CN101948260A - Capsule type snow ice melt inhibiting material, preparation method and application thereof - Google Patents
Capsule type snow ice melt inhibiting material, preparation method and application thereof Download PDFInfo
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- CN101948260A CN101948260A CN2010101065452A CN201010106545A CN101948260A CN 101948260 A CN101948260 A CN 101948260A CN 2010101065452 A CN2010101065452 A CN 2010101065452A CN 201010106545 A CN201010106545 A CN 201010106545A CN 101948260 A CN101948260 A CN 101948260A
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Abstract
The invention provides a capsule type snow ice melt inhibiting material doped into asphalt pavement filling materials in road building or pavement building, a preparation method and application thereof. The capsule type snow ice melt inhibiting material consists of a capsule wall, a capsule core and protection solution, wherein the capsule core is formed by mixing an absorbent with a grain diameter of 30 micrometers and a nanometer bone material, wherein the absorbent is modified by absorbing calcium acetate and magnesium acetate; the mass ratio of capsule wall chitosan or ethyl cellulose to polyethylene glycol is 1:1, the ratio of the mass sum of the modified adsorbent and the bone material to the capsule wall mass is 10:1; the mass ratio of the modified adsorbent to the bone material is 7:3; the mass ratio of the modified adsorbent to the calcium acetate to the magnesium acetate thereof is 2:1:1-2:1.2:0.8; the calcium acetate and the magnesium acetate solution are added into the adsorbent respectively; and the solution is oscillated on an oscillator at room temperature, and is stirred and oscillated continuously, and is filtered after standing; the capsule core is dispersed into the capsule wall solution, and is slowly dripped into the polyethylene glycol solution in stirring to prepare the snow ice melt inhibiting material to be doped into the asphalt pavement filling material after stirring, vacuum filtering, cleaning and drying.
Description
Technical field
The present invention relates to slowly-releasing ice-melt snow material and preparation method and application, relate in particular to a kind of press down ice-melt snow material and preparation method and application, relate to specifically and a kind ofly build the road or build the shell mould of wrapping up in of mixing in the bituminous pavement stopping composition on the road surface and press down ice-melt snow material and preparation method and application.
Technical background
Recent two decades comes owing to Global warming, and environmental pollution is serious, and the cold and hot difference variation of winter climate is unusual, and freezing is alternately frequent, and road surface and ice and snow layer are freezed, and causes many drivings to knock into the back.Snow freezes, freezing, the important land main lines of communication such as city, motorway, airport are obstructed, traffic stop transport the serious threat people daily life, influenced development and national economy.In recent years in winter, interruption of communication also appears in some areas, China south, and motorway is closed.The city all will sprinkle kiloton oxonium salt class Snow Agent to the road surface throwing every year.The agent of ice-melt snow is not laid in part city, south, uses the Industrial Salt snow melt.Northern China and more domestic city major applications sodium-chlor, magnesium chloride are the agent of ice-melt snow, environment is polluted the source, soil becomes the saltings after being mixed by the salt frozen water, the trees flowers and plants in large quantities of roadsides die, a large amount of salt Snow Agent flow into river, river, lake, sea with water after the snow melt, cause severe contamination.
Japan, North America, some countries of Europe have researched and developed other type ice-melt snow agent, and come into operation.The U.S. is with thermal source ice-melt snow, and this project investment is big, can't widespread use, can only use on short-range road such as airport in some low humidity ramps relatively.Also adopted the heating cable thermal source that anti-skidding measure is implemented in above-mentioned highway section on the ramp of underground parking, China Beijing, effect is fine, but lays with to use cost too high, per hour current consumption 160-300 kilowatt on one square metre of road surface.
CN10392040C, CN125067C, CN1657586A have announced ice-melt snow agent and preparation and application.Mainly utilizing the waste wood chaff vinegar liquid that produces in the furfural production process, mainly is the C based on acetic acid
1～3Small molecules organic carboxyl acid or acetate waste liquid are produced its calcium acetate magnesium salt (CMA); Wherein, energy expenditure is big when organic acid is purified.
Summary of the invention
The objective of the invention is to overcome the problem that prior art exists, providing a kind of builds the road or builds the shell mould of wrapping up in of mixing in the bituminous pavement stopping composition on the road surface and press down ice-melt snow material and preparation method, with freezing between slowly-releasing inhibition ice and snow and the road surface, ice and snow can come off when vehicle operating voluntarily, avoid or reduce the traffic accident that causes because of ice and snow road, be easy to mechanical removal ice and snow; After preventing ice dissolution, a large amount of ice-melt snow-broths pour in well under the both sides, road surface and overflow, and ponding is darker below the bridge, has a strong impact on vehicle and travels.
The technical scheme that realizes the object of the invention is: a kind ofly build the road or build the shell mould of wrapping up in of mixing in the bituminous pavement stopping composition on the road surface and press down ice-melt snow material, be made up of shell wall, shell core and protection solution polyoxyethylene glycol; Described shell wall is a chitosan; Shell core is by sorbent material bentonite in powder after 30 microns process absorption calcium acetates, the magnesium acetate modification or silicon bath soil powder, mixes formation with aggregate hydrophobic nano silicon-dioxide or hydrophobic nano calcining calcium; Chitosan and polyoxyethylene glycol mass ratio are 1: 1; 30 microns; Silicon bath soil after bentonite in powder after 30 microns modifications or the 30 microns modifications, with the quality sum of hydrophobic nano silicon-dioxide or hydrophobic nano calcining calcium, with the chitosan mass ratio be 10: 1; Bentonite in powder after the described modification or silicon bath soil powder, the ratio of calcining the quality of calcium with hydrophobic nano silicon-dioxide or hydrophobic nano is 7: 3; Bentonite in powder after the modification or the soil of the silicon bath after modification powder are 2: 1: 1～2: 1.2: 0.8 with calcium acetate wherein, the mass ratio of magnesium acetate; Bentonite in powder after the modification or the silicon bath after modification soil powder is 1: 1 with the ratio of the quality sum of wherein calcium acetate, magnesium acetate.
