CN108395720A - A kind of preparation method of expansion pitch - Google Patents
A kind of preparation method of expansion pitch Download PDFInfo
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- CN108395720A CN108395720A CN201810137273.9A CN201810137273A CN108395720A CN 108395720 A CN108395720 A CN 108395720A CN 201810137273 A CN201810137273 A CN 201810137273A CN 108395720 A CN108395720 A CN 108395720A
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- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
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- C08J2203/18—Binary blends of expanding agents
- C08J2203/184—Binary blends of expanding agents of chemical foaming agent and physical blowing agent, e.g. azodicarbonamide and fluorocarbon
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Abstract
The invention discloses a kind of preparation methods of expansion pitch, belong to paving field of material technology.The present invention is first by function additive, sodium silicate solution, water and pitch the particle insulation reaction under lower temperature, then after heating, thermal insulation foaming is cooled to room temperature, adds isocyanates, continues to be stirred to react to get expansion pitch；Wherein function additive is to be mixed by self-control emulsified dispersed liquid, polyethyleneimine and crosslinking agent, and in mixed process, carbon dioxide is constantly passed through into system；And emulsified dispersed liquid is made of starch octenyl succinate anhydride, enzymolysis chitosan, water and linoleic acid.Expansion pitch prepared by technical solution of the present invention is with excellent mechanical property, foam stabilizing time lengthening, the characteristics of making product adhesion strength effectively be promoted.
Description
Technical field
The invention discloses a kind of preparation methods of expansion pitch, belong to paving field of material technology.
Background technology
Asphalt material rise in price and for the high-quality reduction gathered materials promote road agency carry out road surface salvage material again
Raw research and application.Pavement recycling can be divided into cold renewal and hot recycling, this 2 kinds of methods respectively have plantmix's construction and site operation again
Mode.In terms of energy saving and freight angle, on-the-spot cold regeneration is most suitable mode.Foamed asphalt is as road material
A kind of regenerative agent and stabilizer for expecting on-the-spot cold regeneration have the characteristics that its is protruded.In recent years, foamed asphalt causes research again
The concern of person and road agency.
Foamed asphalt is called expansion pitch, is so that its volume is expanded certain water injection heated bitumen, is formed a large amount of
Asphalt foam, process it is very short time asphalt foam rupture.This process is the physical change of pitch, and chemistry does not occur
Reaction.When foamed asphalt and aggregate contact, asphalt foam moment turns to millions of " little particle ", intersperses among fine granules
（Especially grain size is less than 0.075mm）Surface, formed and be stained with the fines joint sealing materials of a large amount of pitches, by mixing and stirring compacting, these
Fines can be filled in the gap between clammy coarse fodder and form the effect of similar mortar, and mixture is made to reach stable.Foam drips
For blueness compared with emulsified asphalt, curing time is short and does not have to emulsifier, and in addition the applicable range of foamed asphalt is very wide, therefore foam
Pitch is favored in cold regeneration construction.Compared with other stabilizers, advantage is shown as foamed asphalt：（1）Increase material
Shear strength and water stability, pellet is more flexible, endurance compared with cement punishment for this kind of mixture；（2）Foamed asphalt punishment is answered
With extensive；（3）It is energy saving, it is only necessary to which that heated asphalt gathers materials and is not required to heat and dry；（4）Resting period is considerably long（It can generally put
1~3 month）；（5）Construction is small by season and climatic effect.The shortcomings that foamed asphalt, shows as：（1）When making punishment base, compared with stone
Ash/fly ash material cost is high；（2）Plate form rubber needs continuous grading；（3）Pitch, which successfully foams, needs higher temperature
Degree（About 180 DEG C）；（4）The production of foamed asphalt needs special equipment；（5）Foam stability energy is poor, and product adhesion strength is poor, mechanical property
It can be bad.
Therefore, how to improve that conventional expanded pitch foam stability energy is poor, and product adhesion strength is poor, mechanical property is bad to be lacked
Point is that it is promoted and application, meets that industrial production demand is urgently to be resolved hurrily to ask to obtain the expansion pitch of more high combination property
Topic.
Invention content
The present invention solves the technical problem of：Poor for expansion pitch foam stability energy, product adhesion strength is poor, mechanics
The bad disadvantage of performance provides a kind of preparation method of expansion pitch.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
（1）It counts in parts by weight, takes 10~20 parts of starch octenyl succinate anhydrides successively, 8~10 parts of enzymolysis chitosans, 150~
200 parts of water, 4~6 parts of linoleic acid, after first starch octenyl succinate anhydride, enzymolysis chitosan and water are mixed, swelling, then through adding
Thermal agitation disperses, and obtains dispersion liquid, adds linoleic acid, be stirred, obtains emulsified dispersed liquid；
（2）It counts in parts by weight, takes 40~60 parts of emulsified dispersed liquids successively, 8~10 parts of polyethyleneimines, 3~8 parts of crosslinking agents,
First emulsified dispersed liquid and polyethyleneimine are stirred, and carbon dioxide is passed through during being stirred, is then added and hands over
Join agent, continues to be stirred, obtain function additive；
（3）It counts in parts by weight, 30~50 parts of function additives, 8~10 parts of sodium silicate solutions, 10~15 parts of anion is taken to gather successively
Acrylamide, 100~150 parts of water, 300~500 parts of pitch particles, 4~8 parts of isocyanates are first molten by function additive, sodium metasilicate
After liquid, water and the mixing of pitch particle, under stirring, 60~70 DEG C is warming up to 0.8~1.5 DEG C/min rate programs, is protected
After 30~45min of temperature reaction, continue to be warming up to 180~185 DEG C with 2~4 DEG C/min rate programs, 30~45min of thermal insulation foaming
Afterwards, cooled to room temperature adds isocyanates, continues to be stirred to react 10~15min, discharging is to get expansion pitch.
