CN108249989A - The preparation method and siliceous fertilizer of siliceous fertilizer composition and siliceous fertilizer - Google Patents
The preparation method and siliceous fertilizer of siliceous fertilizer composition and siliceous fertilizer Download PDFInfo
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- CN108249989A CN108249989A CN201810098682.2A CN201810098682A CN108249989A CN 108249989 A CN108249989 A CN 108249989A CN 201810098682 A CN201810098682 A CN 201810098682A CN 108249989 A CN108249989 A CN 108249989A
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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
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05D—INORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C; FERTILISERS PRODUCING CARBON DIOXIDE
- C05D9/00—Other inorganic fertilisers
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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
- C05G5/10—Solid or semi-solid fertilisers, e.g. powders
- C05G5/12—Granules or flakes
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Abstract
This disclosure relates to the preparation method and siliceous fertilizer of a kind of siliceous fertilizer composition and siliceous fertilizer, the composition includes：Inactivate siliceous molecular sieve pretreating agent, Nano silica sol, flyash and optional additive, on the basis of the inactivation siliceous molecular sieve pretreating agent of 100 parts by weight, the content of the Nano silica sol is 10~80 parts by weight, the content of the flyash is 10~80 parts by weight, and the content of the additive is 0~30 parts by weight.The available silicon content of siliceous fertilizer being prepared using the composition of the disclosure is high, has the characteristics that dosage is few, fertilizer efficiency is excellent, storage and transportation is convenient, freight is low.
Description
Technical field
This disclosure relates to agriculture field, and in particular, to the preparation method and siliceous fertilizer of a kind of siliceous fertilizer composition and siliceous fertilizer.
Background technology
Siliceous fertilizer belongs to a kind of secondary nutrients, while is that a kind of good quality fertilizer, health care fertilizer and plant are adjusted
Property fertilizer, is a kind of incomparable novel and multifunctional fertilizer of other chemical fertilizer.Siliceous fertilizer can both make fertilizer, provide nutrient, again
It can be used as soil conditioner, improve soil.In addition, also have the effect of diseases prevention, insect prevention and attenuation concurrently.It is nontoxic, tasteless, constant with its
Matter, outstanding advantages of not being lost in, is nuisanceless, become the efficient and high-quality fertilizer of development green ecological agricultural.
At present, the kind of siliceous fertilizer mainly has solubility in citric acid siliceous fertilizer, two major class of Water-soluble silicon fertilizer, and solubility in citric acid siliceous fertilizer refers to not dissolve in
Water and be dissolved in the siliceous fertilizer that can be absorbed by plants after acid, common is mostly that steel slag, flyash, the ore of steel mill are forged through high temperature
Firing technique etc. is process, and general amount of application is larger, is suitble to do soil base and be applied, and market price is relatively low, but fertilizer efficiency effect is excessively slow
Slowly；Water-soluble silicon fertilizer refers to be dissolved in the siliceous fertilizer that water can directly be absorbed by plant, is that high temeperature chemistry synthesizes, crops absorb it
Utilization rate is higher, and amount of application is smaller, is generally commonly used for foliage-spray, punching is applied and trickle irrigation, but production technology is more complicated, cost compared with
It is high.
In petrochemical industry, the application of siliceous molecular sieve is very extensive, may generally serve as the carrier or activity of catalyst
Component.But irreversible inactivation easily occurs after participating in catalysis reaction in it, rich in SiO2Deactivator usually as solid waste quilt
Landfill, leads to larger waste.
Invention content
The purpose of the disclosure is to provide the preparation method and siliceous fertilizer of a kind of siliceous fertilizer composition and siliceous fertilizer, to solve existing contain
The available silicon content of silicon fertilizer is low and siliceous molecular sieve deactivator is difficult to recycle the problem of leading to the wasting of resources.
To achieve these goals, disclosure first aspect：A kind of siliceous fertilizer composition is provided, the composition includes：Inactivation
Siliceous molecular sieve pretreating agent, Nano silica sol, flyash and optional additive are contained with the inactivation of 100 parts by weight
On the basis of si molecular sieves pretreating agent, the content of the Nano silica sol is 10~80 parts by weight, and the content of the flyash is
10~80 parts by weight, the content of the additive is 0~30 parts by weight；
Wherein, the inactivation siliceous molecular sieve pretreating agent is obtains after the siliceous molecular sieve of inactivation is pre-processed
, the pretreatment includes：The siliceous molecular sieve of inactivation with acid, supplement silicon source and surfactant fluid is reacted, is received
Washing, drying after collection solid product.
