal
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES 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
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/80—Soil conditioners
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES 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
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/90—Mixtures of one or more fertilisers with additives not having a specially fertilising activity for affecting the nitrification of ammonium compounds or urea in the soil
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Abstract
The invention discloses a kind of preparation methods of L-Ascorbic Acid L-O-Phosphate composite water conservation slow-release fertilizer, are related to fertilizer preparation technical field.The water-retaining agent that the present invention is prepared as raw material by esterification using polyethylene glycol, polyglutamic acid, can add and subtract the loss of slow soil moisture, and fixed water and soil improves the fertilizer efficiency of fertilizer；Fertiliser granulates surface of the present invention is enclosed with one layer of coating, slow release, raising fertilizer efficiency can reduce cost in the soil；In addition, nitrocellulose can also release nitrogen in biodegradation process, fertilizer efficiency is further increased.
Description
Technical field:
The present invention relates to fertilizer preparation technical fields, and in particular to a kind of L-Ascorbic Acid L-O-Phosphate composite water conservation slow-release fertilizer
Preparation method.
Background technique:
Vitamin C phosphoric esterization mainly has two methods: first is that phosphorylation (such as EP Published Patent of phosphorus oxychloride
388869 and 582924, United States Patent (USP) 4179445, the descriptions such as Japanese Unexamined Patent Publication No. 60-69079), it is original with vitamin C
Material, gets up the hydroxyl protection on 5 and 6 carbon before esterification, i.e., vitamin C first carries out ketal reaction with acetone and generates 5,6-
One isopropylidene of oxygen, one L, mono- ascorbic acid (5,6-0 mono- isopropylidene-L-ascorbic acid), then use pyridine solution
Dissolution, KOH adjust pH value, and phosphorus oxychloride reaction is added dropwise, boils off multiple desalination after pyridine, are concentrated, then carry out resin cation friendship
It changes, collects eluent, MgO is added to react, last low-carbon alcohols partial crystallization filtration drying is completed.Its product is mainly L-AA -2-
Phosplate, by-product are mainly L-AA -3- phosphate and 2- pyrophosphate and two (ascorbic acid) -2,2 '-two phosphorus
Acid esters.Second method is to carry out phosphorylation using phosphate to obtain such as the method for United States Patent (USP) 4647672 and 5110950
Primary product is L-AA -2- polyphosphate, and when such as using sodium trimetaphosphate, product is L-AA -2- triphosphoric acid
Ester, but also contain a certain proportion of L-AA -2- phosplate.Both techniques are mentioned to vitamin C phosphoric ester
When pure, generated waste residue and waste liquid are typically all direct emission, will cause environmental pollution.Contain in the waste residue and waste liquid simultaneously
More inorganic ion such as calcium ion, phosphate radical etc., with for organic matters such as a small amount of vitamin C phosphoric esters, these are all can be with
It is absorbed by plant.
Summary of the invention:
It is a kind of produced during the preparation process with L-Ascorbic Acid L-O-Phosphate technical problem to be solved by the present invention lies in providing
Waste residue and liquid is raw material, and prepare high usage, quickly absorb, the preparation of composite slow-release fertilizer with certain water holding capacity
Method.
The following technical solution is employed for the technical problems to be solved by the invention to realize:
A kind of preparation method of L-Ascorbic Acid L-O-Phosphate composite water conservation slow-release fertilizer, comprising the following steps:
(1) it mixes: L-Ascorbic Acid L-O-Phosphate waste material, urea, potassium chloride, abscisic acid, water-retaining agent is sent to high speed dispersion
In machine, disperse after mixing evenly, in 30 DEG C of standing 20-30min；
(2) preparation of coating liquid: nitrocellulose is added in dehydrated alcohol, then China fir is added in 30 DEG C of stirring 15min
Wood oil and castor oil flow back insulated and stirred 0.5-2h to get coating liquid is arrived；
(3) it prepares: coating liquid uniformly being smeared, is coated in the fertiliser granulates being uniformly mixed in step (1), decompression is steamed
Recycling design is evaporated to get composite slow-release fertilizer is arrived.
The L-Ascorbic Acid L-O-Phosphate waste material, urea, potassium chloride, abscisic acid, water-retaining agent mass ratio be 40-50:5-
10:6-8:1-5:1-4.