A kind ofly build the road or build the shell mould of wrapping up in of mixing in the bituminous pavement stopping composition on the road surface and press down ice-melt snow preparation methods, form by following steps:
(1) preparation method of modified adsorbent wilkinite or modified adsorbent silicon bath soil: in the silicon bath soil of the bentonite in powder of 30 microns in sorbent material or 30 microns, add snow melt magnesium acetate solution, calcium acetate solution respectively, place on the vibrator under 25 ℃ and vibrate, the control stirring velocity is 200r/min, continuous oscillation 24h, static 8h after-filtration; Wherein, the silicon bath of 30 microns bentonite in powder or 30 microns soil is 2: 1: 1～2: 1.2 with the mass ratio of calcium acetate, magnesium acetate: 0.8t, and the concentration of calcium acetate, magnesium acetate solution is respectively 10mg/L～20mg/L; Silicon bath soil is 1 with the ratio of the quality sum of wherein calcium acetate, magnesium acetate after bentonite in powder after the modification or the modification: 1t; Total concentration of metal ions qe 〉=50mg/L in the balanced solution;
(2) press down the preparation that material is avenged in ice-melt:
Sorbent material silicon bath soil powder is calcined the mixed shell core of calcium with aggregate hydrophobic nano silicon-dioxide or hydrophobic nano after the sorbent material bentonite in powder of the modification that above-mentioned steps (1) is obtained or the modification, being distributed to every liter of ethyl acetate solution contains in the shell wall solution of 10～20g chitosan, under the stirring velocity of 600～800r/min, slowly it is dropped to contain and contain in every premium on currency solution in 10～20g polyoxyethylene glycol protection solution, after mixing back restir 3min, vacuumize and make the ethyl acetate volatilization, filter, washing, in baking oven, be dried to water content less than 8% under 50 ℃, obtain microgranular microcapsule slowly-releasing and press down ice-melt snow material; Wherein, the mass ratio of the sorbent material bentonite in powder of modification or silicon bath soil powder and aggregate hydrophobic nano silicon-dioxide or hydrophobic nano calcining calcium aggregate is 7: 3, and the two mixes back quality sum is 10 weight parts; Mass ratio between shell wall chitosan and the polyoxyethylene glycol is 1: 1; Described shell core is 10: 1 with the ratio of shell wall quality; The bentonite in powder of modification or silicon bath soil powder and hydrophobic nano silicon-dioxide or hydrophobic nano calcining calcium mass ratio are 7: 3.
A kind ofly build the road or build the shell mould of wrapping up in of mixing in the bituminous pavement stopping composition on the road surface and press down ice-melt snow material, form by shell wall, shell core and protection solution polyoxyethylene glycol; Described shell wall is an ethyl cellulose; Shell core is by sorbent material bentonite in powder after 30 microns process absorption calcium acetates, the magnesium acetate modification or silicon bath soil powder, mixes formation with aggregate hydrophobic nano silicon-dioxide or hydrophobic nano calcining calcium; Ethyl cellulose and polyoxyethylene glycol mass ratio are 2: 5～1: 2; Silicon bath soil after bentonite in powder after 30 microns modifications or the 30 microns modifications, with the quality sum of hydrophobic nano silicon-dioxide or hydrophobic nano calcining calcium be 10: 1 with the chitosan mass ratio; Bentonite in powder after the described modification or silicon bath soil powder are 7: 3 with the ratio of the quality of hydrophobic nano silicon-dioxide or hydrophobic nano calcining calcium; Bentonite in powder after the modification or the soil of the silicon bath after modification powder are 2: 1: 1～2: 1.2: 0.8 with calcium acetate wherein, the mass ratio of magnesium acetate; Bentonite in powder after the modification or the silicon bath after modification soil powder is 1: 1 with the ratio of the quality sum of wherein calcium acetate, magnesium acetate.
A kind ofly build the road or build the shell mould of wrapping up in of mixing in the bituminous pavement stopping composition on the road surface and press down ice-melt snow preparation methods, form by following steps:
(1) preparation method of modified adsorbent wilkinite or modified adsorbent silicon bath soil: in the silicon bath soil of the bentonite in powder of 30 microns in sorbent material or 30 microns, add snow melt magnesium acetate solution, calcium acetate solution respectively, place on the vibrator under 25 ℃ and vibrate, the control stirring velocity is 200r/min, continuous oscillation 24h, static 8h after-filtration; Wherein, the silicon bath of 30 microns bentonite in powder or 30 microns soil is 2: 1: 1～2: 1.2: 0.8 with the mass ratio of calcium acetate, magnesium acetate, and the concentration of calcium acetate, magnesium acetate solution is respectively 10mg/L～20mg/L; Silicon bath soil is 1: 1 with calcium acetate wherein, the ratio of magnesium acetate quality sum after bentonite in powder after the modification or the modification; Total concentration of metal ions qe 〉=50mg/L in the balanced solution;
(2) press down the preparation that material is avenged in ice-melt:
Sorbent material silicon bath soil powder is calcined the mixed shell core of calcium with aggregate hydrophobic nano silicon-dioxide or hydrophobic nano after the sorbent material bentonite in powder of the modification that above-mentioned steps (1) is obtained or the modification, being distributed to every liter of ethyl acetate solution contains in the shell wall solution of ethyl cellulose of 4～10g, under the stirring velocity of 600～800r/min, slowly it is dropped to contain and contain in every premium on currency solution in 10～20g polyoxyethylene glycol protection solution, after mixing back restir 3min, vacuumize and make the ethyl acetate volatilization, filter, washing, in baking oven, be dried to water content less than 8% under 50 ℃, obtain microgranular microcapsule slowly-releasing and press down ice-melt snow material; Wherein, the mass ratio of the sorbent material bentonite in powder of modification or silicon bath soil powder and aggregate hydrophobic nano silicon-dioxide or hydrophobic nano calcining calcium aggregate is 7: 3, and the two mixes back quality sum is 10 weight parts; Mass ratio between ethyl cellulose and the polyoxyethylene glycol is 2: 5～1: 2; Described shell core is 10: 1 with the ratio of shell wall quality; The bentonite in powder of modification or silicon bath soil powder and hydrophobic nano silicon-dioxide or hydrophobic nano calcining calcium mass ratio are 7: 3.