Optionally, on the basis of the inactivation siliceous molecular sieve pretreating agent of 100 parts by weight, the Nano silica sol
Content is 50~70 parts by weight, and the content of the flyash is 20~50 parts by weight, and the content of the additive is 0~15 weight
Part.
Optionally, the siliceous molecular sieve of the inactivation and acid, supplement silicon source, the molar ratio of surfactant are 1：(0.1~
5)：(0.1~1.5)：(0.05~0.5), the siliceous molecular sieve of the inactivation is with SiO2Meter, the acid is with H+Meter, the supplement silicon
Source is with SiO2Meter；The condition of the reaction is：Temperature is 20~80 DEG C, the time for 0.1~for 24 hours.
Optionally, the acid is selected from least one of hydrochloric acid, sulfuric acid, nitric acid and phosphoric acid；
The supplement silicon source is for selected from least one of silica gel, Ludox and organosilicon acid esters selected from supplement silicon source；
The surfactant is selected from triethanolamine, cetyl trimethylammonium bromide, tetradecyltrimethylammonium bromination
At least one of ammonium, dodecyl alanine, methyl acrylate and alkyl dimethyl Hydroxypropyl phosphate fat glycine betaine.
Optionally, the siliceous molecular sieve of the inactivation is the mistake that caprolactam technology is prepared from cyclohexanone oxime vapour phase rearrangement
Type ZSM 5 molecular sieve living.
Optionally, the granularity of the inactivation siliceous molecular sieve pretreating agent is 100~500 mesh.
Optionally, the SiO of the Nano silica sol2Content is 10-25 weight %, and granularity is 5~100nm；
The granularity of the flyash is 100~200 mesh.
Optionally, the additive is selected from least one of dispersant, antifreezing agent and synergist；The dispersant is
Selected from calcium dodecyl benzene sulfonate, sodium lignin sulfonate, fatty alcohol polyoxyethylene ether, anhydrous sorbitol APEO, dibenzyl
Base phenol polyethenoxy ether, polyoxyethylene sorbitan ether monoleate, styryl phenol polyethenoxy ether, fatty amine polyoxy second
At least one of alkene ether and diisobutyl sodium naphthalene sulfonate, the antifreezing agent be selected from ethylene glycol, 1,2-PD, glycerine,
At least one of urea, polyethylene glycol and sorbierite, the synergist are selected from poly-aspartate, diethyl aminoethyl hexanoate and compound sodium nitrophenolate
At least one of.
Disclosure second aspect：The side that a kind of siliceous fertilizer composition using described in disclosure first aspect prepares siliceous fertilizer is provided
Method, this method include：By the inactivation siliceous molecular sieve pretreating agent, Nano silica sol, flyash and optional additive
It is granulated after mixing, obtains siliceous fertilizer.
The disclosure third aspect：The siliceous fertilizer that a kind of method as described in disclosure second aspect is prepared is provided.
Through the above technical solutions, siliceous molecular sieve of the disclosure to inactivate passes through the pre- place special to its as raw material
Reason method so that main source of the siliceous molecular sieve of inactivation as element silicon in siliceous fertilizer is turned waste into wealth.Using the group of the disclosure
The available silicon content for closing the siliceous fertilizer that object is prepared is high, has the spies such as dosage is few, fertilizer efficiency is excellent, storage and transportation is convenient, freight is low
Point.