The processing method of the L-Ascorbic Acid L-O-Phosphate waste material are as follows:
(1) L-Ascorbic Acid L-O-Phosphate waste residue produced during the preparation process, waste liquid are collected；
(2) waste residue is placed into 1-2h in 3-5 DEG C of sealing, is subsequently placed in 100-110 DEG C of baking oven and dries to constant weight, and in
500-550 DEG C of roasting 1-3h stands to room temperature, is pulverized with grinding；
(3) waste liquid is added in reaction kettle, is subsequently added into the plant amylum of waste liquid quality 20-30%, 50-60 DEG C of stirring
Then 15-30min is added Glycerin and chain initiator, 90-95 DEG C of insulated and stirred 0.5-2h is filtered, obtained solid while hot
Decontamination is washed with deionized water, it is dry to constant weight.
The Glycerin, chain initiator quality be respectively plant amylum quality 10-20%, 1-2%.
The chain initiator is peroxidating trimethylacetic acid tertiary butyl ester or di-cyclohexylperoxy di-carbonate.
Plant amylum is added in waste liquid, and under the influence of waste liquid acid ion alkali ion, plant amylum can occur micro hydrolysis and mention
The activity of high starch surface hydroxyl, then Glycerin and chain initiator are added in reaction system, Glycerin meeting and shallow lake
The hydroxy combining on powder surface enhances it to organic nutrient substance in waste liquid to extend the length and activity of starch chain
Selective absorbing is easier to be absorbed by plant using the starch by the organic nutrient substance of carrier adsorption；Modified starch simultaneously
It is easily decomposed by soil, there is certain soil-water protection effect.
The water-retaining agent the preparation method comprises the following steps: polyethylene glycol is add to deionized water, 30 DEG C of stirring 10min, then
Polyglutamic acid and tetraethyl titanate is added, flow back insulated and stirred 0.5-4h, is cooled to 70-75 DEG C of addition linseed oil stirring 20-
Decontamination is washed with deionized water in 40min, filtering, obtained solid, and 50 DEG C are dried under vacuum to constant weight.
The polyethylene glycol, polyglutamic acid, tetraethyl titanate, linseed oil mass ratio be 4-6:5-8:0.05:0.5-2.
The nitrocellulose, san-mou oil, castor oil, dehydrated alcohol mass ratio be 20-30:4-6:2-3:100-120.
The beneficial effects of the present invention are:
(1) present invention is modified plant amylum by Glycerin, makes it in L-Ascorbic Acid L-O-Phosphate waste liquid
The selective absorption of organic nutrient substance, while modified starch is easier to be decomposed by soil, there is certain water
Native protective effect can improve the dissolution efficiency of slow-release fertilizer；
(2) water-retaining agent prepared as raw material by esterification using polyethylene glycol, polyglutamic acid, can add and subtract in slow soil
The loss of moisture, fixed water and soil, improves the fertilizer efficiency of fertilizer；
(3) fertiliser granulates surface of the present invention is enclosed with one layer of coating, slow release, raising fertilizer efficiency can reduce in the soil
Cost further increases fertilizer efficiency in addition, nitrocellulose can also release nitrogen in biodegradation process.
Specific embodiment:
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below
Specific embodiment is closed, the present invention is further explained.
Embodiment 1
The preparation of composite water conservation slow-release fertilizer:
(1) it mixes: by 45 parts of L-Ascorbic Acid L-O-Phosphate waste materials, 6 parts of urea, 6 parts of potassium chloride, 3 parts of abscisic acids, 3 parts of water conservations
Agent is sent in high speed disperser, is dispersed after mixing evenly, in 30 DEG C of standing 20min；
(2) preparation of coating liquid: 25 parts of nitrocelluloses are added in 110 parts of dehydrated alcohols, 30 DEG C of stirring 15min,
Then san-mou oil and castor oil is added, flows back insulated and stirred 1h to get coating liquid is arrived；
(3) it prepares: coating liquid uniformly being smeared, is coated in the fertiliser granulates being uniformly mixed in step (1), decompression is steamed
Recycling design is evaporated to get composite slow-release fertilizer is arrived.
