CN104231642B - Pitch crack autogenous healing microcapsules containing regenerative agent and preparation method thereof - Google Patents
Pitch crack autogenous healing microcapsules containing regenerative agent and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of pitch crack autogenous healing microcapsules containing regenerative agent and preparation method thereof, it includes uramit resin 4.5g～5.5g, bitumen regenerant 5～7g, surfactant 0.9～2.5g, defoamer 0.1～0.2ml, ammonium chloride 0.5～0.7g, resorcinol 0.5～0.7g, surplus is water；Wherein urea in uramit resin: the mol ratio of formaldehyde is 1:1.3～1.6；The present invention with uramit resin for wall material, bitumen regenerant as core, add proper quantity of defoaming agent, curing agent and chain extender etc. to be modified as modifying agent, after mixing asphalt system, being obviously improved of pitch fatigue behaviour can be realized without extra heating or other trigger conditions, and the microcapsule stability of the present invention is good, can improve the ductility of pitch, the preparation method of the present invention is simple, low cost of manufacture, is suitable to popularization and application on a large scale.
Description
Technical field
The invention belongs to pitch crack autogenous healing microcapsules studying technological domain, be specifically related to a kind of containing regeneration
Pitch crack autogenous healing microcapsules of agent and preparation method thereof.
Background technology
Microcapsules are that development now rapidly and is widely used in the necks such as weaving, medicine, aviation, solar energy and building
The technology in territory, but application in pitch and promoting still in research and development.
Along with the surge increasingly of the volume of traffic, the pressure that road faces is increasing, and bituminous concrete makes at complicated
With under environment, inevasible there will be small cracking and local damage, if these diseases can not be repaiied in time
Multiple, then can affect normal usage energy and the service life of bituminous paving.Accordingly, it would be desirable to research and development one can be led
Dynamic crackle bituminous paving occur and damage carry out perception the technology repaired, and are recovering asphalt concrete material
The service life of bituminous paving is extended while intensity.Introduce the concept of biological selfreparing, supplement as hand with material
Section, utilizes microcapsules technology be coated with by regenerative agent and be added in pitch.When microcrack extends at microcapsules,
Effect microcapsule wall will be caused to rupture, and the regenerative agent of outflow not only improves the character of pitch at crack, promotes simultaneously
At crack, pitch at room temperature or realize good self-healing characteristics under lower temperature, thus can play and delay to split
The effect in crack is repaired in the extension of seam the most completely, extends the fatigue life of bituminous paving.
At present, main recovery technique has doughnut carrying to repair liquid method, silicon hydrogen repairing method etc..In although
Hollow fiber carrying reparation liquid method is high without extra extraneous trigger condition and repair rate, but after repairing at glass tube
Forming cavity, can affect concrete performance, and manufacturing process technology requires strict, cost is high, due to caliber
Limiting regenerative agent amount of storage, make repair rate limited, itself belongs to rigid material in addition, behind road surface easily
Ruptured before not acting on, it is difficult to reach preferable repairing effect.Silicon hydrogen repairing method is repaired carrying of monomer
Pure more complicated with isolation technics, it mainly uses additional substance to fill out crack, the most fundamentally solves crack
Problem, and the platinum catalyst price that the method uses is higher, is unsatisfactory for the requirement of engineering economy.
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 without outward
Add trigger condition can realize pitch crack selfreparing, improve pitch self-reparing capability containing regenerative agent
Pitch crack autogenous healing microcapsules.
Present invention also offers the preparation method of a kind of above-mentioned pitch crack autogenous healing microcapsules containing regenerative agent.
To achieve these goals, the technical solution adopted in the present invention is:
Should containing pitch crack autogenous healing microcapsules of regenerative agent be include in the microcapsule solution of 300mL with
The raw material of lower proportioning:
Wherein urea in uramit resin: the mol ratio of formaldehyde is 1:1.3～1.6；
Above-mentioned surfactant is neopelex, APES (OP-10), dodecane
In base sodium sulphate and POLYSORBATE 80 any one；
Above-mentioned defoamer is n-octyl alcohol or normal 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:
A kind of method preparing the above-mentioned pitch crack autogenous healing microcapsules containing regenerative agent, it is by following step
Rapid composition:
(1) formaldehyde, urea are joined in there-necked flask according to the amount that mol ratio is 1.3～1.6:1, use deionization
Water is completely dissolved, and forms ureaformaldehyde solution, molten with the NaOH solution regulation ureaformaldehyde that concentration is 0.01mol/L
Liquid pH to 8～9, reacts 60～75min at 60～75 DEG C, prepares uramit resin prepolymer；
(2) measure bitumen regenerant add deionized water to being completely dissolved, add surfactant, emulsify 15～20min；
(3) according to above-mentioned quality proportioning, in the bitumen regenerant emulsified, add what step (1) prepared
Uramit resin prepolymer and defoamer, ammonium chloride and resorcinol, be the hydrochloric acid of 0.01mol/L by concentration
Regulation pH value of solution is 2～4, warming-in-water to 55～65 DEG C stirring 2～3h, obtains microcapsule suspensions；
(4) microcapsule suspensions is naturally cooled to room temperature, filter by conventional method, wash, be dried prepared containing
There are the pitch crack autogenous healing microcapsules of regenerative agent.