Compared with existing siliceous fertilizer, the siliceous fertilizer applicable crops that the disclosure provides are extensive and have the advantage that：
1st, suitable for rice, sugarcane, wheat, corn, peanut, soybean, rape, cotton, sesame, millet, sweet potato, potato
Field crops are waited, photosynthesis can be promoted, plant epidermal cell siliceousization can be made, stalk is sturdy, blade is straight and upright, and enhancing is anti-fall
Volt ability, drought resisting cold-resistant, degeneration-resistant, reduction pest and disease damage, improves soil, and promotion organic fertilizer decomposes, inhibition soil germ, anti-continuous cropping,
Quality is improved, increases yield；
2nd, suitable for fruit trees such as apple, pears, peach, nectarine, Kiwi berry, jujube, grape, citrus, banana, lichee, longan, strawberries
Crop, can enhance photosynthesis, improve percentage of fertile fruit, reduce pest and disease damage, enable that fruit is big uniformly, colours, increases sugariness, carries
The high hardness of fruit, storage tolerance prolong storage period, improving quality, increase yield；
3rd, suitable for the melon work such as watermelon, muskmelon, cucumber, sponge gourd, wax gourd, pumpkin, pumpkin, cucurbita pepo, "Hami" melon, muskmelon
Object can enhance photosynthesis, improve percentage of fertile fruit, promote plant strain growth healthy and strong, reduce pest and disease damage, improve soil, inhibit soil
Germ, anti-continuous cropping, improving quality increase yield, promote precocious and listing；
4th, suitable for tomato, eggplant, capsicum, Chinese cabbage, onion, garlic, ginger, wild rice stem, lotus rhizome, radish, beet, wild cabbage etc.
Vegetable crop can enhance photosynthesis, improve percentage of fertile fruit, and enhancing development reduces pest and disease damage, inhibits soil germ, resists
Continuous cropping improves soil, improves quality, increases yield, promotes precocious and listing；
5th, other crops such as tobacco, tealeaves, Chinese medicine, reed, fiber crops, bamboo, lawn are applied also for, photosynthetic work can be enhanced
With improving lodging tolerance, reduce pest and disease damage, drought resisting, degeneration-resistant, anti-continuous cropping, improving quality increases yield, promotes the life of root system
It is long, increase the mechanical strength of grass blade bar, improve greens ball speed and the anti-trample ability in lawn, effectively inhibit the moisture transpiration of turfgrass
Effect improves the ability of drought resisting, hot-dry wind tolerance, cold-resistant and low-temperature resistance；Cuticula increases, and improves resistance energy of the lawn to pest and disease damage
Power has the leaf spot on lawn, brown spot, powdery mildew, droop and aphid, mythimna separata, black cutworm etc. very strong resistance.
Other feature and advantage of the disclosure will be described in detail in subsequent specific embodiment part.
Specific embodiment
The specific embodiment of the disclosure is described in detail below.It is it should be understood that described herein specific
Embodiment is only used for describing and explaining the disclosure, is not limited to the disclosure.
Disclosure first aspect：A kind of siliceous fertilizer composition is provided, the composition includes：Inactivate siliceous molecular sieve pretreatment
Agent, Nano silica sol, flyash and optional additive, with the inactivation siliceous molecular sieve pretreating agent of 100 parts by weight
On the basis of, the content of the Nano silica sol is 10~80 parts by weight, and the content of the flyash is 10~80 parts by weight, described
The content of additive is 0~30 parts by weight.
According to the disclosure, the inactivation siliceous molecular sieve pretreating agent is after the siliceous molecular sieve of inactivation is pre-processed
It obtains, the pretreatment includes：The siliceous molecular sieve of inactivation and acid, supplement silicon source and surfactant fluid are carried out instead
Should, collect washing, drying after solid product.
The disclosure is using the siliceous molecular sieve that inactivates as raw material, by by the siliceous molecular sieve inactivated and acid, supplement silicon source
The preprocess method reacted with surfactant fluid so that pretreated inactivation siliceous molecular sieve pretreating agent conduct
The main source of element silicon, turns waste into wealth in siliceous fertilizer.Using the available silicon content for the siliceous fertilizer that the composition of the disclosure is prepared
Height has the characteristics that dosage is few, fertilizer efficiency is excellent, storage and transportation is convenient, freight is low.
According to the disclosure, the siliceous molecular sieve of the inactivation.The siliceous molecular sieve can be common various types,
Structure can be in FAU types molecular sieve, MFI-type molecular sieve, MEL types molecular sieve, BEA types molecular sieve and MWW type molecular sieves
At least one, preferably MFI-type molecular sieve.
According to the disclosure, the siliceous molecular sieve of the inactivation can be to come from siliceous point obtained under basic reaction conditions
Son sieve, such as ketone oxamidinating deactivated molecular sieve or the siliceous molecular sieve obtained under weakly acidic pH reaction condition, such as alkene
Epoxidation deactivated molecular sieve, arene hydroxylation deactivated molecular sieve, oxidation of alkanes deactivated molecular sieve, can also be from acid reaction
Under the conditions of obtained siliceous molecular sieve, such as olefin chlorine alcoholization deactivated molecular sieve, unsaturated hydrocarbons halogenating reaction deactivated molecular sieve.