A kind ofly build the road or build the road surface and mix the application that shell mould presses down ice-melt snow material of wrapping up in the bituminous pavement stopping composition, will wrap up in shell mould and press down ice-melt snow material and mix 3～6kg/m in the bituminous pavement stopping composition
2
The above-mentioned shell mould of wrapping up in presses down ice-melt snow material, and its shell is to be the white particles shape in light yellow, the shell, and its fineness is 30 microns, mix in the bituminous pavement stopping composition, when supercrust when its surface layer freezes or snows in the winter time the time, calcium ions and magnesium ions slowly releases, and slowly-releasing presses down ice-melt snow.Thereby be convenient to the machinery deicing that clears the snow, in case behind the stagnant ice snow melt, a large amount of icy waters pour in well under the both sides, road surface and overflow, and have a strong impact on traffic.This wraps up in shell mould but ice-melt snow material is about five, six years time of releasing.
Chitosan has another name called poly-glucosamine, and soluble chitin or chitosan are the deacetylated products of chitin, is a kind of polymer straight chain type polysaccharide.Formal name used at school is β (1,4)-2-amino-2-deoxy-D-glucose.Its structure is as follows:
Because deacetylated reaction has destroyed the regularity of chitin molecule structure, therefore, its solubility property is greatly improved than chitin, and chemical property is also comparatively active.Chitosan is water insoluble, alkali and organic solution, is dissolved in dilute acid solns such as formic acid, acetate, lactic acid, hydrochloric acid and phenylformic acid, can generate salt.During general the use, use this class diluted acid chitosan solution more.This solution is positively charged.
Chitosan is a kind of reproducible energy and industrial raw materials, output is only second to Mierocrystalline cellulose, the annual biosynthetic chitosan of nature is 10,000,000,000 tons according to estimates, considerably beyond other glycosaminoglycan, being one of organism the abundantest on the earth, also is one of natural resource that were not fully utilized in 20th century.At present the raw materials for production of chitosan are mainly from the waste of seafood processing industry.These wastes as agricultural waste, also are not fully utilized previously at present.Lake, China inland river, the marine site is big, and the crustacean resource is very abundant, is example with Guangdong, Zhejiang two provinces, and annual depleted shrimp, crab shell are all more than ten million ton, and this is the important source that produces chitosan.
The parcel principle: the chitosan surface has free hydroxyl group and amino, has certain complexing action with calcium ions and magnesium ions, form the nucleocapsid package structure easily, the wilkinite surface can absorbing calcium ions and magnesium ions, hydrophobic nano grade silicon dioxide specific surface is than higher, be adsorbed onto the wilkinite surface easily, wilkinite is wrapped up by chitosan simultaneously, forms microcapsule.And chitosan is macromolecular compound, has certain toughness, has the ability of opposing deformation under the effect of external force.But lack intensity during as roadbed material, played good reinforced effects by adding high strength aggregate hydrophobic nano-silica.
The present invention compares with technology is arranged, and has outstanding substantive distinguishing features and obvious improvement and positive effect:
(1) the present invention is a kind of builds the road or builds the road surface and mix the shell mould of wrapping up in of bituminous pavement stopping composition and press down ice-melt snow material, is made up of shell wall, shell core and protection solution polyoxyethylene glycol; Described shell wall is chitosan or ethyl cellulose, and shell core is to be made of bentonite in powder or native the mixing with aggregate hydrophobic nano-silica or aggregate hydrophobic nano calcining calcium of silicon bath through the micron after absorption calcium acetate, the magnesium acetate modification.
(2) the above-mentioned shell mould of wrapping up in presses down ice-melt snow material, when supercrust when its surface layer freezes or snows in the winter time the time, calcium ions and magnesium ions slowly releases, suppressed to combine between ice and snow and the supercrust, slowly-releasing up to suppress ice and snow and road surface between freezing, ice and snow can come off when vehicle operating voluntarily, avoids the vehicle rear-end collision traffic accident that causes because of ice and snow road, simultaneously, be easy to mechanical removal, can reduce that driving is a chain of knocks into the back or the generation of casualty accident.And after can preventing ice dissolution, a large amount of ice-melt snow-broths pour in well under the both sides, road surface and overflow, and ponding is darker below the bridge.Having a strong impact on vehicle travels.In addition, the present invention is wrapped up in shell mould and is pressed down ice-melt snow material, mixes in the bituminous pavement stopping composition, is about five, six years time of releasing.To sloping road, the back of the body shady road surface can be by 3～6kg/m
2Apply slowly-releasing CMA.
(3) pyroligneous liquor is (based on the C of acetic acid
1～3Small molecular organic acid) decolouring: after adopting catalytic oxidation to become molecular weight to be para benzoquinone 200 or more oxidation of phenol, adopt again that membrane sepn is made with extra care, reverse osmosis concentration.Make with extra care, concentrate and compare with adopting vapor removal, have remarkable energy saving effect.
(4) the present invention utilizes abundant natural resource, as sorbent material wilkinite or silicon bath soil, aggregate hydrophobic nano silicon-dioxide or recyclings such as hydrophobic nano silicon bath soil, shell wall chitosan or ethyl cellulose, reach energy-saving and emission-reduction, recycle is to the environment non-secondary pollution.
