CN104231642A - Pitch crack self-repair microcapsule containing regenerating agent and preparation method thereof - Google Patents
Pitch crack self-repair microcapsule containing regenerating agent and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a pitch crack self-repair microcapsule containing a regenerating agent and a preparation method thereof. The self-repair microcapsule comprises 4.5-5.5 g of polyurea formaldehyde resin, 5-7 g of a pitch regenerating agent, 0.9-2.5 g of a surface active agent, 0.1-0.2 ml of a defoaming agent, 0.5-0.7 g of ammonium chloride, 0.5-0.7 g of resorcinol, and the balance of water, wherein the molar ratio of carbamide to formaldehyde in the polyurea formaldehyde resin is 1:(1.3-1.6). The self-repair microcapsule disclosed by the invention uses the polyurea formaldehyde resin as a wall material and uses the pitch regenerating agent as a core material, an appropriate amount of a defoaming agent, a curing agent, chain extender and the like are added to be used as a modifier for modification, and after an pitch system is mixed, the fatigue performance of pitch can be obviously improved without additional heating or other trigger conditions; in addition, the microcapsule disclosed by the invention has good stability, and the ductility of the pitch can be improved. The preparation method disclosed by the invention is simple, the manufacturing cost is low, and the microcapsule and the preparation method are suitable for extensive promotion and application.
Description
Technical field
The invention belongs to pitch crack autogenous healing microcapsule studying technological domain, be specifically related to a kind of pitch crack autogenous healing microcapsule containing regenerator and preparation method thereof.
Background technology
Microcapsule develop swift and violent now and are widely used in the technology in the fields such as weaving, medicine, aviation, sun power and building, but application in pitch and popularization are still in research and development.
Along with the surge increasingly of the volume of traffic, the increasing pressure that road faces is large, and bituminous concrete, under the environment for use of complexity, inevasiblely there will be small cracking and local damage, if these diseases can not be timely repaired, then can affect normal usage energy and the work-ing life of bituminous pavement.Therefore, need to research and develop a kind of crackle that can initiatively occur bituminous pavement and damage carry out perception and the technology of repairing, while recovering asphalt concrete material intensity, extend the work-ing life of bituminous pavement.Introduce the concept of biological selfreparing, supplement as means with material, utilize microcapsulary that regenerator is coated and be added in pitch.When microfracture extends to microcapsule place, effect microcapsule wall will be caused to break, flow out regenerator not only improve crack place pitch character, impel crack place pitch at room temperature or under lesser temps can realize good self-healing characteristics simultaneously, thus play the effect that crack is repaired in the expansion delaying crack even completely, extend the fatigue lifetime of bituminous pavement.
At present, main recovery technique has tubular fibre to carry repair liquid method, silicon hydrogen repairing method etc.Although tubular fibre carrying repair liquid method is without the need to extra extraneous trigger condition and repair rate is high, but Glass tubing place forms cavity after repairing, concrete performance can be affected, and manufacturing process technology requires strict, cost is high, due to caliber restriction regenerator store content, make repair rate limited, in addition itself belongs to rigid material, for easily rupturing before not acting on behind road surface, is difficult to reach desirable repairing effect.Purification and the isolation technique of repairing monomer in silicon hydrogen repairing method are more complicated, and it mainly adopts additional substance to fill out crack, does not fundamentally solve crack problem, and the platinum catalyst price that the method uses is higher, does not meet the requirement of engineering economics.
Summary of the invention
In order to overcome the deficiency existing for the recovery technique of existing pitch crack, the invention provides a kind of pitch crack autogenous healing microcapsule containing regenerator that can realize the selfreparing in pitch crack, the self-reparing capability of raising pitch without the need to additional trigger condition.
Present invention also offers a kind of preparation method of the above-mentioned pitch crack autogenous healing microcapsule containing regenerator.
To achieve these goals, the technical solution adopted in the present invention is:
Should the pitch crack autogenous healing microcapsule containing regenerator be the raw materials including following proportioning in the microcapsule solution of 300mL:
Wherein urea in uramit resin: the mol ratio of formaldehyde is 1:1.3 ~ 1.6;
Above-mentioned tensio-active agent be in Sodium dodecylbenzene sulfonate, alkylphenol polyoxyethylene (OP-10), sodium lauryl sulphate and POLYSORBATE 80 any one;
Above-mentioned defoamer is n-Octanol or octane.