In the disclosure, alkalinity is come from instead especially suitable for processing to the method that the siliceous molecular sieve of inactivation is pre-processed
The siliceous molecular sieve obtained under the conditions of answering.Further, in a kind of preferred embodiment of the disclosure, the inactivation it is siliceous
Molecular sieve is the inactivation type ZSM 5 molecular sieve that caprolactam technology is prepared from cyclohexanone oxime vapour phase rearrangement, such as Silicate-1
Molecular sieve.The inactivation type ZSM 5 molecular sieve that caprolactam technology is prepared from cyclohexanone oxime vapour phase rearrangement is particularly suitable in acid, benefit
One of component after silicon source and surfactant pretreatment as siliceous fertilizer is filled, the fertilizer efficiency of siliceous fertilizer can be significantly increased.
According to the disclosure, in order to improve the absorbability of siliceous fertilizer, the granularity of the inactivation siliceous molecular sieve pretreating agent can
Think 100~500 mesh.In order to which the granularity for making the inactivation siliceous molecular sieve pretreating agent reaches above range, the pretreatment
It can also include：Collect the step of solid product is washed, is ground after drying.The method of grinding can be people in the art
Known to member, the disclosure does not have special limitation.
According to the disclosure, in order to further improve the available silicon content of siliceous fertilizer, with siliceous point of the inactivation of 100 parts by weight
On the basis of son sieve pretreating agent, the content of the Nano silica sol can be 50~70 parts by weight, and the content of the flyash can
Think 20~50 parts by weight, the content of the additive can be 0~15 parts by weight.
According to the disclosure, in order to reach ideal pretreating effect, siliceous molecular sieve and acid, the supplement silicon of the inactivation
Source, surfactant molar ratio can be 1：(0.1~5)：(0.1~1.5)：(0.05~0.5), siliceous point of the inactivation
Son sieve is with SiO2Meter, the acid is with H+Meter, the supplement silicon source is with SiO2Meter；The condition of the reaction can be：Temperature for 20~
80 DEG C, the time for 0.1~for 24 hours.
According to the disclosure, the acid can be common inorganic acid, such as can be selected from hydrochloric acid, sulfuric acid, nitric acid and phosphorus
At least one of acid.The acid generally exists in form of an aqueous solutions, and the concentration of aqueous solution is not particularly limited, such as can
Think 1-60 weight %, preferably 5-30 weight %.
According to the disclosure, the supplement silicon source can be common various silicon sources when preparing siliceous molecular sieve, for example, described
It can be selected from least one of silica gel, Ludox and organosilicon acid esters to supplement silicon source；Preferably general formula is (OR)4Si's has
Machine esters of silicon acis, wherein, R is the alkyl of 1-4 carbon atom；Further preferably methyl orthosilicate and/or ethyl orthosilicate.
According to the disclosure, the surfactant can be cationic surfactant and/or amphoteric ion surface-active
Agent is preferably selected from triethanolamine, cetyl trimethylammonium bromide, tetradecyltrimethylammonium bromide, dodecylamino
At least one of propionic acid, methyl acrylate and alkyl dimethyl Hydroxypropyl phosphate fat glycine betaine, most preferably cetyl three
Methyl bromide ammonium.
According to the disclosure, after the completion of the reaction, appropriate amount of deionized water may be used, product is washed, Ran Hougan
It is dry, you can to obtain inactivation siliceous molecular sieve pretreating agent.The temperature of the drying can be for example 80~150 DEG C, and the time can be with
For 2~for 24 hours.
According to the disclosure, in order to improve the application effect of siliceous fertilizer, the SiO of the Nano silica sol2Content can be 10-25
Weight %；Granularity can be 5~100nm, preferably 10~40nm, and the granularity refers to SiO in Nano silica sol2Particle it is big
It is small.
According to the disclosure, in order to improve the application effect of siliceous fertilizer, the granularity of the flyash can be 100~200 mesh.