Description of drawings
Fig. 1 is wood vinegar nanometer film separation process scheme figure of the present invention; Among the figure,
1-1,1-2-strainer 1-3-nanometer film separator 1-4 stage chamber pump
1-7,1-8,1-9-valve 1-10-circulation groove.
Fig. 2 is the process flow sheet of reverse osmosis concentration pyroligneous liquor; Among the figure
2-1-counter-osmosis device 2-2-stage chamber pump 2-3-recycle pump
2-4,2-5,2-6-valve.
Fig. 3 is the mol ratio of Ca/Mg and the graph of a relation between the ice-melt amount;
Fig. 4 is CMA of the present invention and NaCl ice-melt amount and timing relationship comparison diagram; Among the figure,
4-1-NaCl 4-2-CMA
Fig. 5 forms graduation curve figure for mineral aggregate; Among the figure,
5-1-standard upper limit 5-2-standard lower limit 5-3-production machine is joined
5-4-standard intermediate value.
Embodiment
Now, the present invention is further described as follows by the drawings and specific embodiments:
Embodiment 1: the preparation of wood vinegar, refining and concentrated
The preparation of wood vinegar: the bacterium chaffs of 500 grams are added in the retort, carry out destructive distillation in being no more than under 300 ℃ the temperature, expellant gas through the condenser cooling, is collected 145～160 gram brownish black acetum pyrolignosum crudum acid solutions, charcoal 140～150 grams respectively under 90～200 ℃.
Static 1～6 month of described crude pyroligneous acid is collected its intermediary organic phase after the layering, wherein mainly contain 7.32% acetic acid, 085% formic acid, 062% propionic acid, 0.15% formaldehyde, 0.25% furfural, 0.62% phenol.Phenol is the major cause of wood vinegar band look, therefore, and the processing of need decolouring.Crude pyroligneous acid is packed in the container, is catalyzer with copper/lithium complex metal ion, and bubbling air is in the reaction 5 hours down of 60～80 ℃ of temperature, 2.7MPa pressure, and wherein, catalyzer: the phenol mol ratio is 1: 2mol, Cu
2+: Li
2+=1: 3.It is para benzoquinone more than 200 that phenol is oxidized to molecular weight.
The filtration of wood vinegar, nanometer film separation and purification: see Fig. 1, with the above-mentioned wood vinegar after leaving standstill oxide treatment, under the effect of pump 1-9, through one-level, secondary filter 1-1, after 1-2 filters (its bottom is provided with valve 1-9), inject nanometer film separator 1-3, under the effect of stage chamber pump 1-4, the wood vinegar among the circulation groove 1-10 is entered stage chamber pump 4 through valve 6, again through valve 1-7, tensimeter 1-5 enters and has carried out the circulation separation among the nanometer film separator 1-3, and the open degree by regulated valve 1-8, make the separating pressure of nanometer film remain on 0.7～0.75MPa under the normal temperature, mainly contain molecular weight less than 100 acetic acid through the isolated wood vinegar of nanometer film separator 1-3, at the bottom of nanometer film separator 1-3, come out; All the other return through pump 1-8, and recirculation separates to the circulation groove 1-10.
Concentrating of wood vinegar: from Fig. 2 as seen, the present invention adopts reverse osmosis technology to concentrate wood vinegar.Wood vinegar after nanometer film is separated is injected circulation groove 2-3, and by valve 2-4, multistage recycle pump 2-2, through valve 2-5 the wood vinegar among the circulation groove 2-3 is pumped among the counter-osmosis device 2-1 again, by the aperture size of regulated valve 2-6, the pressure-controlling that makes counter-osmosis device is at 1.45～1.50MPa.Can remove portion water, small molecular weight material in the wood vinegar through reverse-osmosis treated.Acetic acid content reaches 20～60%wt in the wood vinegar after concentrating in the circulation groove, concentrates to finish.
The preparation of embodiment 2:CMA ice-melt snow material
The preparation of CMA (calcium acetate, magnesium salts) ice-melt snow material:
In reactor, add 200kg oxygen calcium, the oxygen magnesium of 112kg, the water of 50kg, mix and the furnishing pasty state, add the wood vinegar 150kg of 20wt% then gradually, and come control reaction temperature to be no more than 70 ℃ by the feed rate of control wood vinegar; Reacting end after remove by filter insolubles, is 30wt% through evaporation concentration to solids content, and drying just obtains solid CMA snow melt material.
Temperature is to the influence of reaction; Above-mentioned temperature of reaction is controlled at 50～70 ℃, and reaction is control easily, and through 60～100min, its product yield is higher, better performances under this temperature condition.
Reactant concn is to the influence of product yield: above-mentioned reaction belongs to liquid, solid two phase reaction, and heat release again simultaneously is even solid materials is pulverized very tinyly, also can exist local reaction excessive in the reaction process, temperature of reaction is not easy control, reacts problem such as incomplete, and product yield is low.For solving foregoing problems, the present invention has taked reaction preceding with calcium oxide, magnesium oxide and after the wood vinegar blending water is investigated into pasty state or pulpous state, again with the reaction of reaction wood vinegar, have good mobility because of reaction system this moment, storeroom can well mix, sufficient reacting, temperature of reaction is controlled easily.The mol ratio of water and wood vinegar (described water comprises the moisture that wood vinegar itself is contained) superelevation, product yield superelevation.When moisture was increased to a certain degree, product yield tended towards stability.But along with the increase of water consumption, the product concentration that makes reduces, and only by after the evaporation drying, product could crystallization, and high product cost height has consumed energy since like this.When the mol ratio of water and acetic acid was controlled at 50.8～6.2, reaction process was controlled easily, product cost yield height, and the energy consumption reduction etc.
Calcium oxide and magnesian mol ratio are to the influence of product performance; Magnesium acetate among the CMA is the effect of having immediate effect in the snow melt process, and the snow melt time is short, and magnesium salts generally will be higher than calcium salt.Calcium acetate is slow effect in the snow melt process, and the slow time of snow melt is long.Snow melt material C MA should be quick-acting and slow unification of imitating.