The processing of L-Ascorbic Acid L-O-Phosphate waste material:
(1) L-Ascorbic Acid L-O-Phosphate waste residue produced during the preparation process, waste liquid are collected；
(2) waste residue is placed into 1h in 3 DEG C of sealings, is subsequently placed in 100-110 DEG C of baking oven and dries to constant weight, and in 500 DEG C
Roasting 2 stands to room temperature, is pulverized with grinding；
(3) waste liquid is added in reaction kettle, is subsequently added into the plant amylum of waste liquid quality 20%, 50 DEG C of stirring 15min,
Then the Glycerin of cornstarch quality 15% and the di-cyclohexylperoxy di-carbonate of cornstarch quality 1% is added,
90 DEG C of insulated and stirred 2h, are filtered while hot, and decontamination is washed with deionized water in obtained solid, dry to constant weight.
The preparation of water-retaining agent: 4 parts of polyethylene glycol 400s are add to deionized water, then 30 DEG C of stirring 10min are added 6
Part polyglutamic acid and 0.05 part of tetraethyl titanate, flow back insulated and stirred 3h, is cooled to 70 DEG C and 1.5 parts of linseed oil stirrings are added
Decontamination is washed with deionized water in 20min, filtering, obtained solid, and 50 DEG C are dried under vacuum to constant weight.
Embodiment 2
The preparation of composite water conservation slow-release fertilizer:
(1) it mixes: by 50 parts of L-Ascorbic Acid L-O-Phosphate waste materials, 8 parts of urea, 8 parts of potassium sulfates, 4 parts of abscisic acids, 3 parts of water conservations
Agent is sent in high speed disperser, is dispersed after mixing evenly, in 30 DEG C of standing 20min；
(2) preparation of coating liquid: 25 parts of nitrocelluloses are added in 110 parts of dehydrated alcohols, 30 DEG C of stirring 15min,
Then san-mou oil and castor oil is added, flows back insulated and stirred 1h to get coating liquid is arrived；
(3) it prepares: coating liquid uniformly being smeared, is coated in the fertiliser granulates being uniformly mixed in step (1), decompression is steamed
Recycling design is evaporated to get composite slow-release fertilizer is arrived.
The processing of L-Ascorbic Acid L-O-Phosphate waste material:
(1) L-Ascorbic Acid L-O-Phosphate waste residue produced during the preparation process, waste liquid are collected；
(2) waste residue is placed into 1h in 3 DEG C of sealings, is subsequently placed in 100-110 DEG C of baking oven and dries to constant weight, and in 500 DEG C
Roasting 2 stands to room temperature, is pulverized with grinding；
(3) waste liquid is added in reaction kettle, is subsequently added into the plant amylum of waste liquid quality 20%, 50 DEG C of stirring 15min,
Then the Glycerin of cornstarch quality 15% and the di-cyclohexylperoxy di-carbonate of cornstarch quality 1% is added,
90 DEG C of insulated and stirred 2h, are filtered while hot, and decontamination is washed with deionized water in obtained solid, dry to constant weight.
The preparation of water-retaining agent: 4 parts of polyethylene glycol 400s are add to deionized water, then 30 DEG C of stirring 10min are added 6
Part polyglutamic acid and 0.05 part of tetraethyl titanate, flow back insulated and stirred 3h, is cooled to 70 DEG C and 1.5 parts of linseed oil stirrings are added
Decontamination is washed with deionized water in 20min, filtering, obtained solid, and 50 DEG C are dried under vacuum to constant weight.
Reference examples 1
The preparation of composite water conservation slow-release fertilizer:
(1) it mixes: by 45 parts of L-Ascorbic Acid L-O-Phosphate waste materials, 6 parts of urea, 6 parts of potassium chloride, 3 parts of abscisic acids, 3 parts of water conservations
Agent is sent in high speed disperser, is dispersed after mixing evenly, in 30 DEG C of standing 20min；
(2) preparation of coating liquid: 25 parts of nitrocelluloses are added in 110 parts of dehydrated alcohols, 30 DEG C of stirring 15min,
Then san-mou oil and castor oil is added, flows back insulated and stirred 1h to get coating liquid is arrived；
(3) it prepares: coating liquid uniformly being smeared, is coated in the fertiliser granulates being uniformly mixed in step (1), decompression is steamed
Recycling design is evaporated to get composite slow-release fertilizer is arrived.