According to the disclosure, the additive can be selected from least one of dispersant, antifreezing agent and synergist.It is described
Dispersant can be selected from calcium dodecyl benzene sulfonate, sodium lignin sulfonate, fatty alcohol polyoxyethylene ether, anhydrous sorbitol polyoxy
Vinethene, dibenzyl phenol polyethenoxy ether, polyoxyethylene sorbitan ether monoleate, styryl phenol polyethenoxy ether,
At least one of aliphatic amine polyoxyethylene ether and diisobutyl sodium naphthalene sulfonate.The antifreezing agent can be selected from ethylene glycol, 1,
At least one of 2- propylene glycol, glycerine, urea, polyethylene glycol and sorbierite.The synergist can be selected from poly- asparagus fern
At least one of propylhomoserin, diethyl aminoethyl hexanoate and compound sodium nitrophenolate.
Disclosure second aspect：Improve the side that a kind of siliceous fertilizer composition using described in disclosure first aspect prepares siliceous fertilizer
Method, this method include：By the inactivation siliceous molecular sieve pretreating agent, Nano silica sol, flyash and optional additive
It is granulated after mixing, obtains siliceous fertilizer.The process of the granulation is well known to those skilled in the art, and the disclosure is without spy
Different limitation.
The disclosure third aspect：The siliceous fertilizer that a kind of method as described in disclosure second aspect is prepared is provided.
Further the disclosure is illustrated by the following examples, but and is not so limited the disclosure.
Embodiment 1
The siliceous molecular sieve of inactivation in the present embodiment is to prepare caprolactam technology from cyclohexanone oxime vapour phase rearrangement
Inactivate Silicate-1 molecular sieves.
By the siliceous molecular sieve of inactivation, the aqueous solution of nitric acid of 15 weight %, methyl orthosilicate and cetyl trimethyl bromine
It is 1 to change ammonium according to molar ratio：2：0.6：0.2 mixing, is stirred to react 2h at 40 DEG C, collects washing, drying after solid product, and
200 mesh are ground to, obtain inactivation siliceous molecular sieve pretreating agent.
By the above-mentioned inactivation siliceous molecular sieve pretreating agent of 100 parts by weight, the Nano silica sol (SiO of 60 parts by weight2Content
For 25 weight %, granularity 40nm), the flyash (granularity is 150 mesh) of 40 parts by weight, 3 parts by weight dodecyl benzene sulfonic acid
The poly-aspartate of calcium, the ethylene glycol of 2 parts by weight and 2 parts by weight is granulated after mixing, obtains the present embodiment preparation
Siliceous fertilizer.
Embodiment 2
The siliceous molecular sieve of inactivation in the present embodiment is to prepare caprolactam technology from cyclohexanone oxime vapour phase rearrangement
Inactivate Silicate-1 molecular sieves.
By the siliceous molecular sieve of inactivation, 30 weight % aqueous hydrochloric acid solution, silica gel and triethanolamine according to molar ratio be 1：
0.2：1.2：0.08 mixing, is stirred to react 4h at 50 DEG C, collects washing, drying after solid product, and be ground to 400 mesh, obtains
To inactivation siliceous molecular sieve pretreating agent.
By the above-mentioned inactivation siliceous molecular sieve pretreating agent of 100 parts by weight, the Nano silica sol (SiO of 50 parts by weight2Content
For 25 weight %, granularity 40nm), the flyash (granularity is 150 mesh) of 65 parts by weight, 3 parts by weight dodecyl benzene sulfonic acid
The poly-aspartate of calcium, the ethylene glycol of 2 parts by weight and 2 parts by weight is granulated after mixing, obtains the present embodiment preparation
Siliceous fertilizer.
Embodiment 3
The siliceous molecular sieve of inactivation in the present embodiment is to prepare caprolactam technology from cyclohexanone oxime vapour phase rearrangement
Inactivate Silicate-1 molecular sieves.
By the siliceous molecular sieve of inactivation, phosphate aqueous solution, ethyl orthosilicate and the dodecyl alanine of 10 weight %
It is 1 according to molar ratio：4：0.2：0.5 mixing, is stirred to react 4h at 50 DEG C, collects washing, drying after solid product, and grind
To 300 mesh, inactivation siliceous molecular sieve pretreating agent is obtained.
