CN107253873A - A kind of preparation method of Thermo-sensitive graphite fiber alkene composite water conservation coated fertilizer - Google Patents
A kind of preparation method of Thermo-sensitive graphite fiber alkene composite water conservation coated fertilizer Download PDFInfo
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- CN107253873A CN107253873A CN201710438077.0A CN201710438077A CN107253873A CN 107253873 A CN107253873 A CN 107253873A CN 201710438077 A CN201710438077 A CN 201710438077A CN 107253873 A CN107253873 A CN 107253873A
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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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Abstract
The invention discloses a kind of preparation method of Thermo-sensitive graphite fiber alkene composite water conservation coated fertilizer, graphene is first subjected to processing modification using ammoniacal liquor with cetyl trimethylammonium bromide, hybrid reaction ultrasonic disperse is carried out with modified graphene solution solution is made after cellulose addition ammoniacal liquor is soaked afterwards, add nano silicon, cellulose silicon dioxide hybrid materials are prepared using Electrostatic Absorption method, after addition crosslinking agent is crosslinked afterwards, remove to freeze after cetyl trimethylammonium bromide and be made, preparation technology of the present invention is simple, it is with low cost, and raw graphite alkene can be avoided to be reunited, product good mechanical performance, coated fertilizer has protective separation effect, reduce or prevent the release of internal fertilizer.
Description
Technical field
The present invention relates to temperature sensing material technical field, and in particular to a kind of Thermo-sensitive graphite fiber alkene composite water conservation coating material
The preparation method of material.
Background technology
In past more than ten years, development of the porous nanometer material in terms of pharmaceutical preparation causes the emerging of many scientific research personnel
Interest.Due to the biocompatibility of cellulose and degradable, cellulose is applied to pharmacy, Nano medication, biotechnology etc.
Aspect is increasingly becoming focus.Mesoporous material is combined to obtained composite with cellulose also turns into the heat of many researchers
Point, first, cellulose is nontoxic, and silica has the special nature such as high-melting-point, nontoxic, high stability, and both are combined
It is with certain feasibility as auxiliary material.
Now, chemical fertilizer is quite popularized in global agricultural planting, but chemical fertilizer is easily lost in soil
With volatilization, cause plant to fully absorb and utilize and cause the waste of the energy and the pollution of environment.Therefore, chemical fertilizer is improved
Utilization rate, and the cost of labor repeatedly applied fertilizer and the environmental pollution brought are reduced, become the research direction of researchers.
Zhang Jing《The preparation of cellulose base hybrid material and its temperature sensitive performance study》Pass through concentrated sulfuric acid method for pretreating in one text
Nano-cellulose suspension is obtained, nano-cellulose-titanium dioxide sila of high-specific surface area has been prepared using Electrostatic Absorption method
Change material, and the nano-cellulose temperature sensing material prepared and there is temperature sensitive effect is reacted using atom transferred free radical, to sample
The sustained release performance of product is probed into, it was confirmed that nano-cellulose temperature sensing material has good sustained release performance, but in some machines
Tool performance such as toughness is poor, and this makes the application of these temperature sensing materials be very limited.
The content of the invention
The object of the invention is exactly that there is provided a kind of Thermo-sensitive graphite fiber alkene composite water conservation in order to make up the defect of prior art
The preparation method of coated fertilizer, preparation technology is simple, and raw graphite alkene can be avoided to be reunited, and coated fertilizer has protection
Buffer action, reduces or prevents the release of internal fertilizer.
