CN109135758A - A kind of preparation method of antimicrobial form water-loss reducer of soil - Google Patents
A kind of preparation method of antimicrobial form water-loss reducer of soil Download PDFInfo
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- CN109135758A CN109135758A CN201810872985.5A CN201810872985A CN109135758A CN 109135758 A CN109135758 A CN 109135758A CN 201810872985 A CN201810872985 A CN 201810872985A CN 109135758 A CN109135758 A CN 109135758A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09K17/00—Soil-conditioning materials or soil-stabilising materials
- C09K17/40—Soil-conditioning materials or soil-stabilising materials containing mixtures of inorganic and organic compounds
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
- A01N65/08—Magnoliopsida [dicotyledons]
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
- A01N65/08—Magnoliopsida [dicotyledons]
- A01N65/24—Lauraceae [Laurel family], e.g. laurel, avocado, sassafras, cinnamon or camphor
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Abstract
The present invention relates to a kind of preparation methods of antimicrobial form water-loss reducer of soil, belong to water-loss reducer of soil preparation technical field.The present invention is with thyme, Radix Glycyrrhizae and cortex cinnamomi are that raw material extracts reaction lotion, then reaction powder is mixed to prepare solidliquid mixture with lotion is reacted, then by acrylic acid and acrylamide, the mixing of phosphorus mine tailing, mixing suspension is made, mixing suspension and solidliquid mixture are mixed to prepare mixed dispersion liquid again, finally by mixed dispersion liquid and ammonium persulfate powder, sodium bicarbonate powder is mixed to prepare antimicrobial form water-loss reducer of soil, nano silver can destroy bacterium in the present invention, the electrolyte balance of the inside microbes such as virus, bacteriostasis antibiosis effect is set to be further enhanced, hydroxyl in resin, amino isopolarity group can generate colloid substance in conjunction with water, it combines closely with soil and is difficult to be lost, P elements are added in water-loss reducer of soil, to further strengthen the soaking effect of resin, it has broad application prospects.
Description
Technical field
The present invention relates to a kind of preparation methods of antimicrobial form water-loss reducer of soil, belong to water-loss reducer of soil preparation technical field.
Background technique
In northern China, farmland is mostly Arid&semi-arid area, serious water shortage, and productivity is low.Due to China's rainfall
It is on the low side, and be unevenly distributed, this directly affects the survival rate of the raising of agricultural productivity and trees of planting trees.Agricultural water
80% or more of China's total water consumption is accounted for, the shortage of water resource is the first cause for restricting China's agricultural development.Therefore agricultural is improved
The utilization efficiency of water resource implements the important channel that saving water, resisting drought technology is China's agricultural sustainable development.
In recent years, improve soil texture using water-retaining agent and improve crop water and fertilizer utilization rate, be the important side of water-saving technology
Formula.Water-loss reducer of soil is a kind of high molecular polymer with strong water absorption function and water holding capacity, is adsorbing several hundred thousands of times of water
Energy slow release is utilized for plant growth again afterwards, has the function of repeating to absorb water.Water-loss reducer of soil also rises other than water-retaining property
To the function of soil conditioner, Chemical industry.Improve the ecological environment, played in engineering of checking winds and fixing drifting sand determine success or failure work
With.Water-retaining agent is as new type functional material, using having been directed to multiple fields.Its raw material sources is extensive, and superior performance is grasped simultaneously
Make simply, it is without side-effects to environment, there is vast potential for future development.
Currently, water-loss reducer of soil is broadly divided into three classes: starch, cellulose family, synthesized polymer species.Starch soil is protected
Aqua has many advantages, such as that water suction and water retention are high, at low cost, but gel strength is lower after water suction, and long-term poor water retention property is using
In vulnerable to microorganism decompositions such as bacteriums lose water suction, water retention, and product poor heat resistance, unsuitable long term storage；Synthesis is poly-
Closing species water-loss reducer of soil is largely with acrylic acid, acrylamide etc. for monomer, and advantage is that reaction is easily achieved and water absorption rate
It is higher, but be not easy to be biodegradable, easily cause soil hardening, and higher cost；Cellulose has a variety of hydrophilic radicals, and
Since it is fibrous material, there are many capillaries, surface area is big, therefore has very strong water imbibition, is that total amount is most in the world
Greatly, the cheapest natural macromolecular material of price.It is good that cellulose water retention agent inhales salt performance, and pH value is easily adjusted, and biological can drop
Solution property is good, but its water absorption rate is low, the water holding time is short, while being also easy to be decomposed the ability for losing water suction, water conservation by bacterium.