By the above-mentioned inactivation siliceous molecular sieve pretreating agent of 100 parts by weight, the Nano silica sol (SiO of 70 parts by weight2Content
For 25 weight %, granularity 40nm), the flyash (granularity is 150 mesh) of 25 parts by weight, 3 parts by weight dodecyl benzene sulfonic acid
The poly-aspartate of calcium, the ethylene glycol of 2 parts by weight and 2 parts by weight is granulated after mixing, obtains the present embodiment preparation
Siliceous fertilizer.
Embodiment 4
The inactivation siliceous molecular sieve pretreating agent of the present embodiment is same as Example 1.
By the inactivation siliceous molecular sieve pretreating agent of 100 parts by weight, the Nano silica sol (SiO of 80 parts by weight2Content is 25
Weight %, granularity 40nm), the flyash of 10 parts by weight (granularity is 150 mesh), the calcium dodecyl benzene sulfonate of 3 parts by weight, 2
The ethylene glycol of parts by weight and the poly-aspartate of 2 parts by weight are granulated after mixing, obtain silicon manufactured in the present embodiment
Fertilizer.
Embodiment 5
The inactivation siliceous molecular sieve pretreating agent of the present embodiment is same as Example 1.
By the inactivation siliceous molecular sieve pretreating agent of 100 parts by weight, the Nano silica sol (SiO of 10 parts by weight2Content is 25
Weight %, granularity 40nm), the flyash of 80 parts by weight (granularity is 150 mesh), the calcium dodecyl benzene sulfonate of 3 parts by weight, 2
The ethylene glycol of parts by weight and the poly-aspartate of 2 parts by weight are granulated after mixing, obtain silicon manufactured in the present embodiment
Fertilizer.
Embodiment 6
Method according to embodiment 1 prepares siliceous fertilizer, the siliceous molecular sieve difference lies in, the inactivation in the present embodiment be from
The inactivation Y type molecular sieve of hydrocarbon raw material hydrocracking process.
Embodiment 7
Method according to embodiment 1 prepares siliceous fertilizer, and difference lies in the granularity of Nano silica sol is 100nm.
Embodiment 8
Method according to embodiment 1 prepares siliceous fertilizer, and difference lies in the SiO of Nano silica sol2Content be 30 weight %, grain
It spends for 200nm.
Embodiment 9
Method according to embodiment 1 prepares siliceous fertilizer, and difference lies in the granularity of flyash is 50 mesh.
Comparative example 1
The siliceous molecular sieve of inactivation in this comparative example is same as Example 1.
By the siliceous molecular sieve of the inactivation of 100 parts by weight, the Nano silica sol (SiO of 60 parts by weight2Content is 25 weights
Measure %, granularity 40nm), the flyash of 40 parts by weight (granularity is 150 mesh), the calcium dodecyl benzene sulfonate of 3 parts by weight, 2 weights
It measures the ethylene glycol of part and the poly-aspartate of 2 parts by weight is granulated after mixing, obtain the siliceous fertilizer of this comparative example preparation.
Comparative example 2
The siliceous molecular sieve of inactivation in this comparative example is same as Example 1.
By the siliceous molecular sieve of inactivation, water, methyl orthosilicate and cetyl trimethylammonium bromide according to molar ratio be 1：
2：0.6：0.2 mixing, is stirred to react 2h at 40 DEG C, collects washing, drying after solid product, it is pre- to obtain inactivation siliceous molecular sieve
Inorganic agent.
By the above-mentioned inactivation siliceous molecular sieve pretreating agent of 100 parts by weight, the Nano silica sol (SiO of 60 parts by weight2Content
For 25 weight %, granularity 40nm), the flyash (granularity is 150 mesh) of 40 parts by weight, 3 parts by weight dodecyl benzene sulfonic acid
The poly-aspartate of calcium, the ethylene glycol of 2 parts by weight and 2 parts by weight is granulated after mixing, obtains the present embodiment preparation
Siliceous fertilizer.
Comparative example 3
The siliceous molecular sieve of inactivation in this comparative example is same as Example 1.
By the siliceous molecular sieve of inactivation, 15 weight % aqueous solution of nitric acid, methyl orthosilicate and water according to molar ratio be 1：
2：0.6：0.2 mixing, is stirred to react 2h at 40 DEG C, collects washing, drying after solid product, it is pre- to obtain inactivation siliceous molecular sieve
Inorganic agent.