The present invention is achieved by the following technical solutions：
A kind of preparation method of Thermo-sensitive graphite fiber alkene composite water conservation coated fertilizer, comprises the following steps：
（1）The graphene of 20-30 parts by weight is dissolved in 100-200 parts by weight absolute ethyl alcohols, 2-5 is added dropwise under quick magnetic agitation
Parts by weight ammoniacal liquor, is persistently stirred after adding, and 1-2 parts by weight cetyl trimethylammonium bromides are first dissolved in after absolute ethyl alcohol,
Solution is added dropwise under fast stirring, is kept for 60-80 DEG C, magnetic agitation 2-5 hours is stand-by；
（2）After 10-15 percent by weight fiber is immersed in into 20-30 parts by weight ammoniacal liquor 40-60 minutes, takes out fiber and add step（1）
In gains, after low temperature ultrasonic is scattered, magnetic agitation is after 1-12 hours, 20-30 DEG C, places 2-3 days, stand-by；
（3）By step（2）35-55 DEG C of resulting solution heating water bath, adds 3-6 parts by weight nano silicons while stirring, protects
After holding temperature heating 40-60 minutes, addition 2-4 parts by weight glutaraldehydes, keeping temperature, continue stirring reaction 10-12 hours, with
The ethanol solution of sodium acetate is extractant, and extraction removes cetyl trimethylammonium bromide, successively with steaming after being centrifuged
Distilled water, ethanol wash 3-4 time afterwards freezed, both the Thermo-sensitive graphite fiber alkene composite water conservation coated fertilizer.
Step（2）Described low temperature ultrasonic be separated into ice-water bath handle 5-10 minutes after, ultrasonic disperse, supersonic frequency
For 40-80KHz, kept for 5 minutes, be spaced 1 minute every time, repeated 5-6 times.
Described fiber is that source is wheat stalk, maize straw, soybean stalk, the one or more in bagasse.
Described freezes to put in freeze dryer, is refrigerated to -10--20 DEG C, is evacuated to drying chamber pressure 30-40Pa, heating
40-50 DEG C, until the ice in material all distils.
A kind of application method of Thermo-sensitive graphite fiber alkene composite water conservation coated fertilizer, it is characterised in that by the coating
It is added to after material disintegrating in the rotating disk of granulated fertilizer, parcel arrives fertilizer surface in the presence of atomized water, forms uniform
Clad, be heating and curing, cool down.
It is an advantage of the invention that：
Graphene is first carried out processing modification by the present invention using ammoniacal liquor with cetyl trimethylammonium bromide, afterwards adds cellulose
Enter to carry out hybrid reaction ultrasonic disperse with modified graphene solution after ammoniacal liquor is soaked and be made solution, add nano-silica
SiClx, cellulose-silicon dioxide hybrid materials are prepared using Electrostatic Absorption method, after addition crosslinking agent is crosslinked afterwards, are removed
Freeze and be made after cetyl trimethylammonium bromide, graphene surface-active after modification is improved, and is also greatly reduced
The effect of the reunion of graphene, cellulose after AMMONIA TREATMENT can surface grafting amido, improve cellulose thermo-response, it
Graphene adsorbable amido during hybrid reaction afterwards so that graphene can grafted cellulose, carried out afterwards with silica miscellaneous
Change crosslinking so that graphene and nano silicon, cellulose three forms rock-steady structure, using the method system for removing template agent removing
Into mesoporous graphene, preparation technology of the present invention is simple, with low cost and raw graphite alkene can be avoided to be reunited, product machine
Tool function admirable, coated fertilizer has protective separation effect, reduces or prevent the release of internal fertilizer.
Embodiment
A kind of preparation method of Thermo-sensitive graphite fiber alkene composite water conservation coated fertilizer, comprises the following steps：
（1）The graphene of 25 parts by weight is dissolved in 150 parts by weight absolute ethyl alcohols, 4 parts by weight ammonia are added dropwise under quick magnetic agitation
Water, is persistently stirred after adding, and 1.5 parts by weight cetyl trimethylammonium bromides are first dissolved in after absolute ethyl alcohol, is quickly being stirred
Lower dropwise addition solution is mixed, is kept for 70 DEG C, magnetic agitation 3 hours is stand-by；
（2）After 12 percent by weight fiber are immersed in into 25 parts by weight ammoniacal liquor 50 minutes, take out fiber and add step（1）In gains,
After low temperature ultrasonic is scattered, magnetic agitation is after 8 hours, 25 DEG C, places 2 days, stand-by；
（3）By step（2）45 DEG C of resulting solution heating water bath, adds 4 parts by weight nano silicons, keeping temperature while stirring
After heating 50 minutes, 3 parts by weight glutaraldehydes of addition, keeping temperature, continue stirring reaction 10 hours, with the anhydrous second of sodium acetate
Alcoholic solution is extractant, and extraction removes cetyl trimethylammonium bromide, uses distilled water, ethanol washing 3 after being centrifuged successively
It is secondary after freezed, both the Thermo-sensitive graphite fiber alkene composite water conservation coated fertilizer.
