A kind of preparation method of water-loss reducer of soilTechnical field
The present invention relates to technical field of land improvement, and in particular to a kind of preparation method of water-loss reducer of soil.
Background technology
Reasonable is efficiently the key issue that must focus in agricultural production using limited water resource, few in aridRain, soil are barren, the area of vegetation sparse, and water shortage is even more to limit the principal element of agricultural development.Water-loss reducer of soil is special due to itDifferent chemical composition, physical arrangement and water absorbing properties, in farmland, drought-resistant water-preserving, keep a full stand of seedings volume increase and flowers and trees production etc. have extensivelyWealthy application prospect.
Different according to synthetic material, water-loss reducer can be divided into synthetic resin water-loss reducer, starch water-loss reducer and cellulose familyThe type of water-loss reducer etc. 3.Wherein the water suction of synthetic resin water-loss reducer, water holding capacity are strong, but degradability is poor；Starch water-loss reducerGel strength is low after water suction, and fungus resistance is poor；Cellulose water retention agent suction salt performance is good, and pH value is easily adjusted, biodegradable, butIt is that its water absorption rate is low, the water holding time is short, but cellulose base water-loss reducer is still the optimal green water-loss reducer of the feature of environmental protection.
With the fast development of biogas engineering, the biogas residue resource as fermentation residue is also increasingly abundanter.Utilize biogas residueIn cellulose carry out graft modification prepare water-loss reducer of soil, be to realize a kind of new method that changing rejected material to useful resource efficiently utilizes.
Water absorption rate height and the novel cellulose base water conservation of water holding time length are prepared while utilization of waste as resourceAgent has positive meaning to soil moisture preservation technique field.
The content of the invention
Present invention mainly solves technical problem, have that water absorption rate is low and retentiveness is poor for current cellulose base water-loss reducerThe defects of, there is provided a kind of preparation method of water-loss reducer of soil.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of preparation method of water-loss reducer of soil, it is characterised in that specifically preparation process is：
（1）Heat and boil after maize straw biogas residue and sodium hydroxide solution are mixed, after naturally cool to being filtered after room temperature, separateFilter residue is obtained, heat temperature raising after filter residue, ethylenediamine and sodium periodate solution are mixed, filters after stirring reaction, separates againIt is standby to filter cake；
（2）Weigh new fresh and tender ginger and be put into squeezing in squeezer and obtain ginger juice, ginger juice is fitted into stainless steel pallet, is put into refrigeratorPrecooling, obtain precooling ginger juice；
（3）By buffalo milk and standby filter cake by etc. mass ratio mix after heat and boil, obtain mixed liquor, treat that it naturally cools to 70Mixed liquor is blended into above-mentioned precooling ginger juice again at~80 DEG C, 5~8min is stood and treats its solidification, obtain gelatinous mixture；
（4）Water-loss reducer crude product is obtained after above-mentioned gelatinous mixture is ground, water-loss reducer crude product and Silane coupling agent KH550 is moltenSonic oscillation impregnates and is separated by filtration to obtain dipping filter residue after liquid mixing, dries to constant weight, obtains pre-processing water-loss reducer crude product；
（5）Poured into after above-mentioned pretreatment water-loss reducer crude product and acrylonitrile are mixed in DMF, add peroxideChange benzoyl, the heat temperature raising under nitrogen guard mode, insulated and stirred reaction, question response terminates rear centrifugal treating, isolatedCentrifugation；
（6）After above-mentioned centrifugation is rinsed with absolute ethyl alcohol, after the centrifugation after flushing and sodium hydroxide solution are mixedHeat temperature raising, filtered after stirring saponification, isolated saponification filter residue, finally by saponification filter residue and drying, gained desciccateAs water-loss reducer of soil.
Step（1）Described in maize straw biogas residue and sodium hydroxide solution mass ratio be 1：10, sodium hydroxide solutionMass fraction be 20%, it be 1~2h that processing time is boiled in heating, and the mass ratio of filter residue, ethylenediamine and sodium periodate solution is 6：1：20, the mass fraction of sodium periodate solution is 10%, and the temperature of heat temperature raising is 75~85 DEG C, the stirring reaction time is 1~2h。
Step（2）Described in precooling temperature be 4~6 DEG C, pre-coo time is 20~30min.
Step（3）Described in mixed liquor and precooling ginger juice mass ratio be 5:1.
Step（4）Described in water-loss reducer crude product and Silane coupling agent KH550 solution mass ratio be 1:10, it is silane coupledThe mass fraction of agent KH550 solution is 5%, and the power of sonic oscillation dipping is 200~300W, and the frequency of sonic oscillation dipping is25~35kHz, sonic oscillation dip time are 1~2h.