By the above-mentioned inactivation siliceous molecular sieve pretreating agent of 100 parts by weight, the Nano silica sol (SiO of 60 parts by weight2Content
For 25 weight %, granularity 40nm), the flyash (granularity is 150 mesh) of 40 parts by weight, 3 parts by weight dodecyl benzene sulfonic acid
The poly-aspartate of calcium, the ethylene glycol of 2 parts by weight and 2 parts by weight is granulated after mixing, obtains the present embodiment preparation
Siliceous fertilizer.
Testing example 1
The available silicon content in the siliceous fertilizer of embodiment 1-9 and comparative example 1-3 is measured, test method is：NY/T797-2004,
Test result is listed in table 1.
Table 1
| Embodiment | SiO2, w% |
| Embodiment 1 | 55.1 |
| Embodiment 2 | 52.8 |
| Embodiment 3 | 54.2 |
| Embodiment 4 | 50.5 |
| Embodiment 5 | 49.7 |
| Embodiment 6 | 44.3 |
| Embodiment 7 | 46.3 |
| Embodiment 8 | 42.2 |
| Embodiment 9 | 41.5 |
| Comparative example 1 | 15.5 |
| Comparative example 2 | 4.3 |
| Comparative example 3 | 6.8 |
Testing example 2
Manure trial is carried out to the siliceous fertilizer of embodiment 1-9 and comparative example 1-3.
Test material：Zhejiang somewhere, soil types be 25.3g/kg containing organic matter, full nitrogen 186.9mg/kg, available phosphorus
10.6mg/kg, available potassium 112.5mg/kg, pH value 7.55.Topography is flat, and the row of filling is convenient.It is two excellent 6326 for examination rice varieties.
Using simplified greenhouse Nutrition Soil separation layer dry rice seedling method.Leaf age starts to transplant up to 3.8-4.1 leaves or so, planting density 15349
Plant/acre.Using great Qu methods of comparison, repetition is not set, each processing area is 1 mu.
Test process：Experiment sets 13 processing, and processing 1-12 is test group：Use embodiment of the present disclosure 1-9 and comparative example
The siliceous fertilizer of 1-3,10kg/ mus of amount of application, pesticide application amount are conventional 50%；Processing 13 is control group：Not Applying silicon fertilizer, and often
Advise spraying pesticide.
Result of the test：By experimental observation, the rice growing way of test group 10-12 and control group is poor, and stalk is tiny, blade
Yellowing, small holes caused by worms are more, have slight early ageing phenomenon, spike of rice is shorter when ripe；The rice application of test group 1-9 embodiment 1-9's
Siliceous fertilizer, growing way is preferable, and stalk is sturdy, and blade is thick, matter is hard, and small holes caused by worms are few, and spike of rice is longer.Specific data are listed in table 2.
Table 2
As can be seen from Table 2, the rice of control group does not apply the siliceous fertilizer of the disclosure, plant height, spike length, number of productive ear, bear fruit grains and
Yield has apparent gap than test group 1-9, and the rice growing way of test group 1-9 is good, and yield is high, and the fertilizer and pesticide applied
Amount less than control group, not only saves planting cost, but also protect agricultural environment, has good planting benefit.By test group
The comparison of 1-9 and test group 10-12 using the inactivation that acid, supplement silicon source and surfactant are pre-processed as it can be seen that contained
Siliceous fertilizer prepared by si molecular sieves pretreating agent, plant height, spike length, number of productive ear, bear fruit grains, mass of 1000 kernel and yield have significant increasing
It is long.
The preferred embodiment of the disclosure described in detail above, still, the disclosure is not limited in the above embodiment
Detail, in the range of the technology design of the disclosure, a variety of simple variants can be carried out to the technical solution of the disclosure, this
A little simple variants belong to the protection domain of the disclosure.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the disclosure to it is various can
The combination of energy no longer separately illustrates.
In addition, arbitrary combination can also be carried out between a variety of different embodiments of the disclosure, as long as it is without prejudice to originally
Disclosed thought should equally be considered as disclosure disclosure of that.