Step（2）Described low temperature ultrasonic is separated into handled 8 minutes in ice-water bath after, ultrasonic disperse, supersonic frequency is
50KHz, is kept for 5 minutes every time, is spaced 1 minute, is repeated 5 times.
Described fiber is that source is wheat stalk, maize straw, soybean stalk, the one or more in bagasse.
Described freezes to put in freeze dryer, is refrigerated to -15 DEG C, is evacuated to drying chamber pressure 35Pa, heats 45 DEG C, directly
Ice into material all distils.
A kind of application method of Thermo-sensitive graphite fiber alkene composite water conservation coated fertilizer, it is characterised in that by the coating
It is added to after material disintegrating in the rotating disk of granulated fertilizer, parcel arrives fertilizer surface in the presence of atomized water, forms uniform
Clad, be heating and curing, cool down.
Claims (5)
1. a kind of preparation method of Thermo-sensitive graphite fiber alkene composite water conservation coated fertilizer, it is characterised in that comprise the following steps：
（1）The graphene of 20-30 parts by weight is dissolved in 100-200 parts by weight absolute ethyl alcohols, 2-5 is added dropwise under quick magnetic agitation
Parts by weight ammoniacal liquor, is persistently stirred after adding, and 1-2 parts by weight cetyl trimethylammonium bromides are first dissolved in after absolute ethyl alcohol,
Solution is added dropwise under fast stirring, is kept for 60-80 DEG C, magnetic agitation 2-5 hours is stand-by；
（2）After 10-15 percent by weight fiber is immersed in into 20-30 parts by weight ammoniacal liquor 40-60 minutes, takes out fiber and add step（1）
In gains, after low temperature ultrasonic is scattered, magnetic agitation is after 1-12 hours, 20-30 DEG C, places 2-3 days, stand-by；
（3）By step（2）35-55 DEG C of resulting solution heating water bath, adds 3-6 parts by weight nano silicons while stirring, protects
After holding temperature heating 40-60 minutes, addition 2-4 parts by weight glutaraldehydes, keeping temperature, continue stirring reaction 10-12 hours, with
The ethanol solution of sodium acetate is extractant, and extraction removes cetyl trimethylammonium bromide, successively with steaming after being centrifuged
Distilled water, ethanol wash 3-4 time afterwards freezed, both the Thermo-sensitive graphite fiber alkene composite water conservation coated fertilizer.
2. according to a kind of preparation method of Thermo-sensitive graphite fiber alkene composite water conservation coated fertilizer of claim 1, it is characterised in that
Step（2）Described low temperature ultrasonic be separated into ice-water bath handle 5-10 minutes after, ultrasonic disperse, supersonic frequency is 40-
80KHz, is kept for 5 minutes every time, is spaced 1 minute, is repeated 5-6 times.
3. according to the preparation method of a kind of modified graphene of claim 1 and nano-cellulose compound temperature-sensitive material, its feature exists
It is that source is wheat stalk in, described fiber, maize straw, soybean stalk, the one or more in bagasse.
4. according to a kind of preparation method of Thermo-sensitive graphite fiber alkene composite water conservation coated fertilizer of claim 1, it is characterised in that
Described freezes to put in freeze dryer, is refrigerated to -10--20 DEG C, is evacuated to drying chamber pressure 30-40Pa, heats 40-50 DEG C,
Until the ice in material all distils.