The processing of L-Ascorbic Acid L-O-Phosphate waste material:
(1) L-Ascorbic Acid L-O-Phosphate waste residue produced during the preparation process, waste liquid are collected；
(2) waste residue is placed into 1h in 3 DEG C of sealings, is subsequently placed in 100-110 DEG C of baking oven and dries to constant weight, and in 500 DEG C
Roasting 2 stands to room temperature, is pulverized with grinding；
(3) waste liquid is added in reaction kettle, is subsequently added into the plant amylum of waste liquid quality 20%, 50 DEG C of stirring 15min,
90 DEG C of insulated and stirred 2h, are filtered while hot, and decontamination is washed with deionized water in obtained solid, dry to constant weight.
The preparation of water-retaining agent: 4 parts of polyethylene glycol 400s are add to deionized water, then 30 DEG C of stirring 10min are added 6
Part polyglutamic acid and 0.05 part of tetraethyl titanate, flow back insulated and stirred 3h, is cooled to 70 DEG C and 1.5 parts of linseed oil stirrings are added
Decontamination is washed with deionized water in 20min, filtering, obtained solid, and 50 DEG C are dried under vacuum to constant weight.
Reference examples 2
The preparation of composite water conservation slow-release fertilizer:
(1) it mixes: by 45 parts of L-Ascorbic Acid L-O-Phosphate waste materials, 6 parts of urea, 6 parts of potassium chloride, 3 parts of abscisic acids, 3 parts of water conservations
Agent is sent in high speed disperser, is dispersed after mixing evenly, in 30 DEG C of standing 20min；
(2) preparation of coating liquid: 25 parts of nitrocelluloses are added in 110 parts of dehydrated alcohols, 30 DEG C of stirring 15min,
Then san-mou oil and castor oil is added, flows back insulated and stirred 1h to get coating liquid is arrived；
(3) it prepares: coating liquid uniformly being smeared, is coated in the fertiliser granulates being uniformly mixed in step (1), decompression is steamed
Recycling design is evaporated to get composite slow-release fertilizer is arrived.
The processing of L-Ascorbic Acid L-O-Phosphate waste material:
(1) L-Ascorbic Acid L-O-Phosphate waste residue produced during the preparation process, waste liquid are collected；
(2) waste residue is placed into 1h in 3 DEG C of sealings, is subsequently placed in 100-110 DEG C of baking oven and dries to constant weight, and in 500 DEG C
Roasting 2 stands to room temperature, is pulverized with grinding；
(3) waste liquid is added in reaction kettle, is subsequently added into the plant amylum of waste liquid quality 20%, 50 DEG C of stirring 15min,
Then the Glycerin of cornstarch quality 15% and the di-cyclohexylperoxy di-carbonate of cornstarch quality 1% is added,
90 DEG C of insulated and stirred 2h, are filtered while hot, and decontamination is washed with deionized water in obtained solid, dry to constant weight.
Water-retaining agent: polyglutamic acid.
The preparation of the fertilizer of retaining water and releasing nutrients slowly is carried out using embodiment 1-2, reference examples 1-2, and its performance is measured, as a result such as
Shown in table 1.
The performance measurement of 1 composite water conservation slow-release fertilizer of table
| Test item | Preliminary solubility (%) | Differential solubility (%) | 28 days dissolution rates (%) |
| Embodiment 1 | 4.82 | 1.47 | 36 |
| Embodiment 2 | 4.74 | 1.45 | 35 |
| Reference examples 1 | 2.15 | 1.20 | 27 |
| Reference examples 2 | 5.38 | 1.69 | 38 |
The above sample is measured 25 according to " slow release fertilizer " national standard (GB/T23348-200) that China in 2009 formulates
Dissolution experiment at DEG C: 10g slow release fertilizer is weighed, is put into the double-deck pouch that 100 mesh nylon gauzes are made into, is sealed, by pouch
It is put into the plastic bottle containing 250ml distilled water, seals, 25 DEG C of constant temperature incubations, separated in time sampling, every sub-sampling
When water sample moved into another bottle, shake up rear test sample.250ml distilled water is added into the bottle equipped with nylon cloth again, is added
It is put into insulating box after lid sealing, continues to cultivate, every kind of fertilizer carries out 3 parallel tests.According to test result, measurement 24 is calculated
The preliminary solubility of the fertilizer dissolved out in fertilizer core in hour.The fertilizer nutrient of preliminary solubility (%)=24 hour dissolution
Gross mass × 100% of fertilizer nutrient in quality/fertilizer sample；Differential solubility (%)=(amount of nutrients being dissolved in water/
The nitrogen pool * 100- preliminary solubility of slow-release fertilizer)/(release number of days -1)；28 days accumulative dissolution rate (%)=28 day fertilizer nutrients
Cumulative release amount/fertilizer nutrient total content × 100%.