The raw material of preferred following proportioning in the microcapsule solution of 300mL:
Above-mentioned bitumen regenerant can be made up of the raw material of following proportion by weight:
The raw material composition of the preferred following proportion by weight of above-mentioned bitumen regenerant:
Prepare a method for the above-mentioned pitch crack autogenous healing microcapsule containing regenerator, it is made up of following steps:
(1) amount being 1.3 ~ 1.6:1 by formaldehyde, urea according to mol ratio joins in there-necked flask, dissolve completely with deionized water, form urea formaldehyde solution, urea formaldehyde pH value of solution to 8 ~ 9 are regulated by the NaOH solution that concentration is 0.01mol/L, 60 ~ 75min is reacted, obtained uramit resin prepolymer at 60 ~ 75 DEG C;
(2) measure bitumen regenerant and add deionized water to dissolving completely, add tensio-active agent, emulsification 15 ~ 20min;
(3) according to above-mentioned quality proportioning, the obtained uramit resin prepolymer of step (1) and defoamer, ammonium chloride and Resorcinol is added in the bitumen regenerant of emulsification, be 2 ~ 4 with the hydrochloric acid conditioning solution pH that concentration is 0.01mol/L, 2 ~ 3h is stirred in warming-in-water to 55 ~ 65 DEG C, obtains microcapsule suspensions;
(4) microcapsule suspensions is naturally cooled to room temperature, with ordinary method filtration, washing, the dry obtained pitch crack autogenous healing microcapsule containing regenerator.
A kind of pitch crack autogenous healing microcapsule containing regenerator provided by the invention and preparation method thereof, these microcapsule its be for wall material with uramit resin, bitumen regenerant is core, and add proper quantity of defoaming agent, solidifying agent and chainextender etc. carry out modification as properties-correcting agent, after mixing asphalt system, without the need to additionally heating or other trigger conditions can realize the obvious improvement of pitch fatigue property, obviously can strengthen the self-reparing capability of pitch, and pitch self performance can not be reduced, and microcapsule stability of the present invention is good, pitch Crack failure wall material, thus bitumen regenerant is discharged, infiltrate in pitch and carry out asphalt-regenerating, improve the ductility of pitch, preparation method of the present invention is simple, low cost of manufacture, be suitable for applying on a large scale.
Accompanying drawing explanation
Fig. 1 is Microcapsules Size distribution histogram prepared by embodiment 1.
Embodiment
Now with experiment, technical scheme of the present invention is further described, but the present invention is not limited only to following enforcement situation in conjunction with the embodiments.
Embodiment 1
To prepare the pitch crack autogenous healing microcapsule containing regenerator of 300mL, it is made up of the raw material of following proportioning:
The bitumen regenerant of above-mentioned 6g is made up of the raw material of following proportion by weight:
In the uramit resin of the present embodiment, the mol ratio of urea and formaldehyde is 1:1.4.
The sulfonated phenylethylene maleic anhydride copolymer of the present embodiment, monomer mole ratio is 45:55, and number-average molecular weight is 1.2 × 10
5, molecular weight distribution is 4.3, and it belongs to commercially available prod.
The styrene butadiene styrene triblock copolymer of the present embodiment is called for short SBS, and its inlay character is 3:7, and its number-average molecular weight is 5.5 × 10
4belong to commercially available prod.
The heavy mineral oil of the present embodiment is the base oil extract in oil at the bottom of the tower of oil after atmospheric tower distillation and decompression component.
By the raw material of above-mentioned mass distribution ratio conveniently preparation technology obtain the bitumen regenerant of the present embodiment.
The above-mentioned pitch crack autogenous healing microcapsule containing regenerator are obtained by following methods:
(1) 5.79g formaldehyde and 2.86g urea is weighed according to urea: the mol ratio of formaldehyde is that the amount of 1:1.4 joins in there-necked flask and dissolves completely with deionized water, form urea formaldehyde solution, urea formaldehyde pH value of solution to 8 is regulated again by the NaOH solution that concentration is 0.01mol/L, under 65 DEG C of water bath condition, at the uniform velocity stir urea formaldehyde solution reaction 65min, obtained uramit resin prepolymer;
(2) bitumen regenerant measuring 6g is placed in beaker, and add deionized water to dissolving completely, add 1.5g Sodium dodecylbenzene sulfonate as tensio-active agent, through emulsification pretreatment machine, emulsification 18min, obtains emulsified bitumen regenerator;
(3) uramit resin prepolymer 5g obtained for step (1) and octane 0.15mL, ammonium chloride 0.6g and Resorcinol 0.6g are added in emulsified bitumen regenerator prepared by step (2), be 3 with the hydrochloric acid conditioning solution pH that concentration is 0.01mol/L, warming-in-water to 60 DEG C stirs 2.5h, obtains microcapsule suspensions;
(4) microcapsule suspensions is naturally cooled to room temperature, with ordinary method filtration, washing, drying, obtained 300mL contains the pitch crack autogenous healing microcapsule of regenerator.