Relation between embodiment 3:CMA ice-melt snow material usage and the ice-melt amount
In 8 100ml porcelain crucibles, respectively go into 50ml water, and placed in-10 ℃ the thermostat container freezing 12 hours, make the identical ice cube of shape.Get the CMA Snow Agent of different mol ratio, each sample ligand is made full solution, take by weighing each sample Snow Agent 60ml then respectively, pour into one by one in the above-mentioned ice cube that makes, the total amount of metering liquid behind the 30min, it the results are shown in following table:
The CMA snow melt dosage of table 1. different mol ratio and the relation between the ice-melt amount
| CaO/MgO mol | 2/1 | 1.5/1 | 1/1 | 1.5/1 | 1/2 | 1/2.5 | 1/3 | 1/3.5 |
| Amount of snowmelt amount ml | 9.0 | 9.2 | 9.6 | 9.8 | 10.2 | 10.5 | 10.1 | 9.6 |
From last table 1, Fig. 3 as seen, the ice-melt amount changes unpredictably along with the CaO/MgO mole and changes, and when the CaO/MgO mole equaled, the ice-melt amount reached maximum,
Embodiment 4: the ice-melt time is to the influence of ice-melt amount
The water that in 14 100ml porcelain crucibles, respectively adds 50ml, and all place-10 to place in-10 ℃ the thermostat container freezing 12 hours the described porcelain crucible, CMA Snow Agent, sodium-chlor sample are made into the solution of 20wt% respectively, the 60ml that materialses respectively pours in above-mentioned 14 porcelain crucibles that fill ice cube one by one, measure 5,15,25,35,45,55 simultaneously respectively, each sample circulation ice (ice-melt amount ml) during 65min, see the following form, scheme?
The relation of table 2. ice-melt amount (ml) and ice-melt time (min)
| The ice- |
5 | 15 | 25 | 35 | 45 | 55 | 65 |
| CMA NaCl | 0.8 1.1 | 2.8 3.7 | 6.3 7.2 | 11.2 13.9 | 16.5 17.8 | 23.8 26.3 | 25.7 31.5 |
Can see NaCl and CMA ice-melt amount and ice-melt time relation from last table 2, Fig. 4.
Embodiment 5: the preparation of slowly-releasing CMA (calcium magnesium acetate) microcapsule
The present invention is a sorbent material with the wilkinite, is aggregate with the hydrophobic nano-silica, and preparation slowly-releasing CMA presses down ice-melt snow material.
(1) density of adsorbents adsorb balance time absorption calcium acetate, magnesium: accurately take by weighing 30 microns the bentonite in powder of (10 ± 0.0005) g or silicon dried soil powder sample of sorbent in 250ml tool plug Erlenmeyer flask, the calcium acetate standardized solution 100ml that adds mass concentration 100mg/L, each mass concentration point all is provided with 2 parallel samples. and under 25 ℃ of conditions of constant temperature, place vibrator to vibrate, rotating speed is 200r/min, continuous oscillation 24h, filter with the middling speed qualitative filter paper after leaving standstill 8h, measure Ca in the balanced solution with atomic absorption spectrophotometry
2+
Mass concentration is calculated the equilibrium adsorption density qe of sorbent material by following formula:
Qe=(C0-Ce)/W0. (1); In the formula,
Qe-be equilibrium adsorption density (the adsorbent ionic weight of every gram during balance, mg/g);
C0-is an initial mass of ion concentration (mg/L);
Ce is an equilibrium phase mass of ion concentration (mg/L);
W0-is adsorbent mass concentration (g/L).The mass concentration of all series of samples sorbent materials is W0=100g/L in this experiment.
(2) sorbent material wilkinite or silicon bath soil absorption calcium magnesium acetate (1)
Accurately take by weighing wilkinite or the silicon dried soil sample of 30 microns (10 ± 0.0005) g, place 250ml tool plug Erlenmeyer flask, the adding mass concentration is respectively calcium acetate and each 50ml of magnesium acetate standardized solution of 100mg/L, each mass concentration point all is provided with 2 parallel samples, under 25 ℃ of conditions of constant temperature, place vibrator to vibrate, rotating speed is 200r/min, continuous oscillation 24h, filter with the middling speed qualitative filter paper after leaving standstill 8h, measure total metal ion mass concentration in the balanced solution with atomic absorption spectrophotometry, calculate the equilibrium adsorption density qe. (50mg/g) of sorbent material by following formula (1).
Sorbent material wilkinite or silicon dried soil absorption calcium magnesium acetate (2)
The silicon dried soil sample that accurately takes by weighing 30 microns (10 ± 0.0005) g is in 250ml tool plug Erlenmeyer flask, the adding mass concentration is respectively calcium acetate 60ml and the magnesium acetate 40ml standardized solution of 100mg/L, each mass concentration point all is provided with 2 parallel samples. and under 25 ℃ of conditions of constant temperature, place vibrator to vibrate, rotating speed is 200r/min, continuous oscillation 24h, filter with the middling speed qualitative filter paper after leaving standstill 8h, measure total metal ion mass concentration in the balanced solution with atomic absorption spectrophotometry, the equilibrium adsorption density qe. (60mg/g) that calculates sorbent material by following formula (1) for the purpose of the present invention, qe selective value＞50mg/g.Experimental result shows that adsorption effect was best when calcium acetate and magnesium acetate mol ratio were 3: 2.