Claims (10)
1. a kind of siliceous fertilizer composition, which is characterized in that the composition includes：Inactivate siliceous molecular sieve pretreating agent, nano silicasol
Glue, flyash and optional additive, it is described on the basis of the inactivation siliceous molecular sieve pretreating agent of 100 parts by weight
The content of Nano silica sol is 10~80 parts by weight, and the content of the flyash is 10~80 parts by weight, and the additive contains
It measures as 0~30 parts by weight；
Wherein, the inactivation siliceous molecular sieve pretreating agent is to be obtained after the siliceous molecular sieve of inactivation is pre-processed, institute
Pretreatment is stated to include：The siliceous molecular sieve of inactivation with acid, supplement silicon source and surfactant fluid is reacted, collects solid
It is washed after product, is dry.
2. composition according to claim 1, wherein, with the inactivation siliceous molecular sieve pretreating agent of 100 parts by weight
On the basis of, the content of the Nano silica sol is 50~70 parts by weight, and the content of the flyash is 20~50 parts by weight, described
The content of additive is 0~15 parts by weight.
3. composition according to claim 1 or 2, wherein, siliceous molecular sieve and acid, supplement silicon source, the table of the inactivation
The molar ratio of face activating agent is 1：(0.1~5)：(0.1~1.5)：(0.05~0.5), the siliceous molecular sieve of the inactivation with
SiO2Meter, the acid is with H+Meter, the supplement silicon source is with SiO2Meter；The condition of the reaction is：Temperature is 20~80 DEG C, the time
For 0.1~for 24 hours.
4. composition according to claim 1 or 2, wherein, the acid is in hydrochloric acid, sulfuric acid, nitric acid and phosphoric acid
It is at least one；
The supplement silicon source is for selected from least one of silica gel, Ludox and organosilicon acid esters selected from supplement silicon source；
The surfactant is selected from triethanolamine, cetyl trimethylammonium bromide, tetradecyltrimethylammonium bromide, ten
At least one of dialkyl amido propionic acid, methyl acrylate and alkyl dimethyl Hydroxypropyl phosphate fat glycine betaine.
5. composition according to claim 1 or 2, wherein, the siliceous molecular sieve of the inactivation is from cyclohexanone oxime gas
Phase rearrangement prepares the inactivation type ZSM 5 molecular sieve of caprolactam technology.
6. composition according to claim 1 or 2, wherein, the granularity of the inactivation siliceous molecular sieve pretreating agent is 100
~500 mesh.
7. composition according to claim 1 or 2, wherein, the SiO of the Nano silica sol2Content is 10-25 weight %,
Granularity is 5~100nm；
The granularity of the flyash is 100~200 mesh.
8. composition according to claim 1 or 2, wherein, the additive is selected from dispersant, antifreezing agent and synergist
At least one of；The dispersant be selected from calcium dodecyl benzene sulfonate, sodium lignin sulfonate, fatty alcohol polyoxyethylene ether,
Anhydrous sorbitol APEO, dibenzyl phenol polyethenoxy ether, polyoxyethylene sorbitan ether monoleate, styryl
At least one of phenol polyethenoxy ether, aliphatic amine polyoxyethylene ether and diisobutyl sodium naphthalene sulfonate, the antifreezing agent be selected from
At least one of ethylene glycol, 1,2-PD, glycerine, urea, polyethylene glycol and sorbierite, the synergist are selected from poly-
At least one of aspartic acid, diethyl aminoethyl hexanoate and compound sodium nitrophenolate.
9. the method that the siliceous fertilizer composition in a kind of 1-8 using claim described in any one prepares siliceous fertilizer, which is characterized in that
This method includes：The inactivation siliceous molecular sieve pretreating agent, Nano silica sol, flyash and optional additive are mixed
It is granulated after uniformly, obtains siliceous fertilizer.
10. a kind of siliceous fertilizer that method as described in claim 9 is prepared.
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| CN109666484A (en) * | 2019-02-19 | 2019-04-23 | 张云伟 | A kind of preparation method of soil remediation medicament that repairing organophosphorus pesticide pollution |
| CN110283010A (en) * | 2019-05-21 | 2019-09-27 | 滁州市给力肥料科技有限公司 | A kind of novel nano siliceous fertilizer and preparation method and its application method |
| CN113020250A (en) * | 2021-04-07 | 2021-06-25 | 淮南师范学院 | Method for producing low-cadmium rice and simultaneously repairing cadmium pollution of rice field soil |
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