The characteristic of the pitch crack autogenous healing microcapsule containing regenerator prepared by the present embodiment is analyzed, specific as follows:
(1) the particle diameter test of microcapsule
Get effective microcapsule granule sample number 392, Microcapsules Size test experience conveniently detects its particle diameter, detect Microcapsules Size distribution situation as shown in Figure 1.
As shown in Figure 1, Microcapsules Size mainly concentrates between 5um to 30um, and these part microcapsule account for overall 73.0%, and the median size of microcapsule is 21.14um.From obtained Microcapsules Size distribution situation, illustrate that, in microcapsule preparation process, whole reaction system is comparatively stable, emulsion system is also comparatively stable, demulsifying phenomenon is not there is in reaction process, thus the regenerator microcapsule that the less and distribution of obtained particle diameter is concentrated.
(2) the capsule-core content of microcapsule and clad ratio
Be placed in stainless steel pallet through suction filtration by above-mentioned obtained microcapsule, be placed in vacuum drying oven and dry to constant weight, through accurate weighing after taking-up, weight is 5.861g.It is fully ground, is soaking 72h with acetone, for making the abundant stripping of capsule-core, an acetone soln need need be changed every 24h in immersion process, last filter acetone solution can obtain urea-formaldehyde resin cyst wall, and cyst wall is fully dry and weigh, and the cyst wall quality obtained is 1.614g.
Calculate capsule-core quality, can calculate capsule-core content, formula is as follows:
Cyst wall quality according to obtaining can calculate capsule-core quality, and can calculate microcapsule coated rate, formula is as follows:
Through test the microcapsule capsule-core content recorded prepared by the present embodiment be 72.46%, the clad ratio of microcapsule is 84.94%.
Embodiment 2
To prepare the pitch crack autogenous healing microcapsule containing regenerator of 300mL, it is made up of the raw material of following proportioning:
The bitumen regenerant of above-mentioned 5.3g is made up of the raw material of following proportion by weight:
By the raw material of above-mentioned mass distribution ratio conveniently preparation technology obtain the bitumen regenerant of the present embodiment.
The preparation method of the above-mentioned pitch crack autogenous healing microcapsule containing regenerator is identical with embodiment 1.
Through test the microcapsule capsule-core content recorded prepared by the present embodiment be 70.16%, the clad ratio of microcapsule is 82.36%.
Embodiment 3
To prepare the pitch crack autogenous healing microcapsule containing regenerator of 300mL, it is made up of the raw material of following proportioning:
The bitumen regenerant of above-mentioned 6.7g is made up of the raw material of following proportion by weight:
By the raw material of above-mentioned mass distribution ratio conveniently preparation technology obtain the bitumen regenerant of the present embodiment.
The preparation method of the above-mentioned pitch crack autogenous healing microcapsule containing regenerator is identical with embodiment 1.
Through test the microcapsule capsule-core content recorded prepared by the present embodiment be 68.20%, the clad ratio of microcapsule is 80.33%.
Embodiment 4
To prepare the pitch crack autogenous healing microcapsule containing regenerator of 300mL, it is made up of the raw material of following proportioning:
The bitumen regenerant of above-mentioned 5g is made up of the raw material of following proportion by weight:
By the raw material of above-mentioned mass distribution ratio conveniently preparation technology obtain the bitumen regenerant of the present embodiment.
The preparation method of the above-mentioned pitch crack autogenous healing microcapsule containing regenerator is identical with embodiment 1.
Through test the microcapsule capsule-core content recorded prepared by the present embodiment be 65.42%, the clad ratio of microcapsule is 79.98%.
Embodiment 5
To prepare the pitch crack autogenous healing microcapsule containing regenerator of 300mL, it is made up of the raw material of following proportioning:
The bitumen regenerant of above-mentioned 7g is made up of the raw material of following proportion by weight:
By the raw material of above-mentioned mass distribution ratio conveniently preparation technology obtain the bitumen regenerant of the present embodiment.
The preparation method of the above-mentioned pitch crack autogenous healing microcapsule containing regenerator is identical with embodiment 1.
Through test the microcapsule capsule-core content recorded prepared by the present embodiment be 72.10%, the clad ratio of microcapsule is 81.20%.