Step（5）Described in pretreatment water-loss reducer crude product and acrylonitrile mass ratio be 2:25, N, N- dimethyl formylThe quality of amine is 5~8 times of pretreatment both water-loss reducer crude product and acrylonitrile gross mass, and the addition of benzoyl peroxide is guarantorThe 2% of aqua crude product quality, the temperature of heat temperature raising is 60~65 DEG C, and the insulated and stirred reaction time is 4~6h.
Step（6）Described in flushing after centrifugation and sodium hydroxide solution mass ratio be 1:10, sodium hydroxideThe concentration of solution is 0.5mol/L, and the temperature of heat temperature raising is 75~85 DEG C, and the stirring saponification time is 1~2h.
The beneficial effects of the invention are as follows：
（1）The present invention will be enriched in the maize straw biogas residue of fibre composition first and alkali lye mixing is boiled, and alkali soluble is removed by cookingProperty lignin component, and make under thermodynamic activity fiber solution fine, reduce the crystallinity of fiber, increase its plasticity, then in secondIt is exposed the hydroxyl of fibrous inside in the presence of diamines and sodium metaperiodate, while part of hydroxyl is oxidized to hydrophilic carboxylicBase and aldehyde radical, fiber surface hydrophily carboxyl and aldehyde radical quantity are added, reach the mesh for improving cellulose base water-loss reducer water absorption rate's；
（2）The present invention, which mixes the fiber after hydrophilic modifying and the buffalo milk of high fat content, to boil, and by the mixing after boilingLiquid is blended into the ginger juice of precooling, using the casein in the Ginger Protease and buffalo milk in ginger juice, is reacted at high temperature, in short-termIn be frozen into spawn and be attached to fiber surface, obtain water-loss reducer crude product, then protecting by the method for radical polymerizationAqua crude product surface grafting polyacrylonitrile, finally makes itrile group be transformed into hydrophily carboxyl and acid amides its saponification in the basic conditionsBase, the further water absorption rate for improving water-loss reducer, while the introducing of gel particle make it that the water of water-loss reducer absorption is in combine water shapeState, more the problem of water-loss reducer retentiveness difference is caused with the presence of free water state after traditional water-loss reducer absorption water are avoided, are effectively carriedThe high water retention property of water-loss reducer, has broad application prospects.
Embodiment
It is 1 in mass ratio：Maize straw biogas residue and mass fraction are to be put into iron pan after 20% sodium hydroxide solution mixes by 10In, 1~2h of processing is boiled in heating, after naturally cool to being filtered after room temperature, isolated filter residue, then be 6 in mass ratio：1：20 will75~85 DEG C are heated to after the sodium periodate solution mixing that filter residue, ethylenediamine and mass fraction are 10%, stirring reaction 1~Filtered again after 2h, isolated filter cake；Weigh new fresh and tender ginger and be put into 20~30min of squeezing in squeezer, collection is squeezedThe ginger juice arrived, ginger juice is fitted into stainless steel pallet, is put into refrigerator, 20~30min of precooling at 4~6 DEG C, obtains precooling gingerJuice；Collect buffalo milk and buffalo milk and filter cake are boiled 5~10min, obtain mixed liquor, treat it by waiting mass ratio to be heated after mixingIt is 5 in mass ratio again when naturally cooling to 70~80 DEG C:1 is blended into mixed liquor in precooling ginger juice, stands 5~8min and treats that it is solidifyingGu obtain gelatinous mixture；Gelatinous mixture is put into 10~15min of grinding in ball mill and obtains water-loss reducer crude product, is pressedMass ratio is 1:Water-loss reducer crude product and mass fraction are to be put into sonic oscillation after 5% Silane coupling agent KH550 solution mixes by 10Instrument, filter residue must be impregnated to be separated by filtration after 1~2h of 200~300W power and 25~35kHz frequency ultrasound vibration dipping, is putEnter baking oven to dry to constant weight at 105~110 DEG C, obtain pre-processing water-loss reducer crude product；It is 2 in mass ratio:25 protect pretreatmentPoured into after aqua crude product and acrylonitrile mixing in the DMF of 5~8 times of both gross masses, then to N, N- dimethylThe benzoyl peroxide of water-loss reducer crude product quality 2% is added in formamide, 60~65 are heated under nitrogen guard modeDEG C, insulated and stirred reacts 4~6h, question response terminate after by 10~15min of reaction solution centrifugal treating, isolated centrifugation；It is in mass ratio 1 after centrifugation is rinsed 3~5 times with absolute ethyl alcohol:Centrifugation after flushing and concentration are by 1075~85 DEG C are heated to after the mixing of 0.5mol/L sodium hydroxide solutions, is filtered after 1~2h of stirring saponification, it is isolatedSaponification filter residue, saponification filter residue is finally put into baking oven, after drying 1~2h at 105~110 DEG C, gained desciccate is soilEarth water-loss reducer.