Currently, water-retaining agent quality on the market is difficult to ensure, most water-retaining agent water conservation duration are too short, can inhale on surface
Water but time have grown the ability for just losing water suction and discharging water, cause to easily corrode plant root in soil moisture, dry
Soil hardening is easily caused under the conditions of drought.
Therefore, developing a kind of water-loss reducer of soil for being able to solve above-mentioned performance issue is highly desirable.
Summary of the invention
The technical problems to be solved by the invention: it is poor for current water-loss reducer of soil antibacterial ability, lead to water-loss reducer of soil
It is easily degraded by Bacteria destroyed, while water holding capacity is insufficient, the bad defect of water retention property provides a kind of antimicrobial form soil water-retaining
The preparation method of agent.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
A kind of preparation method of antimicrobial form water-loss reducer of soil, it is characterised in that specific preparation step are as follows:
(1) thyme, Radix Glycyrrhizae and cortex cinnamomi 3:1:1 in mass ratio are put into wide-mouth bottle, is impregnated with dehydrated alcohol, wide-mouth bottle is put
Enter sonic oscillation in ultrasonic vibration instrument, filtrate is obtained by filtration after oscillation, puts the filtrate into vacuum oven and be concentrated until product
Reaction lotion is made in constant weight；
(2) using silver-colored stick as electrode anode, platinum stick is powered as electrode cathode, silver nitrate solution as electrolyte, will after energization
Particle scrapes on platinum stick, and reaction powder is obtained after being washed with distilled water 3~5 times, by reaction powder with above-mentioned lotion of reacting by matter
Amount is uniformly mixed obtained solidliquid mixture than 1:20, spare；
(3) it weighs in 300~500g acrylic acid investment beaker, places the beaker in ice-water bath, sodium hydroxide is added dropwise into beaker
Solution adjusts pH value and weighs 20~22 powdered reaction liquid, 13~17 parts of acryloyls according to parts by weight to 4~6 obtained reaction solutions
In amine and 5~7 parts of phosphorus mine tailing investment three-necked flasks, three-necked flask is placed in water-bath and is vibrated, mixing suspension is made；
(4) spare solidliquid mixture is mixed with mixing suspension 1:5 in mass ratio in investment single-necked flask, by single-necked flask
It is put into magnetic agitation in water-bath, mixed dispersion liquid is made after stirring；
(5) the ammonium persulfate powder and mixed dispersion liquid quality 3 of above-mentioned mixed dispersion liquid quality 3~5% are added into three-necked flask
~5% sodium bicarbonate powder, 4~6h of isothermal reaction obtain filter residue after reaction, filter residue are placed in oven and dried, and put after dry
Enter in grinder and grind, antimicrobial form water-loss reducer of soil is made.
Bath temperature in ultrasonic vibration instrument as described in step (1) is 40~45 DEG C, and supersonic frequency is 30~32kHz,
The sonic oscillation time is 48~50h, and the temperature in vacuum oven is 20~25 DEG C, and vacuum degree is 80~100Pa.
The mass fraction of silver nitrate solution described in step (2) is 10~15%, and the voltage of direct current is 50~60V, is led to
The electric time is 6~8h.
The mass fraction of sodium hydroxide solution described in step (3) is 15~20%, the bath temperature of water-bath is 50~
60 DEG C, supersonic frequency is 40~45kHz, and duration of oscillation is 15~20min.
The bath temperature of water-bath described in step (4) is 50~60 DEG C, and the revolving speed of magnetic agitation is 300~350r/
Min, magnetic agitation time are 3~5h.
Bath temperature described in step (5) is 40~50 DEG C, and supersonic frequency when isothermal reaction is 40~45kHz, permanent
The warm reaction time is 4~6h, and the temperature in baking oven is 60~70 DEG C, and drying time is 3~4h.