A kind of pitch crack autogenous healing microcapsules containing regenerative agent that the present invention provides and preparation method thereof, this is micro-
Capsule its be as core with uramit resin for wall material, bitumen regenerant, and add proper quantity of defoaming agent, solidification
Agent and chain extender etc. are modified as modifying agent, after mixing asphalt system, it is not necessary to additionally heat or other touch
Clockwork spring part can realize being obviously improved of pitch fatigue behaviour, can be remarkably reinforced the self-reparing capability of pitch, and
Pitch self performance will not be reduced, and the microcapsule stability of the present invention is good, pitch Crack failure wall material, from
And bitumen regenerant is discharged, penetrate into and pitch carries out asphalt-regenerating, improve the ductility of pitch, the present invention
Preparation method is simple, low cost of manufacture, be suitable to popularization and application on a large scale.
Accompanying drawing explanation
Fig. 1 is the Microcapsules Size distribution histogram of embodiment 1 preparation.
Detailed description of the invention
In conjunction with embodiment and experiment, technical scheme is further described, but the present invention is not only
It is limited to following enforcement situation.
Embodiment 1
As a example by the pitch crack autogenous healing microcapsules containing regenerative agent preparing 300mL, it is by following proportioning
Raw material forms:
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, urea is 1:1.4 with the mol ratio of formaldehyde.
The sulfonated phenylethylene maleic anhydride multipolymer of the present embodiment, monomer mole ratio is 45:55, and number is divided equally
Son amount is 1.2 × 105, 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, its block ratio for 3:7,
Its number-average molecular weight is 5.5 × 104Belong to commercially available prod.
The heavy mineral oil of the present embodiment is to carry in oil tower base oil after atmospheric tower distills and decompression component
The base oil produced.
The raw material of above-mentioned mass distribution ratio is prepared according to conventional fabrication process the bitumen regenerant of the present embodiment.
The above-mentioned pitch crack autogenous healing microcapsules containing regenerative agent are prepared by following methods:
(1) 5.79g formaldehyde is weighed with 2.86g urea according to urea: the mol ratio of formaldehyde is that the amount of 1:1.4 joins
There-necked flask is completely dissolved by deionized water, forms ureaformaldehyde solution, then be the NaOH of 0.01mol/L by concentration
Solution regulation ureaformaldehyde pH value of solution is to 8, under 65 DEG C of water bath condition, and at the uniform velocity stirring ureaformaldehyde solution reaction
65min, prepares uramit resin prepolymer；
(2) bitumen regenerant measuring 6g is placed in beaker, and addition deionized water, to being completely dissolved, adds 1.5g
Neopelex as surfactant, clipped mulser, emulsify 18min, obtain emulsified asphalt again
Raw agent；
(3) uramit resin prepolymer 5g step (1) prepared and normal octane 0.15mL, chlorination
Ammonium 0.6g and resorcinol 0.6g adds in emulsified asphalt regenerative agent prepared by step (2), is 0.01mol/L by concentration
Hydrochloric acid conditioning solution pH be 3, warming-in-water to 60 DEG C stirring 2.5h, obtain microcapsule suspensions；
(4) microcapsule suspensions is naturally cooled to room temperature, filter by conventional method, wash, be dried, prepare
300mL contains the pitch crack autogenous healing microcapsules of regenerative agent.
The characteristic of the pitch crack autogenous healing microcapsules containing regenerative agent prepared by the present embodiment is analyzed,
Specific as follows:
(1) the particle diameter test of microcapsules
Take effective microcapsule granule sample number 392, according to conventional Microcapsules Size test experience to its particle diameter
Detecting, detected Microcapsules Size distribution situation is as shown in Figure 1.