Example 1
It is 1 in mass ratio：Maize straw biogas residue and mass fraction are to be put into after 20% sodium hydroxide solution mixes in iron pan by 10,Processing 1h is boiled in heating, after naturally cool to being filtered after room temperature, isolated filter residue, then be 6 in mass ratio：1：20 by filter residue,75 DEG C are heated to after ethylenediamine and the sodium periodate solution mixing that mass fraction is 10%, is filtered again after stirring reaction 1h,Isolated filter cake；Weigh new fresh and tender ginger and be put into squeezer and squeeze 20min, collect the ginger juice that squeezing obtains, ginger juice is filledEnter in stainless steel pallet, be put into refrigerator, the precooling 20min at 4 DEG C, obtain precooling ginger juice；Collect buffalo milk and by buffalo milk andFilter cake boils 5min by heating after waiting mass ratio mixing, obtains mixed liquor, is in mass ratio again when it naturally cools to 70 DEG C5:1 is blended into mixed liquor in precooling ginger juice, stands 5min and treats its solidification, obtains gelatinous mixture；Gelatinous mixture is putEnter to grind 10min in ball mill and obtain water-loss reducer crude product, be in mass ratio 1:Water-loss reducer crude product and mass fraction are 5% silicon by 10Sonic oscillation instrument is put into after the mixing of alkane coupling agent KH550 solution, dipping 1h is vibrated with 200W power and 25kHz frequency ultrasoundAfter be separated by filtration and must impregnate filter residue, be put into baking oven and dried at 105 DEG C to constant weight, obtain pre-processing water-loss reducer crude product；By qualityThan for 2:25 will pour into the DMF of 5 times of both gross masses after pretreatment water-loss reducer crude product and acrylonitrile mixingIn, then the benzoyl peroxide of water-loss reducer crude product quality 2% is added into DMF, under nitrogen guard modeBe heated to 60 DEG C, insulated and stirred reaction 4h, question response terminate after by reaction solution centrifugal treating 10min, isolated centrifugationPrecipitation；It is in mass ratio 1 after centrifugation is rinsed 3 times with absolute ethyl alcohol:Centrifugation after flushing and concentration are by 1075 DEG C are heated to after the mixing of 0.5mol/L sodium hydroxide solutions, is filtered after stirring saponification 1h, isolated saponification filterSlag, saponification filter residue is finally put into baking oven, after drying 1h at 105 DEG C, gained desciccate is water-loss reducer of soil.
Example 2
It is 1 in mass ratio：Maize straw biogas residue and mass fraction are to be put into after 20% sodium hydroxide solution mixes in iron pan by 10,Processing 2h is boiled in heating, after naturally cool to being filtered after room temperature, isolated filter residue, then be 6 in mass ratio：1：20 by filter residue,80 DEG C are heated to after ethylenediamine and the sodium periodate solution mixing that mass fraction is 10%, is filtered again after stirring reaction 1h,Isolated filter cake；Weigh new fresh and tender ginger and be put into squeezer and squeeze 25min, collect the ginger juice that squeezing obtains, ginger juice is filledEnter in stainless steel pallet, be put into refrigerator, at 5 DEG C precooling 25min, obtain precooling ginger juice；Collect buffalo milk and by buffalo milk andFilter cake boils 8min by heating after waiting mass ratio mixing, obtains mixed liquor, is in mass ratio again when it naturally cools to 75 DEG C5:1 is blended into mixed liquor in precooling ginger juice, stands 7min and treats its solidification, obtains gelatinous mixture；Gelatinous mixture is putEnter to grind 13min in ball mill and obtain water-loss reducer crude product, be in mass ratio 1:Water-loss reducer crude product and mass fraction are 5% silicon by 10Sonic oscillation instrument is put into after the mixing of alkane coupling agent KH550 solution, dipping 1h is vibrated with 250W power and 30kHz frequency ultrasoundAfter be separated by filtration and must impregnate filter residue, be put into baking oven and dried at 108 DEG C to constant weight, obtain pre-processing water-loss reducer crude product；By qualityThan for 2:25 will pour into the DMF of 7 times of both gross masses after pretreatment water-loss reducer crude product and acrylonitrile mixingIn, then the benzoyl peroxide of water-loss reducer crude product quality 2% is added into DMF, under nitrogen guard modeBe heated to 63 DEG C, insulated and stirred reaction 5h, question response terminate after by reaction solution centrifugal treating 13min, isolated centrifugationPrecipitation；It is in mass ratio 1 after centrifugation is rinsed 4 times with absolute ethyl alcohol:Centrifugation after flushing and concentration are by 1080 DEG C are heated to after the mixing of 0.5mol/L sodium hydroxide solutions, is filtered after stirring saponification 1h, isolated saponification filterSlag, saponification filter residue is finally put into baking oven, after drying 1h at 108 DEG C, gained desciccate is water-loss reducer of soil.