The method have the benefit that:
(1) present invention extracts reaction lotion first by thyme, Radix Glycyrrhizae and cortex cinnamomi soaked in absolute ethyl alcohol in heated bath,
Again using silver-colored stick as anode, platinum stick as cathode, silver nitrate solution as electrolyte, it is powered and reaction powder is made, it then will be anti-
It answers powder to be mixed to prepare solidliquid mixture with lotion is reacted, then mixes acrylic acid with acrylamide, phosphorus mine tailing, be made mixed
Suspension is closed, then mixing suspension and solidliquid mixture are mixed to prepare mixed dispersion liquid, finally by mixed dispersion liquid and over cure
Sour ammonium powder, sodium bicarbonate powder are mixed in hybrid reaction under conditions of heated bath and sonic oscillation, filtering, dry, grinding system
Antimicrobial form water-loss reducer of soil, the present invention extract plant extraction liquid from thyme, Radix Glycyrrhizae and cortex cinnamomi, thyme, Radix Glycyrrhizae and
In cortex cinnamomi have spice plant nutrition liquid abundant, these plant nutrition liquid dissolution of bacteria, germ cell membrane, make cytoplasm
Outflow destroys the cellular morphology of bacterium, germ, makes bacterium, germ loss of activity, to achieve the effect that antibacterial, passes through simultaneously
Nano-Ag particles are made in the mode of electrolysis, and nano silver is mixed with plant extraction liquid, and nano silver can destroy bacterium, virus etc.
The electrolyte balance of inside microbes, dispersed nano-silver particles mention bacteriostasis antibiosis effect further
Height is difficult water-loss reducer of soil by microorganism absorption degradation；
(2) for the present invention using acrylic acid and acrylamide as Material synthesis high hydroscopic resin, this resin material microstructure is in three
Network structure is tieed up, the hydrophilic radicals such as carboxyl, hydroxyl, amide groups and sulfonic acid group, hydrophilic radical absorption are all had on main chain, side chain
The ability that moisture makes resin material have water conservation, makes moisture be not easy to be lost easily, while hydroxyl, amino isopolarity base in resin
Group can generate colloid substance in conjunction with water, combine closely with soil and be difficult to be lost, so that water holding capacity is further strengthened, by phosphorus
Element is added in water-loss reducer of soil, and phosphonium ion can move on polymer chain, and phosphonium ion and other cations form electrostatic reprimand
Power expands cation to outside, forms osmotic pressure by the difference of cation interior extracellular concentration in internal networking structure, makes water
Molecule can easily penetrate into resin internal networking structure, to further strengthen the soaking effect of resin, have wide
Application prospect.
Specific embodiment
Thyme, Radix Glycyrrhizae and cortex cinnamomi 3:1:1 in mass ratio are put into wide-mouth bottle, impregnated with dehydrated alcohol, by wide-mouth bottle
Be put into ultrasonic vibration instrument, bath temperature be 40~45 DEG C, supersonic frequency be 30~32kHz under conditions of sonic oscillation 48~
50h is obtained by filtration filtrate after oscillation, puts the filtrate into vacuum oven, temperature be 20~25 DEG C, vacuum degree be 80~
Concentration under conditions of 100Pa is until reaction lotion is made in product constant weight；Using silver-colored stick as electrode anode, platinum stick is as electrode yin
Pole, the silver nitrate solution that mass fraction is 10~15% are used as electrolyte, are powered 6 under conditions of voltage is 50~60V direct current
~8h scrapes particle on platinum stick after energization, obtained after being washed with distilled water 3~5 times reaction powder, will reaction powder with it is above-mentioned
It reacts lotion 1:20 in mass ratio and is uniformly mixed obtained solidliquid mixture, it is spare；Weigh 300~500g acrylic acid investment beaker
In, it places the beaker in ice-water bath, the sodium hydroxide solution that mass fraction is 15~20% is added dropwise into beaker and adjusts pH value to 4
~6 obtained reaction solutions weigh 20~22 powdered reaction liquid, 13~17 parts of acrylamides and 5~7 parts of phosphorus tails according to parts by weight
Miberal powder is put into three-necked flask, three-necked flask is placed in the water-bath that bath temperature is 50~60 DEG C, is 40 in supersonic frequency
15~20min is vibrated under conditions of~45kHz, and mixing suspension is made；Spare solidliquid mixture is pressed with mixing suspension
In mass ratio 1:5 mixing investment single-necked flask, single-necked flask is put into the water-bath that bath temperature is 50~60 DEG C, with 300
Mixed dispersion liquid is made in revolving speed 3~5h of magnetic agitation of~350r/min after stirring；Above-mentioned mixing point is added into three-necked flask
The ammonium persulfate powder of dispersion liquid quality 3~5% and the sodium bicarbonate powder of mixed dispersion liquid quality 3~5% are 40 in bath temperature
~50 DEG C, supersonic frequency is 4~6h of isothermal reaction under conditions of 40~45kHz, obtains filter residue after reaction, filter residue is put into temperature
For 3~4h dry in 60~70 DEG C of baking ovens, it is put into grinder and grinds after dry, antimicrobial form water-loss reducer of soil is made.