Embodiment 6
In the preparation method of the pitch crack autogenous healing microcapsule containing regenerator of above-described embodiment 1 ~ 5, step (1) weighs formaldehyde and urea according to urea: the mol ratio of formaldehyde is that the amount of 1:1.3 joins in there-necked flask and dissolves completely with deionized water, form urea formaldehyde solution, urea formaldehyde pH value of solution to 9 is regulated again by the NaOH solution that concentration is 0.01mol/L, under 60 DEG C of water bath condition, at the uniform velocity stir urea formaldehyde solution reaction 75min, obtained uramit resin prepolymer;
(2) measure bitumen regenerant and be placed in beaker, add deionized water to dissolving completely, add Sodium dodecylbenzene sulfonate as tensio-active agent, through emulsification pretreatment machine, emulsification 15min, obtains emulsified bitumen regenerator;
(3) uramit resin prepolymer obtained for step (1) and octane, ammonium chloride and Resorcinol are added in emulsified bitumen regenerator prepared by step (2), be 2 with the hydrochloric acid conditioning solution pH that concentration is 0.01mol/L, warming-in-water to 55 DEG C stirs 3h, obtains microcapsule suspensions;
(4) microcapsule suspensions is naturally cooled to room temperature, with ordinary method filtration, washing, drying, obtained 300mL contains the pitch crack autogenous healing microcapsule of regenerator.
Other all identical with corresponding embodiment.
Embodiment 7
In the preparation method of the pitch crack autogenous healing microcapsule containing regenerator of above-described embodiment 1 ~ 5, step (1) weighs formaldehyde and urea according to urea: the mol ratio of formaldehyde is that the amount of 1:1.6 joins in there-necked flask and dissolves completely with deionized water, form urea formaldehyde solution, urea formaldehyde pH value of solution to 9 is regulated again by the NaOH solution that concentration is 0.01mol/L, under 75 DEG C of water bath condition, at the uniform velocity stir urea formaldehyde solution reaction 60min, obtained uramit resin prepolymer;
(2) measure bitumen regenerant and be placed in beaker, add deionized water to dissolving completely, add Sodium dodecylbenzene sulfonate as tensio-active agent, through emulsification pretreatment machine, emulsification 20min, obtains emulsified bitumen regenerator;
(3) uramit resin prepolymer obtained for step (1) and octane, ammonium chloride and Resorcinol are added in emulsified bitumen regenerator prepared by step (2), be 4 with the hydrochloric acid conditioning solution pH that concentration is 0.01mol/L, warming-in-water to 65 DEG C stirs 2h, obtains microcapsule suspensions;
(4) microcapsule suspensions is naturally cooled to room temperature, with ordinary method filtration, washing, drying, obtained 300mL contains the pitch crack autogenous healing microcapsule of regenerator.
Other all identical with corresponding embodiment.
Embodiment 8
In above-described embodiment 1 ~ 7, tensio-active agent used can be replaced with the alkylphenol polyoxyethylene of equivalent (OP-10), sodium lauryl sulphate and POLYSORBATE 80, other raw material and proportioning identical with corresponding embodiment.
The preparation method of microcapsule is identical with corresponding embodiment.
Embodiment 9
In above-described embodiment 1 ~ 7, defoamer octane used can be replaced with the n-Octanol of equivalent, other raw material and proportioning identical with corresponding embodiment.
The preparation method of microcapsule is identical with corresponding embodiment.
Analyze according to the microcapsule characteristic test of above-described embodiment 1, the characteristic of the microcapsule prepared by the embodiment of the present invention 8 ~ 9 is close with the detected result of embodiment 1 respectively.
In order to verify beneficial effect of the present invention, by matrix pitch as a comparison case, the pitch crack autogenous healing microcapsule containing regenerator prepared by embodiment 1 are added in the matrix pitch of equivalent respectively according to the volume of 0.1wt%, 0.3wt%, 0.5wt%, carry out bitumen ductility test and DSR test, specific as follows:
(1) self-healing ductility test
According to T0605-2011 " bitumen ductility test ", the pitch that matrix pitch and microcapsule volume are respectively 0.1wt%, 0.3wt%, 0.5wt% is detected, the ductility healing rate of its correspondence respectively: 24.97%, 21.31%, 38.65% and 39.45%.
Can draw thus, the less self-reparing capability to pitch of microcapsule volume promotes not obvious, along with the increase of microcapsule volume, the healing rate of pitch also can increase thereupon, but when volume is increased to 0.5wt%, the healing rate increasing degree of pitch diminishes, and also significantly can not reduce asphaltic nature while obviously promoting pitch self-reparing capability.