5. a kind of application method of Thermo-sensitive graphite fiber alkene composite water conservation coated fertilizer, it is characterised in that by the coating material
It is added to after feed powder is broken in the rotating disk of granulated fertilizer, parcel arrives fertilizer surface in the presence of atomized water, forms uniform
Clad, is heating and curing, cooling.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710438077.0A CN107253873A (en) | 2017-06-12 | 2017-06-12 | A kind of preparation method of Thermo-sensitive graphite fiber alkene composite water conservation coated fertilizer |
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| CN201710438077.0A CN107253873A (en) | 2017-06-12 | 2017-06-12 | A kind of preparation method of Thermo-sensitive graphite fiber alkene composite water conservation coated fertilizer |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110194446A (en) * | 2019-06-10 | 2019-09-03 | 广西科学院 | A kind of 2D cellulose obtained using cellulose depth hydrolysis is the graphene 2D raw powder's production technology of raw material |
| CN113036208A (en) * | 2021-02-26 | 2021-06-25 | 中山大学 | Advanced porous polymer nanosheet and preparation method and application thereof |
| CN116693965A (en) * | 2023-06-16 | 2023-09-05 | 青岛文武港科技有限公司 | Reusable PE (polyethylene) isolation preservative film |
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| CN105251453A (en) * | 2015-11-05 | 2016-01-20 | 江苏大学 | Preparation method and application of graphene/cellulose/titanium dioxide composite material |
| CN105481552A (en) * | 2015-12-12 | 2016-04-13 | 常州大学 | Preparation method for soybean straw slow-release nitrogen fertilizer |
| CN106179281A (en) * | 2016-08-15 | 2016-12-07 | 河南师范大学 | A kind of gold ion solid extracting agent and its preparation method and application |
| CN106747899A (en) * | 2016-11-11 | 2017-05-31 | 中国农业科学院农业资源与农业区划研究所 | A kind of film-coated and slow release fertilizer and preparation method thereof and making apparatus |
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2017
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| CN105251453A (en) * | 2015-11-05 | 2016-01-20 | 江苏大学 | Preparation method and application of graphene/cellulose/titanium dioxide composite material |
| CN105481552A (en) * | 2015-12-12 | 2016-04-13 | 常州大学 | Preparation method for soybean straw slow-release nitrogen fertilizer |
| CN106179281A (en) * | 2016-08-15 | 2016-12-07 | 河南师范大学 | A kind of gold ion solid extracting agent and its preparation method and application |
| CN106747899A (en) * | 2016-11-11 | 2017-05-31 | 中国农业科学院农业资源与农业区划研究所 | A kind of film-coated and slow release fertilizer and preparation method thereof and making apparatus |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110194446A (en) * | 2019-06-10 | 2019-09-03 | 广西科学院 | A kind of 2D cellulose obtained using cellulose depth hydrolysis is the graphene 2D raw powder's production technology of raw material |
| CN110194446B (en) * | 2019-06-10 | 2022-05-13 | 广西科学院 | Preparation method of graphene 2D powder taking 2D cellulose obtained by deeply hydrolyzing cellulose as raw material |
| CN113036208A (en) * | 2021-02-26 | 2021-06-25 | 中山大学 | Advanced porous polymer nanosheet and preparation method and application thereof |
| CN113036208B (en) * | 2021-02-26 | 2022-05-10 | 中山大学 | Advanced porous polymer nanosheet and preparation method and application thereof |
| CN116693965A (en) * | 2023-06-16 | 2023-09-05 | 青岛文武港科技有限公司 | Reusable PE (polyethylene) isolation preservative film |
| CN116693965B (en) * | 2023-06-16 | 2024-03-19 | 青岛文武港科技有限公司 | Reusable PE (polyethylene) isolation preservative film |
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Application publication date: 20171017 |