Thyme, Radix Glycyrrhizae and cortex cinnamomi 3:1:1 in mass ratio are put into wide-mouth bottle, impregnated with dehydrated alcohol, by wide-mouth bottle
It is put into ultrasonic vibration instrument, is 40 DEG C in bath temperature, supersonic frequency is sonic oscillation 48h under conditions of 30kHz, mistake after oscillation
Filter obtains filtrate, puts the filtrate into vacuum oven, is 20 DEG C in temperature, concentration under conditions of vacuum degree is 80Pa is until produce
Reaction lotion is made in object constant weight；Using silver-colored stick as electrode anode, platinum stick is as electrode cathode, the silver nitrate that mass fraction is 10%
Solution is as electrolyte, and be powered 6h under conditions of voltage is 50V direct current, scrapes particle on platinum stick after energization, with distillation
Reaction powder is obtained after water washing 3 times, and reaction powder is uniformly mixed obtained solid-liquid with the above-mentioned lotion 1:20 in mass ratio that reacts
Mixture, it is spare；It weighs in 300g acrylic acid investment beaker, places the beaker in ice-water bath, mass fraction is added dropwise into beaker
20 powdered reaction liquid, 13 part third are weighed according to parts by weight for 15% sodium hydroxide solution adjusting pH value to 4 obtained reaction solutions
In acrylamide and 5 parts of phosphorus mine tailing investment three-necked flasks, three-necked flask is placed in the water-bath that bath temperature is 50 DEG C, super
Acoustic frequency vibrates 15min under conditions of being 40kHz, and mixing suspension is made；By spare solidliquid mixture and mixing suspension
In the mixing investment single-necked flask of 1:5 in mass ratio, single-necked flask is put into the water-bath that bath temperature is 50 DEG C, with 300r/
Mixed dispersion liquid is made in the revolving speed magnetic agitation 3h of min after stirring；Above-mentioned mixed dispersion liquid quality 3% is added into three-necked flask
Ammonium persulfate powder and mixed dispersion liquid quality 3% sodium bicarbonate powder, be 40 DEG C in bath temperature, supersonic frequency is
Isothermal reaction 4h under conditions of 40kHz obtains filter residue after reaction, and filter residue is put into dry 3h in the baking oven that temperature is 60 DEG C, is done
It is put into grinder and grinds after dry, antimicrobial form water-loss reducer of soil is made.
Thyme, Radix Glycyrrhizae and cortex cinnamomi 3:1:1 in mass ratio are put into wide-mouth bottle, impregnated with dehydrated alcohol, by wide-mouth bottle
It is put into ultrasonic vibration instrument, is 43 DEG C in bath temperature, supersonic frequency is sonic oscillation 49h under conditions of 31kHz, mistake after oscillation
Filter obtains filtrate, puts the filtrate into vacuum oven, is 23 DEG C in temperature, concentration under conditions of vacuum degree is 90Pa is until produce
Reaction lotion is made in object constant weight；Using silver-colored stick as electrode anode, platinum stick is as electrode cathode, the silver nitrate that mass fraction is 13%
Solution is as electrolyte, and be powered 7h under conditions of voltage is 55V direct current, scrapes particle on platinum stick after energization, with distillation
Reaction powder is obtained after water washing 4 times, and reaction powder is uniformly mixed obtained solid-liquid with the above-mentioned lotion 1:20 in mass ratio that reacts
Mixture, it is spare；It weighs in 400g acrylic acid investment beaker, places the beaker in ice-water bath, mass fraction is added dropwise into beaker
21 powdered reaction liquid, 15 part third are weighed according to parts by weight for 17% sodium hydroxide solution adjusting pH value to 5 obtained reaction solutions
In acrylamide and 6 parts of phosphorus mine tailing investment three-necked flasks, three-necked flask is placed in the water-bath that bath temperature is 55 DEG C, super
Acoustic frequency vibrates 17min under conditions of being 43kHz, and mixing suspension is made；By spare solidliquid mixture and mixing suspension
In the mixing investment single-necked flask of 1:5 in mass ratio, single-necked flask is put into the water-bath that bath temperature is 55 DEG C, with 325r/
Mixed dispersion liquid is made in the revolving speed magnetic agitation 4h of min after stirring；Above-mentioned mixed dispersion liquid quality 4% is added into three-necked flask
Ammonium persulfate powder and mixed dispersion liquid quality 4% sodium bicarbonate powder, be 45 DEG C in bath temperature, supersonic frequency is
Isothermal reaction 5h under conditions of 43kHz obtains filter residue after reaction, and filter residue is put into dry 3h in the baking oven that temperature is 65 DEG C, is done
It is put into grinder and grinds after dry, antimicrobial form water-loss reducer of soil is made.