As shown in Figure 1, Microcapsules Size is concentrated mainly between 5um to 30um, and these part microcapsules account for always
The 73.0% of body, the average grain diameter of microcapsules is 21.14um.From the point of view of obtained Microcapsules Size distribution situation,
Illustrate that, in microcapsules preparation process, whole reaction system is relatively stable, and emulsion system is the most relatively stable, reaction
During there is not demulsifying phenomenon, thus prepare the regenerative agent microcapsules that particle diameter is less and distribution is concentrated.
(2) the capsule-core content of microcapsules and clad ratio
By above-mentioned prepared microcapsules in suction filtration is placed on stainless steel pallet, it is placed in vacuum drying chamber drying
To constant weight, through accurate weighing after taking-up, weight is 5.861g.It is fully ground, is being used acetone soak 72h,
For making capsule-core be fully dissolved out, need to need to change an acetone soln every 24h in immersion process, finally filter third
Ketone solution i.e. can get Lauxite cyst wall, is fully dried by cyst wall and weighs, and the cyst wall quality obtained is 1.614g.
Calculating capsule-core quality, can calculate capsule-core content, formula is as follows:
Cyst wall quality according to obtaining can calculate capsule-core quality, can calculate microcapsule coated rate, and formula is as follows:
Recording the microcapsules capsule-core content prepared by the present embodiment through test is 72.46%, and the clad ratio of microcapsules is
84.94%.
Embodiment 2
As a example by the pitch crack autogenous healing microcapsules containing regenerative agent preparing 300mL, it is by following proportioning
Raw material forms:
The bitumen regenerant of above-mentioned 5.3g is made up of the raw material of following proportion by weight:
The raw material of above-mentioned mass distribution ratio is prepared according to conventional fabrication process the bitumen regenerant of the present embodiment.
The preparation method of the above-mentioned pitch crack autogenous healing microcapsules containing regenerative agent is same as in Example 1.
Recording the microcapsules capsule-core content prepared by the present embodiment through test is 70.16%, and the clad ratio of microcapsules is
82.36%.
Embodiment 3
As a example by the pitch crack autogenous healing microcapsules containing regenerative agent preparing 300mL, it is by following proportioning
Raw material forms:
The bitumen regenerant of above-mentioned 6.7g is made up of the raw material of following proportion by weight:
The raw material of above-mentioned mass distribution ratio is prepared according to conventional fabrication process the bitumen regenerant of the present embodiment.
The preparation method of the above-mentioned pitch crack autogenous healing microcapsules containing regenerative agent is same as in Example 1.
Recording the microcapsules capsule-core content prepared by the present embodiment through test is 68.20%, and the clad ratio of microcapsules is
80.33%.
Embodiment 4
As a example by the pitch crack autogenous healing microcapsules containing regenerative agent preparing 300mL, it is by following proportioning
Raw material forms:
The bitumen regenerant of above-mentioned 5g is made up of the raw material of following proportion by weight:
The raw material of above-mentioned mass distribution ratio is prepared according to conventional fabrication process the bitumen regenerant of the present embodiment.
The preparation method of the above-mentioned pitch crack autogenous healing microcapsules containing regenerative agent is same as in Example 1.
Recording the microcapsules capsule-core content prepared by the present embodiment through test is 65.42%, and the clad ratio of microcapsules is
79.98%.
Embodiment 5
As a example by the pitch crack autogenous healing microcapsules containing regenerative agent preparing 300mL, it is by following proportioning
Raw material forms:
The bitumen regenerant of above-mentioned 7g is made up of the raw material of following proportion by weight:
The raw material of above-mentioned mass distribution ratio is prepared according to conventional fabrication process the bitumen regenerant of the present embodiment.
The preparation method of the above-mentioned pitch crack autogenous healing microcapsules containing regenerative agent is same as in Example 1.
Recording the microcapsules capsule-core content prepared by the present embodiment through test is 72.10%, and the clad ratio of microcapsules is
81.20%.