(3) one of preparation of calcium magnesium acetate microcapsule (is shell wall with the chitosan)
1. after 30 microns bentonite in powder that adsorbed calcium acetate, magnesium acetate or silicon bath soil 7g, 3g hydrophobic nano-silica powder or hydrophobic nano calcining calcium being mixed, be distributed in the shell wall solution of ethyl acetate (10%w/v: every liter of ethyl acetate solution contains the 10g chitosan) 100ml of chitosan-containing, low whipping speed is slowly it to be dropped to injector for medical purpose under the 600r/min to contain polyoxyethylene glycol (10%w/v; Contain the 10g polyoxyethylene glycol in every premium on currency solution) 100ml protection solution in; vacuumize behind the stirring 3min and make the ethyl acetate volatilization, filter washing; in baking oven, be dried to water content less than 8% under 50 ℃, promptly obtain microgranular microcapsule slowly-releasing and wrap up in shell mould and press down ice-melt snow material.
2. adsorbed calcium acetate with 30 microns; the bentonite in powder of magnesium acetate or silicon dried soil powder 7g; after 3g hydrophobic nano-silica powder powder or hydrophobic nano calcining calcium powder mix; be distributed in the 100ml solution that contains the 20g chitosan in every liter of ethyl acetate; low whipping speed is slowly it to be dropped in the 100ml protection solution that contains the 20g polyoxyethylene glycol in every premium on currency solution with injector for medical purpose under the 800r/min; vacuumize behind the churning time 5min and make the ethyl acetate volatilization; after filtration; washing; in baking oven 50 ℃ down dry water content promptly get microgranular microcapsule slowly-releasing and wrap up in shell mould and press down ice-melt and avenge material less than 8%.
(4) two of the preparation of calcium magnesium acetate microcapsule (are shell wall with the ethyl cellulose)
1. with 30 microns bentonite in powder or silicon bath soil 7g and 3g hydrophobic nano-silica powder or hydrophobic nano silicon dried soils that adsorbed calcium acetate, magnesium acetate, be distributed to after the mixing contain ethyl cellulose the shell wall solution of ethyl acetate (4%w/v:1 rises ethyl acetate solution and contains the 4g ethyl cellulose) 100ml in, low whipping speed be under the 600r/min with injector for medical purpose slowly it is dropped to contain polyoxyethylene glycol (10%, w/v; Contain the 10g polyoxyethylene glycol in the 1 premium on currency solution) 100ml protection solution in; vacuumize behind the stirring 3min and make the ethyl acetate volatilization, filter washing; in baking oven, be dried to water content less than 8% under 50 ℃, promptly obtain particulate microcapsule slowly-releasing and wrap up in shell mould and press down ice-melt snow material.
2. adsorbed calcium acetate with 30 microns; the bentonite in powder of magnesium acetate or silicon dried soil powder 7g; after 3g hydrophobic nano-silica powder powder or hydrophobic nano calcining calcium powder mix; being distributed to every w/v:1 rises in the 100ml solution that ethyl acetate solution contains the 10g ethyl cellulose; low whipping speed is slowly it to be dropped in the 100ml protection solution that contains the 20g polyoxyethylene glycol in every premium on currency solution with injector for medical purpose under the 800r/min; vacuumize behind the churning time 5min and make the ethyl acetate volatilization; after filtration; washing; dry water content is wrapped up in shell mould ice-melt snow material less than 8% but promptly get microgranular microcapsule slowly-releasing under 50 ℃ in baking oven.
(4) mensuration of microcapsule product embedding rate
Take by weighing the microcapsule of 1g, the ethanol that adds 5ml95%, grinding several minutes makes the wall material dissolve broken wall fully, the distilled water that adds 10ml again, stirring makes calcium acetate magnesium salt soluble in water fully, filters with funnel, clean filter residue several times repeatedly with distillation moisture again, collect filtrate, be settled to 100ml, the filtrate that accurately pipettes behind the 10ml constant volume is used the EDTA titration.
The embedding rate of micro encapsulation (%)=(the core content in the product)/(the core content that adds suspension) * 100.
Table 3. ability that thaws ice and snow:
| Sample number into spectrum | The quality (g) of ice | Add Snow Agent (g) | Envrionment temperature (℃) | Melt aquifer yield (ml) |
| 1 | 50 | 30 | -10 | 41 |
| 2 | 50 | 30 | -20 | 29 |
| 3 | 50 | 30 | -30 | 15 |
The performance of slowly-releasing CMA: slowly-releasing CMA has a hydrophobic nature, because summer, road bitumen was waited until softening the expansion, porosity is reduced, and causes slowly-releasing CMA to be coated in the road, and slowly-releasing CMA has hydrophobic nature simultaneously, therefore, can not run off with rainwater; Strengthen because of the road porosity winter, less than 4%; Part slowly-releasing CMA comes out, and brings into play its slow releasing function.Road surface has portion C MA and disengages, and up to suppressing freezing between ice and snow and the road surface, ice and snow can come off when vehicle operating voluntarily, avoids the traffic accident that causes because of ice and snow road, is easy to removing during artificial or mechanism's snow removing.
Embodiment 6: press down ice-melt snow road surfacing production mix proportion (Jilin Area)
The technological standard that adopts
1, " asphalt highway construction technique normalizing " (JTG F40-2004)
2, " highway engineering gather materials testing regulation " (JTG E42-2005);
3, " highway engineering pitch and asphalt testing regulation " (JTJ052-2000);
The compound standard
1, category of roads: motorway;
2, traffic grade: heavily loaded traffic;
3, project organization layer position: upper layer;
4, road use properties climatic region: summer sweltering heat-Dong cold (1-3) district;
Target Mixture Ratio
1, mineral aggregate cooperates ratio
Table 4. mineral aggregate cooperates ratio
| The specification of gathering materials (mm) | 19～9.5 | 9.5～4.75 | 4.75～2.36 | Mechanism sand | Slowly-releasing CMA |
| The cooperation ratio | 34 | 21.5 | 15 | 26 | 3.5 |
2, best bitumen aggregate ratio: 4.5%.