Thyme, Radix Glycyrrhizae and cortex cinnamomi 3:1:1 in mass ratio are put into wide-mouth bottle, impregnated with dehydrated alcohol, by wide-mouth bottle
It is put into ultrasonic vibration instrument, is 45 DEG C in bath temperature, supersonic frequency is sonic oscillation 50h under conditions of 32kHz, mistake after oscillation
Filter obtain filtrate, put the filtrate into vacuum oven, temperature be 25 DEG C, vacuum degree be 100Pa under conditions of concentration until
Reaction lotion is made in product constant weight；Using silver-colored stick as electrode anode, platinum stick is as electrode cathode, the nitric acid that mass fraction is 15%
Silver-colored solution is as electrolyte, and be powered 8h under conditions of voltage is 60V direct current, scrapes particle on platinum stick after energization, with steaming
Distilled water wash 5 times after obtain reaction powder, will reaction powder with it is above-mentioned react lotion 1:20 in mass ratio be uniformly mixed be made admittedly
Liquid mixture, it is spare；It weighs in 500g acrylic acid investment beaker, places the beaker in ice-water bath, quality point is added dropwise into beaker
Number weighs 22 powdered reaction liquid, 17 parts according to parts by weight to 6 obtained reaction solutions for 20% sodium hydroxide solution adjusting pH value
In acrylamide and 7 parts of phosphorus mine tailing investment three-necked flasks, three-necked flask is placed in the water-bath that bath temperature is 60 DEG C,
Supersonic frequency vibrates 20min under conditions of being 45kHz, and mixing suspension is made；By spare solidliquid mixture with mix it is suspended
In liquid 1:5 in mass ratio mixing investment single-necked flask, single-necked flask is put into the water-bath that bath temperature is 60 DEG C, with
Mixed dispersion liquid is made in the revolving speed magnetic agitation 5h of 350r/min after stirring；Above-mentioned mixed dispersion liquid is added into three-necked flask
The ammonium persulfate powder of quality 5% and the sodium bicarbonate powder of mixed dispersion liquid quality 5% are 50 DEG C in bath temperature, supersonic frequency
Rate is isothermal reaction 6h under conditions of 45kHz, obtains filter residue after reaction, filter residue is put into dry in the baking oven that temperature is 70 DEG C
4h is put into grinder after dry and grinds, and antimicrobial form water-loss reducer of soil is made.
The water-loss reducer of soil that comparative example is produced with company of Hefei City is as a comparison case to antimicrobial form soil produced by the present invention
Water-loss reducer of soil in earth water-retaining agent and comparative example is detected, and testing result is as shown in table 1:
Water absorption rate test
1g example 1~3 prepared by the present invention and comparative example water-loss reducer of soil are weighed respectively, are put into deionized water and are impregnated for 24 hours, use
Sieve filters off residual moisture, and weighing measures water absorption rate.Water absorption rate calculating formula are as follows:
Water absorption rate=(quality of water-retaining agent-drying water-retaining agent quality after water suction)/drying water-retaining agent quality.
Water-retaining agent after above-mentioned water suction is placed in centrifuge (1000r/min) by retentiveness test to carry out at centrifugation oscillation
It manages, after 1min, outwells the water isolated, electronic scale weighs up its quality again by above-mentioned residue, measures retentiveness.Retentiveness meter
Formula are as follows:
After the oscillation of retentiveness=centrifugation after quality/water suction of water-retaining agent water-retaining agent quality.
It is tested with wheat paddock and 8 mu of wheat paddocks of areal is tested, be divided into 4 groups, each 2 mu, respectively test
Group 1~3 and control group, experimental group 1~3 apply the water-loss reducer of soil of Examples 1 to 3 respectively, and control group applies the soil of comparative example
Earth water-retaining agent.It is counted, is tried with sowing the wheat after 15d to the fresh weight of the emergence rate of wheat, soil moisture content, wheat plant
It tests and the results are shown in Table 1.