Embodiment 6
In the preparation method of the pitch crack autogenous healing microcapsules containing regenerative agent of above-described embodiment 1～5, step
(1) weigh formaldehyde and urea according to urea: the mol ratio of formaldehyde be the amount of 1:1.3 join there-necked flask spends from
Sub-water is completely dissolved, and forms ureaformaldehyde solution, then regulates urea first by the NaOH solution that concentration is 0.01mol/L
Aldehyde pH value of solution is to 9, and under 60 DEG C of water bath condition, at the uniform velocity stirring ureaformaldehyde solution reaction 75min, prepares polyureas
Formaldehyde resin performed polymer；
(2) measuring bitumen regenerant to be placed in beaker, addition deionized water, to being completely dissolved, adds dodecyl
Benzene sulfonic acid sodium salt as surfactant, clipped mulser, emulsify 15min, obtain emulsified asphalt regenerative agent；
(3) uramit resin prepolymer step (1) prepared and normal octane, ammonium chloride and isophthalic two
Phenol adds in emulsified asphalt regenerative agent prepared by step (2), is the hydrochloric acid conditioning solution of 0.01mol/L by concentration
PH is 2, warming-in-water to 55 DEG C stirring 3h, obtains microcapsule suspensions；
(4) microcapsule suspensions is naturally cooled to room temperature, filter by conventional method, wash, be dried, prepare
300mL contains the pitch crack autogenous healing microcapsules of regenerative agent.
Other all identical with corresponding embodiment.
Embodiment 7
In the preparation method of the pitch crack autogenous healing microcapsules containing regenerative agent of above-described embodiment 1～5, step
(1) weigh formaldehyde and urea according to urea: the mol ratio of formaldehyde be the amount of 1:1.6 join there-necked flask spends from
Sub-water is completely dissolved, and forms ureaformaldehyde solution, then regulates urea first by the NaOH solution that concentration is 0.01mol/L
Aldehyde pH value of solution is to 9, and under 75 DEG C of water bath condition, at the uniform velocity stirring ureaformaldehyde solution reaction 60min, prepares polyureas
Formaldehyde resin performed polymer；
(2) measuring bitumen regenerant to be placed in beaker, addition deionized water, to being completely dissolved, adds dodecyl
Benzene sulfonic acid sodium salt as surfactant, clipped mulser, emulsify 20min, obtain emulsified asphalt regenerative agent；
(3) uramit resin prepolymer step (1) prepared and normal octane, ammonium chloride and isophthalic two
Phenol adds in emulsified asphalt regenerative agent prepared by step (2), is the hydrochloric acid conditioning solution of 0.01mol/L by concentration
PH is 4, warming-in-water to 65 DEG C stirring 2h, obtains microcapsule suspensions；
(4) microcapsule suspensions is naturally cooled to room temperature, filter by conventional method, wash, be dried, prepare
300mL contains the pitch crack autogenous healing microcapsules of regenerative agent.
Other all identical with corresponding embodiment.
Embodiment 8
In above-described embodiment 1～7, surfactant used can with the APES (OP-10) of equivalent,
Lauryl sodium sulfate and POLYSORBATE 80 are replaced, and other raw material and proportioning are identical with corresponding embodiment.
The preparation method of microcapsules is identical with corresponding embodiment.
Embodiment 9
In above-described embodiment 1～7, defoamer normal octane used can be replaced with the n-octyl alcohol of equivalent, other
Raw material and proportioning are identical with corresponding embodiment.
The preparation method of microcapsules is identical with corresponding embodiment.
Analyze according to the microcapsules characteristic test of above-described embodiment 1, the micro-glue prepared by the embodiment of the present invention 8～9
The characteristic of capsule is close with the testing result of embodiment 1 respectively.
In order to verify beneficial effects of the present invention, by matrix pitch as a comparison case, by prepared by embodiment 1
Pitch crack autogenous healing microcapsules containing regenerative agent add respectively according to the volume of 0.1wt%, 0.3wt%, 0.5wt%
Enter in the matrix pitch of equivalent, carry out bitumen ductility test and DSR tests, specific as follows:
(1) self-healing ductility test
According to T0605-2011 " bitumen ductility test " matrix pitch and microcapsules volume be respectively 0.1wt%,
The pitch of 0.3wt%, 0.5wt% detects, the ductility healing rate of its correspondence respectively: 24.97%, 21.31%,
38.65% and 39.45%.
Therefore deducing that, the less self-reparing capability to pitch of microcapsules volume promotes inconspicuous, along with micro-glue
The increase of capsule volume, the healing rate of pitch also can increase therewith, but when volume increases to 0.5wt%, pitch
Healing rate increasing degree diminishes, hence it is evident that asphaltic nature also will not be greatly reduced while promoting pitch self-reparing capability.