Production mix proportion
1, mineral aggregate cooperates ratio
Pitch adopts Shaanxi state wound SBS modifying asphalt.It is qualified that the every index of starting material detects.The pitch batching plant adopts inlet side Ning Hefu 4000 type batching plants, and is every functional.
Table 5. mineral aggregate cooperates ratio
| The specification of gathering materials (mm) | 19～9.5 | 9.5～4.75 | 4.75～2.36 | Mechanism sand | Slowly-releasing CMA |
| The cooperation ratio | 29 | 28 | 12 | 26 | 5 |
Table 6. mineral aggregate test-results
3, best bitumen aggregate ratio: 4.5%.
Form calculating and grating value from the visible mineral aggregate of last table 7; Fig. 5 has shown standard upper limit 5-1, standard lower limit 5-2, production grating 5-3 and standard intermediate value 5-4.
The best oilstone of table 8.Marshall method is had a competition and is tested the result
The pavement performance check: the pavement performance of the common AC-16 of high speed and the pavement performance of MMAC-16 are carried out following comparison, and bitumen aggregate ratio is 4.5%
Dynamic stability (rut) test
Touchstone: rower
Sample forming method: roller-compaction
The test conditions of standard:
Testing circumstance medium: air
Test ambient temperature: 60 ± 1 (℃)
Test period: 60 (min)
Test the speed that goes and back running: 21 (inferior/min)
Wheel load: 0.7 ± 0.05 (MPa)
Specimen size: 300 * 300 * 50 (mm)
The common AC-16 of table 9. high speed uses on the road with the MMAC-16 pavement performance and compares
| Mix type | AC-16 | MMAC-16 |
| Dynamic stability (inferior/mm) | 9114 | 12475 |
The test of immersion residual stability
The best bitumen aggregate ratio of suggestion level adapted Marshall prepares marshal piece, press the JTJ052-2000T0709 method, measures the stability behind test specimen stability and the immersion 48h respectively, calculates the residual stability that soaks, and wherein code requirement is not less than 85%, tests to the results are shown in following table.
Table 10. immersion residual stability
| Mix type | AC-16 | MMAC-16 (not adding slowly-releasing CMA) | MMAC-16 (admixture slowly-releasing CMA) | Code requirement |
| Residual stability (%) | 90.0 | 87.7 | 85.4 | 85 |
Freeze thawing splitting retained strength is than testing: suggestion level adapted optimum oil stone is than a preparation marshal piece, press the JTJ052-2000T0729 method, measure the freeze thawing and the cleavage strength of freeze thawing marshal piece not respectively, calculate the cleavage strength ratio, code requirement is not less than 80%, and test-results sees Table.
Table 11. freeze thawing split test result
| Mix type | AC-16 | MMAC-16 (not adding slowly-releasing CMA) | MMAC-16 (admixture slowly-releasing CMA) | Code requirement |
| Retained strength is than (%) | 90.0 | 64.4 | 77.7 | 80 |
Table 12. low-temperature bending test result
| Mix type | AC-16 | MMAC-16 (not adding slowly-releasing CMA) | MMAC-16 (admixture slowly-releasing CMA) | Code requirement |
| Retained strength is than (%) | 90.0 | 64.4 | 77.7 | 80 |
The test specimen that the picking meet the specifications requires is pressed JTJ052-2000 T0715 method, carries out pliability test by root, measures breaking strain.
Table 13. breaking strain result
| Mix type | AC-16 | MMAC-16 |
| Breaking strain (μ ε) | 2516 | 2424 |
Water penetration test
To carry out water penetration test by JTJ052-2000 (T0730) method through the wheel tracking test test specimen of wheel roller moulding.
Table 14. water penetration test result
| Mix type | AC-16 | MMAC-16 |
| Infiltration coefficient (ml/min) | 46 | 2424 |
Slowly-releasing CMA consumption:
Slowly-releasing CMA consumption is a benchmark with link table layer thickness 40～50mm, every square metre of 3～6kg slowly-releasing CMA that road crust applies.
Claims (5)
1. the road surface of building the road or the build shell mould of wrapping up in of mixing the bituminous pavement stopping composition presses down ice-melt snow material, is made up of shell wall, shell core and protection solution polyoxyethylene glycol; Described shell wall is a chitosan; Shell core is by sorbent material bentonite in powder after 30 microns process absorption calcium acetates, the magnesium acetate modification or silicon bath soil powder, mixes formation with aggregate hydrophobic nano silicon-dioxide or hydrophobic nano calcining calcium; Chitosan and polyoxyethylene glycol mass ratio are 1: 1, the silicon bath soil after the bentonite in powder after 30 microns modifications or the 30 microns modifications, with the mass parts sum of hydrophobic nano silicon-dioxide or hydrophobic nano calcining calcium be 10: 1 with the chitosan mass ratio; Bentonite in powder after the described modification or silicon bath soil powder are 7: 3 with the ratio of the quality of hydrophobic nano silicon-dioxide or hydrophobic nano calcining calcium; Bentonite in powder after the modification or the soil of the silicon bath after modification powder are 2: 1: 1～2: 1.2: 0.8 with calcium acetate wherein, the mass ratio of magnesium acetate; Bentonite in powder after the modification or the silicon bath after modification soil powder is 1: 1 with the ratio of the quality sum of wherein calcium acetate, magnesium acetate.