1 performance measurement result of table
| Test item | Example 1 | Example 2 | Example 3 | Comparative example |
| Water absorption rate (%) | 694 | 712 | 122 | 462 |
| Retentiveness (%) | 89.1 | 90.5 | 92.3 | 31.5 |
| Bacteriostasis rate (%) | 96.7 | 97.3 | 97.8 | 72.5 |
| Wheat bud ratio (%) | 89.1 | 89.5 | 90.2 | 78.2 |
| Soil moisture content (%) | 13.42 | 13.51 | 13.66 | 8.98 |
| Wheat plant fresh weight (g/5 plants) | 1.54 | 1.61 | 1.65 | 1.08 |
According to data in table 1 it is found that antimicrobial form water-loss reducer of soil produced by the present invention, has both excellent water absorbing properties and water-retaining property
Can, and fungistatic effect is obvious, has broad prospects in the development of water-keeping material industry.
Claims (6)
1. a kind of preparation method of antimicrobial form water-loss reducer of soil, it is characterised in that specific preparation step are as follows:
(1) thyme, Radix Glycyrrhizae and cortex cinnamomi 3:1:1 in mass ratio are put into wide-mouth bottle, is impregnated with dehydrated alcohol, wide-mouth bottle is put
Enter sonic oscillation in ultrasonic vibration instrument, filtrate is obtained by filtration after oscillation, puts the filtrate into vacuum oven and be concentrated until product
Reaction lotion is made in constant weight；
(2) using silver-colored stick as electrode anode, platinum stick is powered as electrode cathode, silver nitrate solution as electrolyte, will after energization
Particle scrapes on platinum stick, and reaction powder is obtained after being washed with distilled water 3~5 times, by reaction powder with above-mentioned lotion of reacting by matter
Amount is uniformly mixed obtained solidliquid mixture than 1:20, spare；
(3) it weighs in 300~500g acrylic acid investment beaker, places the beaker in ice-water bath, sodium hydroxide is added dropwise into beaker
Solution adjusts pH value and weighs 20~22 powdered reaction liquid, 13~17 parts of acryloyls according to parts by weight to 4~6 obtained reaction solutions
In amine and 5~7 parts of phosphorus mine tailing investment three-necked flasks, three-necked flask is placed in water-bath and is vibrated, mixing suspension is made；
(4) spare solidliquid mixture is mixed with mixing suspension 1:5 in mass ratio in investment single-necked flask, by single-necked flask
It is put into magnetic agitation in water-bath, mixed dispersion liquid is made after stirring；
(5) the ammonium persulfate powder and mixed dispersion liquid quality 3 of above-mentioned mixed dispersion liquid quality 3~5% are added into three-necked flask
~5% sodium bicarbonate powder, 4~6h of isothermal reaction obtain filter residue after reaction, filter residue are placed in oven and dried, and put after dry
Enter in grinder and grind, antimicrobial form water-loss reducer of soil is made.
2. a kind of preparation method of antimicrobial form water-loss reducer of soil according to claim 1, it is characterised in that: in step (1)
Bath temperature in the ultrasonic vibration instrument is 40~45 DEG C, and supersonic frequency is 30~32kHz, the sonic oscillation time is 48~
50h, the temperature in vacuum oven are 20~25 DEG C, and vacuum degree is 80~100Pa.
3. a kind of preparation method of antimicrobial form water-loss reducer of soil according to claim 1, it is characterised in that: in step (2)
The mass fraction of the silver nitrate solution is 10~15%, and the voltage of direct current is 50~60V, and conduction time is 6~8h.
4. a kind of preparation method of antimicrobial form water-loss reducer of soil according to claim 1, it is characterised in that: in step (3)
The mass fraction of the sodium hydroxide solution is 15~20%, and the bath temperature of water-bath is 50~60 DEG C, supersonic frequency 40
~45kHz, duration of oscillation are 15~20min.
5. a kind of preparation method of antimicrobial form water-loss reducer of soil according to claim 1, it is characterised in that: in step (4)
The bath temperature of the water-bath is 50~60 DEG C, and the revolving speed of magnetic agitation is 300~350r/min, and the magnetic agitation time is
3~5h.
6. a kind of preparation method of antimicrobial form water-loss reducer of soil according to claim 1, it is characterised in that: in step (5)
The bath temperature is 40~50 DEG C, and supersonic frequency when isothermal reaction is 40~45kHz, and the isothermal reaction time is 4~6h,
Temperature in baking oven is 60~70 DEG C, and drying time is 3~4h.
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Application publication date: 20190104 |