As can be seen from the table, when not being modified processing to plant amylum, the dissolution release performance of slow-release fertilizer
It is substantially reduced, to reduce the service efficiency of slow-release fertilizer.
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (7)
1. a kind of preparation method of L-Ascorbic Acid L-O-Phosphate composite water conservation slow-release fertilizer, which comprises the following steps:
(1) it mixes: L-Ascorbic Acid L-O-Phosphate waste material, urea, potassium chloride, abscisic acid, water-retaining agent is sent to high speed disperser
In, disperse after mixing evenly, in 30 DEG C of standing 20-30min；
(2) preparation of coating liquid: nitrocellulose is added in dehydrated alcohol, then san-mou oil is added in 30 DEG C of stirring 15min
And castor oil, insulated and stirred 0.5-2h is flowed back to get coating liquid is arrived；
(3) it prepares: coating liquid uniformly being smeared, is coated in the fertiliser granulates being uniformly mixed in step (1), is evaporated under reduced pressure back
Solvent is received to get composite slow-release fertilizer is arrived.
2. the preparation method of L-Ascorbic Acid L-O-Phosphate composite water conservation slow-release fertilizer according to claim 1, it is characterised in that:
The L-Ascorbic Acid L-O-Phosphate waste material, urea, potassium chloride, abscisic acid, water-retaining agent mass ratio be 40-50:5-10:6-8:1-
5:1-4.
3. the preparation method of L-Ascorbic Acid L-O-Phosphate composite water conservation slow-release fertilizer according to claim 1, it is characterised in that:
The nitrocellulose, san-mou oil, castor oil, dehydrated alcohol mass ratio be 20-30:4-6:2-3:100-120.
4. the preparation method of L-Ascorbic Acid L-O-Phosphate composite water conservation slow-release fertilizer according to claim 1, which is characterized in that
The processing method of the L-Ascorbic Acid L-O-Phosphate waste material are as follows:
(1) L-Ascorbic Acid L-O-Phosphate waste residue produced during the preparation process, waste liquid are collected；
(2) waste residue is placed into 1-2h in 3-5 DEG C of sealing, is subsequently placed in 100-110 DEG C of baking oven and dries to constant weight, and in 500-
550 DEG C of roasting 1-3h stand to room temperature, are pulverized with grinding；
(3) waste liquid is added in reaction kettle, is subsequently added into the plant amylum of waste liquid quality 20-30%, 50-60 DEG C of stirring 15-
Then 30min is added Glycerin and chain initiator, 90-95 DEG C of insulated and stirred 0.5-2h is filtered while hot, obtained solid is used
Deionized water washes away impurity, dry to constant weight.
5. the preparation method of L-Ascorbic Acid L-O-Phosphate composite water conservation slow-release fertilizer according to claim 4, it is characterised in that:
The Glycerin, chain initiator quality be respectively plant amylum quality 10-20%, 1-2%.
6. the preparation method of L-Ascorbic Acid L-O-Phosphate composite water conservation slow-release fertilizer according to claim 1, which is characterized in that
The water-retaining agent the preparation method comprises the following steps: polyethylene glycol is add to deionized water, then poly- paddy is added in 30 DEG C of stirring 10min
Propylhomoserin and tetraethyl titanate, flow back insulated and stirred 0.5-4h, is cooled to 70-75 DEG C of addition linseed oil stirring 20-40min, filters,
Decontamination is washed with deionized water in obtained solid, and 50 DEG C are dried under vacuum to constant weight.
7. the preparation method of L-Ascorbic Acid L-O-Phosphate composite water conservation slow-release fertilizer according to claim 6, it is characterised in that:
The polyethylene glycol, polyglutamic acid, tetraethyl titanate, linseed oil mass ratio be 4-6:5-8:0.05:0.5-2.
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