2. the road surface of building the road or the build shell mould of wrapping up in of mixing the bituminous pavement stopping composition presses down ice-melt snow preparation methods, is made up of following steps:
(1) preparation method of modified adsorbent wilkinite or modified adsorbent silicon bath soil: in the silicon bath soil of the bentonite in powder of 30 microns in sorbent material or 30 microns, add magnesium acetate solution, calcium acetate solution respectively, place on the vibrator under 25 ℃ and vibrate, the control stirring velocity is 200r/min, continuous oscillation 24h, static 8h after-filtration; Wherein, the silicon bath of 30 microns bentonite in powder or 30 microns soil is 2: 1: 1～2: 1.2: 0.8 with the mass ratio of calcium acetate, magnesium acetate, and the concentration of calcium acetate, magnesium acetate solution is respectively 10mg/L～20mg/L; Silicon bath soil is 1: 1 with the ratio of the quality sum of wherein calcium acetate, magnesium acetate after bentonite in powder after the modification or the modification; Total concentration of metal ions qe 〉=50mg/L in the balanced solution;
(2) wrap up in the preparation that shell mould presses down ice-melt snow material:
Sorbent material silicon bath soil powder after the sorbent material bentonite in powder of the modification that above-mentioned steps (1) is obtained or the modification, with aggregate hydrophobic nano silicon-dioxide or the mixed shell core of hydrophobic nano calcining calcium, being distributed to every liter of ethyl acetate solution contains in the shell wall solution of 10～20g chitosan, under the stirring velocity of 600～800r/min, slowly it is dropped to and contain in every premium on currency solution in 10～20g polyoxyethylene glycol protection solution, after mixing back restir 3min, vacuumize and make the ethyl acetate volatilization, filter, washing, in baking oven, be dried to water content less than 8% under 50 ℃, obtain microgranular microcapsule slowly-releasing and press down ice-melt snow material; Wherein, the mass ratio of the sorbent material bentonite in powder of modification or silicon bath soil powder and aggregate hydrophobic nano silicon-dioxide or hydrophobic nano calcining calcium aggregate is 7: 3t, and the two mixing quality sum is 10 weight parts; Mass ratio between chitosan and the polyoxyethylene glycol is 1: 1; Described shell core is 10: 1 with the ratio of shell wall quality; The bentonite in powder of modification or silicon bath soil powder and hydrophobic nano silicon-dioxide or hydrophobic nano calcining calcium mass ratio are 7: 3.
3. build the road or build the road surface and mix the shell mould of wrapping up in of bituminous pavement stopping composition and press down ice-melt snow material, form by shell wall, shell core and protection solution polyoxyethylene glycol; Described shell wall is an ethyl cellulose; Shell core is by sorbent material bentonite in powder after 30 microns process absorption calcium acetates, the magnesium acetate modification or silicon bath soil powder, mixes formation with aggregate hydrophobic nano silicon-dioxide or hydrophobic nano calcining calcium; Ethyl cellulose and polyoxyethylene glycol mass ratio are 2: 5～1: 2, silicon bath soil after bentonite in powder after 30 microns modifications or the 30 microns modifications, with the mass parts sum of hydrophobic nano silicon-dioxide or hydrophobic nano calcining calcium be 10: 1 weight parts with chitosan matter deal ratio; Bentonite in powder after the described modification or silicon bath soil powder, the ratio of calcining the quality of calcium with hydrophobic nano silicon-dioxide or hydrophobic nano is: 7: 3; Bentonite in powder after the modification or the soil of the silicon bath after modification powder are 2: 1: 1～2: 1.2: 0.8 with calcium acetate wherein, the mass ratio of magnesium acetate; Bentonite in powder after the modification or the silicon bath after modification soil powder is 1: 1 with the ratio of the quality sum of wherein calcium acetate, magnesium acetate.
4. build the road or build the road surface and mix the shell mould of wrapping up in of bituminous pavement stopping composition and press down ice-melt snow preparation methods, form by following steps:
(1) preparation method of modified adsorbent wilkinite or modified adsorbent silicon bath soil: in the silicon bath soil of the bentonite in powder of 30 microns in sorbent material or 30 microns, add magnesium acetate solution, calcium acetate solution that snow melt is used respectively, place on the vibrator under 25 ℃ and vibrate, the control stirring velocity is 200r/min, continuous oscillation 24h, static 8h after-filtration; Wherein, the silicon bath of 30 microns bentonite in powder or 30 microns soil is 2: 1: 1～2: 1.2: 0.8 with the mass ratio of calcium acetate, magnesium acetate, and the concentration of calcium acetate, magnesium acetate solution is respectively 10mg/L～20mg/L; Silicon bath soil is 1: 1 with the ratio of the mass parts sum of wherein calcium acetate, magnesium acetate after bentonite in powder after the modification or the modification; Total concentration of metal ions qe 〉=50mg/L in the balanced solution;
(2) wrap up in the preparation that shell mould presses down ice-melt snow material:
Sorbent material silicon bath soil powder is calcined the mixed shell core of calcium with aggregate hydrophobic nano silicon-dioxide or hydrophobic nano after the sorbent material bentonite in powder of the modification that above-mentioned steps (1) is obtained or the modification, being distributed to every liter of ethyl acetate solution contains in the solution of ethyl cellulose of 4～10g, under the stirring velocity of 600～800r/min, slowly it is dropped to contain and contain in every premium on currency solution in 10～20g polyoxyethylene glycol protection solution, after mixing back restir 3min, vacuumize and make the ethyl acetate volatilization, filter, washing, in baking oven, be dried to water content less than 8% under 50 ℃, obtain microgranular microcapsule slowly-releasing and press down ice-melt snow material; Wherein, the mass ratio of the sorbent material bentonite in powder of modification or silicon bath soil powder and aggregate hydrophobic nano silicon-dioxide or hydrophobic nano calcining calcium aggregate is 7: 3, and the two mixing quality sum is 10 weight parts; Mass ratio between ethyl cellulose and the polyoxyethylene glycol is 2: 5～1: 2; Described shell core is 10: 1 with the ratio of shell wall quality; The bentonite in powder of modification or silicon bath soil powder and hydrophobic nano silicon-dioxide or hydrophobic nano calcining calcium mass ratio are 7: 3.
5. build the road or build the application that shell mould presses down ice-melt snow material of wrapping up in that the bituminous pavement stopping composition is mixed on the road surface, will press down ice-melt snow material and mix every square metre of 3～6kg in the bituminous pavement stopping composition.
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