Example 3
It is 1 in mass ratio：Maize straw biogas residue and mass fraction are to be put into after 20% sodium hydroxide solution mixes in iron pan by 10,Processing 2h is boiled in heating, after naturally cool to being filtered after room temperature, isolated filter residue, then be 6 in mass ratio：1：20 by filter residue,85 DEG C are heated to after ethylenediamine and the sodium periodate solution mixing that mass fraction is 10%, is filtered again after stirring reaction 2h,Isolated filter cake；Weigh new fresh and tender ginger and be put into squeezer and squeeze 30min, collect the ginger juice that squeezing obtains, ginger juice is filledEnter in stainless steel pallet, be put into refrigerator, the precooling 30min at 6 DEG C, obtain precooling ginger juice；Collect buffalo milk and by buffalo milk andFilter cake boils 10min by heating after waiting mass ratio mixing, obtains mixed liquor, is in mass ratio again when it naturally cools to 80 DEG C5:1 is blended into mixed liquor in precooling ginger juice, stands 8min and treats its solidification, obtains gelatinous mixture；Gelatinous mixture is putEnter to grind 15min in ball mill and obtain water-loss reducer crude product, be in mass ratio 1:Water-loss reducer crude product and mass fraction are 5% silicon by 10Sonic oscillation instrument is put into after the mixing of alkane coupling agent KH550 solution, dipping 2h is vibrated with 300W power and 35kHz frequency ultrasoundAfter be separated by filtration and must impregnate filter residue, be put into baking oven and dried at 110 DEG C to constant weight, obtain pre-processing water-loss reducer crude product；By qualityThan for 2:25 will pour into the DMF of 8 times of both gross masses after pretreatment water-loss reducer crude product and acrylonitrile mixingIn, then the benzoyl peroxide of water-loss reducer crude product quality 2% is added into DMF, under nitrogen guard modeBe heated to 65 DEG C, insulated and stirred reaction 6h, question response terminate after by reaction solution centrifugal treating 15min, isolated centrifugationPrecipitation；It is in mass ratio 1 after centrifugation is rinsed 5 times with absolute ethyl alcohol:Centrifugation after flushing and concentration are by 1085 DEG C are heated to after the mixing of 0.5mol/L sodium hydroxide solutions, is filtered after stirring saponification 2h, isolated saponification filterSlag, saponification filter residue is finally put into baking oven, after drying 2h at 110 DEG C, gained desciccate is water-loss reducer of soil.
Reference examples
The cellulose family water-loss reducer of soil of Shaanxi company production is as reference examples；
The cellulose water retention agent provided in water-loss reducer of soil produced by the present invention and reference examples is subjected to water absorption rate and retentivenessTest；
Water absorption rate test method：1g water-loss reducer of soil is weighed, is put into pure water and soaks 24h, residual moisture is filtered off with screen cloth, claimsWeight, determine water absorption rate.Water absorption rate calculating formula is：
Water absorption rate=（The quality of the quality of water-loss reducer-drying water-loss reducer after water suction）The quality of/drying water-loss reducer；
Retentiveness method of testing：Water-loss reducer after above-mentioned water suction is placed in centrifuge（1 000 r/min）In carry out centrifugation vibrationHandle, after 1 min, outwell the water isolated, electronic scale weighs up its quality again by above-mentioned residue, determines retentiveness.Water holdingProperty calculating formula is：
After the vibration of retentiveness=centrifugation after quality/water suction of water-loss reducer water-loss reducer quality；
Test result is shown in Table 1
Table 1
| Test event | Example 1 | Example 2 | Example 3 | Reference examples |
| Dry the quality of water-loss reducer（g） | 1 | 1 | 1 | 1 |
| The quality of water-loss reducer after water suction（g） | 657 | 669 | 682 | 456 |
| The quality of water-loss reducer after centrifugation vibration（g） | 560 | 582 | 595 | 156 |
| Water absorption rate（%） | 656 | 668 | 682 | 455 |
| Retentiveness（%） | 85.2 | 86.9 | 87.2 | 34.2 |
The obtained water-loss reducer of soil water absorption rate of the present invention is high it can be seen from experimental data in table 1, and retentiveness is excellent, has wideWealthy application prospect.