(2) self-healing DSR test
Above-mentioned matrix pitch and microcapsules volume are respectively the pitch of 0.1wt%, 0.3wt%, 0.5wt% respectively
Carry out DSR test, the following Tables 1 and 2 of result；
The first tired DSR result of the test of table 1
Using the 60% of each group of pitch introductory die value as test cut off, from table 1 it follows that four groups of drips
Blue or green modulus time difference used when dropping to initial modulus 60% differs greatly, the matrix pitch that decrease speed is the fastest,
Only time-consuming 509s drops down to G* 60, damage rate is maximum, D0 healing stage=13333.53Pa/s, its excess-three group by
Little to being greatly D respectively1<D2<D3；In first fatigue test, the phase angle mean value of matrix pitch
δMean value=58.85, its excess-three cell mean is respectively 60.17,59.80,60.02；By comparing, admixture
The asphaltic nature having microcapsules there occurs change, under the effect of regenerative agent, makes asphaltic nature be more biased towards in flexibility.
Table 2 heals-tired DSR result of the test again
In analytical table 2, data understand: through the healing of 0.5h, matrix pitch and the modulus of first group of sample pitch
Recovery value relatively, respectively 2MPa and 1.9MPa；Second group is recovered with the modulus of the 3rd group of sample pitch
Value is relatively big, respectively 3.3MPa and 3.6MPa, and the modulus recovery value of the 3rd group of pitch is maximum；Four groups of pitches
Damage rate is followed successively by from small to large: D3<D1<D2<DMatrix pitch；They are loaded onto the time of destruction and are respectively as follows:
tMatrix pitch=342s, t1=335s, t2=340s and t3=449s, the time lengthening 27.56% destroyed than matrix pitch opposing,
Can be seen that regenerative agent microcapsules volume is the sample pitch self-healing energy of 0.5wt% after the healing of 0.5h
Power is optimal.
Comprehensively reaching a conclusion, along with the increase of microcapsules volume, pitch is gradually reduced, reviews one's lessons by oneself reactivation fatigue life
Power strengthens, and volume is that the sample pitch self-reparing capability of 0.5wt% is the strongest.
Proving further described above by experiment, the microcapsules prepared by embodiment 2～9 prolong in self-healing
Degree test, self-healing DSR test all can reach above-mentioned experiment effect.
Claims (4)
1. the pitch crack autogenous healing microcapsules containing regenerative agent, it is characterised in that: micro-at 300mL
Capsule solution includes the raw material of following proportioning:
Wherein urea in uramit resin: the mol ratio of formaldehyde is 1:1.3～1.6；
Above-mentioned surfactant is neopelex, APES, lauryl sodium sulfate
And in Tween 80 any one；
Above-mentioned defoamer is n-octyl alcohol or normal octane；
Above-mentioned bitumen regenerant is made up of the raw material of following proportion by weight:
Pitch crack autogenous healing microcapsules containing regenerative agent the most according to claim 1, it is characterised in that:
The raw material of following proportioning is included in the microcapsule solution of 300mL:
Pitch crack autogenous healing microcapsules containing regenerative agent the most according to claim 1, it is characterised in that:
Described bitumen regenerant is made up of the raw material of following proportion by weight:
4. the micro-glue of pitch crack autogenous healing containing regenerative agent prepared described in any one of claims 1 to 3
The method of capsule, it is to comprise the steps of:
(1) formaldehyde, urea are joined in there-necked flask according to the amount that mol ratio is 1.3～1.6:1, use deionization
Water is completely dissolved, and forms ureaformaldehyde solution, molten with the NaOH solution regulation ureaformaldehyde that concentration is 0.01mol/L
Liquid pH to 8～9, reacts 60～75min at 60～75 DEG C, prepares uramit resin prepolymer；
(2) measure bitumen regenerant add deionized water to being completely dissolved, add surfactant, emulsify 15～20min；
(3) according to above-mentioned quality proportioning, in the bitumen regenerant emulsified, add what step (1) prepared
Uramit resin prepolymer and defoamer, ammonium chloride and resorcinol, be the hydrochloric acid of 0.01mol/L by concentration
Regulation pH value of solution is 2～4, warming-in-water to 55～65 DEG C stirring 2～3h, obtains microcapsule suspensions；
(4) microcapsule suspensions is naturally cooled to room temperature, filter by conventional method, wash, be dried prepared containing
There are the pitch crack autogenous healing microcapsules of regenerative agent.
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