(2) self-healing DSR tests
The pitch that above-mentioned matrix pitch and microcapsule volume are respectively 0.1wt%, 0.3wt%, 0.5wt% is carried out DSR test respectively, and result is as following table 1 and table 2;
The first tired DSR test-results of table 1
Using 60% of each group of pitch introductory die value as test cut-out point, as can be seen from Table 1, when four groups of asphalt modulus drop to initial modulus 60%, the time difference used differs greatly, and the matrix pitch that lowering speed is the fastest, only 509s consuming time just drops to G
* 60, damage rate is maximum, D
0 healing stage=13333.53Pa/s, the ascending of its excess-three group is D respectively
1<D
2<D
3; In first fatigue test, the phasing degree mean value δ of matrix pitch
mean value=58.85, its excess-three cell mean is respectively 60.17,59.80,60.02; By more known, admixture has the asphaltic nature of microcapsule to there occurs change, under the effect of regenerator, makes asphaltic nature more be partial to flexibility.
Table 2 heals-tired DSR test-results again
In analytical table 2, data are known: through the healing of 0.5h, and the modulus recovery value of matrix pitch and first group of sample pitch relatively, is respectively 2MPa and 1.9MPa; Second group comparatively large with the modulus recovery value of the 3rd group of sample pitch, and be respectively 3.3MPa and 3.6MPa, the modulus recovery value of the 3rd group of pitch is maximum; The damage rate of four groups of pitches is followed successively by from small to large: D
3<D
1<D
2<D
matrix pitch; The time that they are loaded on destruction is respectively: t
matrix pitch=342s, t
1=335s, t
2=340s and t
3=449s, resists the time lengthening destroyed 27.56%, can find out after the healing of 0.5h than matrix pitch, regenerator microcapsule volume is that the sample pitch self-healing capability of 0.5wt% is best.
Comprehensively reach a conclusion, along with the increase of microcapsule volume, pitch reduces fatigue lifetime gradually, and self-reparing capability strengthens, and volume is that the sample pitch self-reparing capability of 0.5wt% is the strongest.
Prove further described above by experiment, the microcapsule prepared by embodiment 2 ~ 9 all can reach above-mentioned experiment effect at self-healing ductility test, self-healing DSR in testing.
Claims (5)
1. the pitch crack autogenous healing microcapsule containing regenerator, is characterized in that: the raw material including following proportioning in the microcapsule solution of 300mL:
Wherein urea in uramit resin: the mol ratio of formaldehyde is 1:1.3 ~ 1.6;
Above-mentioned tensio-active agent be in Sodium dodecylbenzene sulfonate, alkylphenol polyoxyethylene (OP-10), sodium lauryl sulphate and POLYSORBATE 80 any one;
Above-mentioned defoamer is n-Octanol or octane.
2. the pitch crack autogenous healing microcapsule containing regenerator according to claim 1, is characterized in that: the raw material including following proportioning in the microcapsule solution of 300mL:
3. the pitch crack autogenous healing microcapsule containing regenerator according to claim 2, is characterized in that: described bitumen regenerant is made up of the raw material of following proportion by weight:
4. the pitch crack autogenous healing microcapsule containing regenerator according to claim 1, is characterized in that: described bitumen regenerant is made up of the raw material of following proportion by weight:
5. prepare a method for the pitch crack autogenous healing microcapsule containing regenerator described in any one of Claims 1 to 4, it is made up of following steps:
(1) amount being 1.3 ~ 1.6:1 by formaldehyde, urea according to mol ratio joins in there-necked flask, dissolve completely with deionized water, form urea formaldehyde solution, urea formaldehyde pH value of solution to 8 ~ 9 are regulated by the NaOH solution that concentration is 0.01mol/L, 60 ~ 75min is reacted, obtained uramit resin prepolymer at 60 ~ 75 DEG C;
(2) measure bitumen regenerant and add deionized water to dissolving completely, add tensio-active agent, emulsification 15 ~ 20min;
(3) according to above-mentioned quality proportioning, the obtained uramit resin prepolymer of step (1) and defoamer, ammonium chloride and Resorcinol is added in the bitumen regenerant of emulsification, be 2 ~ 4 with the hydrochloric acid conditioning solution pH that concentration is 0.01mol/L, 2 ~ 3h is stirred in warming-in-water to 55 ~ 65 DEG C, obtains microcapsule suspensions;
(4) microcapsule suspensions is naturally cooled to room temperature, with ordinary method filtration, washing, the dry obtained pitch crack autogenous healing microcapsule containing regenerator.
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