Step（1）The enzymolysis chitosan preparation process is：It is 1 in mass ratio by chitosan and water：10~1：15 stirrings
After mixing, swelling is stood, adds the chitosan enzyme of 0.06~0.08 times of chitosan mass, after constant temperature stirring digests, enzyme deactivation is dense
Contracting, it is dry, obtain enzymolysis chitosan.
Step（2）The crosslinking agent is the chromium nitrate solution that mass fraction is 6~8%.
Step（3）The anionic polyacrylamide is the anionic polyacrylamide that molecular weight is 600~8,000,000.
Step（3）The pitch particle preparation process is：After asphalt Freezing smashing, 60~80 mesh sieve is crossed, must be dripped
Green particle.
Step（3）The isocyanates is：Methyl diphenylene diisocyanate, dicyclohexyl methyl hydride diisocyanate or different
Any one in isophorone diisocyanate.
The beneficial effects of the invention are as follows：
（1）The present invention is by adding starch octenyl succinate anhydride, anionic polyacrylamide and enzymolysis chitosan, and with nitric acid
Chromium is crosslinking agent, in preparation process, makes the macromolecular substances such as anionic polyacrylamide and chitosan in system that part occur
Crosslinking, trivalent chromic ion cross-linking system have stronger gelling strength, and cohesive force increases between colloid after crosslinking, and the foam stabilizing time prolongs
It is long, so that product adhesion strength is effectively promoted, and cross-linking system has good viscoelasticity, viscosity can be certainly after high speed shear
It is dynamic to restore, so that product half foam life period is effectively extended；
（2）The present invention is by polyethyleneimine of the addition with primary amino group, and in preparation process, polyethyleneimine can absorb dioxy
Change carbon, to form cross-linked network structure inside system, and each component fine dispersion is fixed on polyethyleneimine formation
In cross-linked network structure, and during subsequent heat, carbon dioxide discharges again, and system pH is made to reduce, to accelerate
The hydrolytic process of sodium metasilicate, and expansion asphalt interface film on formed poly silicic acid inorganic gel network, to make interfacial film
Mechanical property is obviously improved, and improves product half foam life period, and in follow-up isocyanates adition process, isocyanates can be with body
Water reacts in system, generates carbon dioxide, and the carbon dioxide generated at this time can be combined to form crosslinked with polyethyleneimine again
System is playing foaming effect, while improving system expansion rate, the foam stability of product is being made further to be promoted.
Specific implementation mode
It is 1 in mass ratio by chitosan and water：10~1：15 mixing are poured into No. 1 beaker, and 10 are stirred with glass bar
After~15min, after under room temperature, standing 3~5h of swelling, the chitosan of 0.06~0.08 times of chitosan mass is added
No. 1 beaker is then moved into digital display and tested the speed constant temperature blender with magnetic force, is 30~35 DEG C in temperature, rotating speed is 300~500r/ by enzyme
Under the conditions of min, constant temperature stirring 45~60min of enzymolysis, under the conditions of temperature is 85~90 DEG C, after keeping the temperature 10~15min of enzyme deactivation,
Material in No. 1 beaker is transferred to Rotary Evaporators, is 75~85 DEG C in temperature, under the conditions of pressure is 500~550kPa, decompression is dense
Contract 1~2h, obtains concentrate, then concentrate is transferred in baking oven, dry to constant weight under the conditions of temperature is 105~110 DEG C, obtains
Digest chitosan；It counts in parts by weight, takes 10~20 parts of starch octenyl succinate anhydrides successively, 8~10 parts digest chitosans,
Starch octenyl succinate anhydride, enzymolysis chitosan and water are first mixed and pour into No. 2 burnings by 150~200 parts of water, 4~6 parts of linoleic acid
After being stirred 5~10min with glass bar, 3~5h is swollen under room temperature, standing, then beaker immigration digital display is tested the speed for cup
Constant temperature blender with magnetic force is 65~70 DEG C in temperature, and under the conditions of rotating speed is 800~1200r/min, heating stirring disperses 1~2h,
Dispersion liquid is obtained, then linoleic acid is added into dispersion liquid, continues to be stirred 30~45min with 300~500r/min rotating speeds, obtain newborn
Change dispersion liquid；It counts in parts by weight, takes 40~60 parts of emulsified dispersed liquids, 8~10 parts of polyethyleneimines, 3~8 parts of crosslinkings successively
The three-necked flask of belt stirrer is first added in emulsified dispersed liquid and polyethyleneimine by agent, in speed of agitator be 400~600r/min
Under the conditions of, carbon dioxide gas is passed through into three-necked flask with 100~120mL/min rates, after being continually fed into 2~3h, is stopped
It is passed through carbon dioxide gas, and crosslinking agent is added, continues to be stirred 30~45min with 400~600r/min rotating speeds, obtains function
Auxiliary agent；It counts in parts by weight, takes 30~50 parts of function additives successively, the sodium silicate solution that 8~10 parts of mass fractions are 8~10%,
10~15 parts of anionic polyacrylamide, 100~150 parts of water, 300~500 parts of pitch particles, 4~8 parts of isocyanates first will
Function additive, sodium silicate solution, water and pitch particle under the conditions of rotating speed is 600~800r/min, be stirred 30~
45min is warming up to 60~70 DEG C under stirring with 0.8~1.5 DEG C/min rate programs, and insulated and stirred reaction 30~
After 45min, continue to be warming up to 180~185 DEG C with 2~4 DEG C/min rate programs, after 30~45min of thermal insulation foaming, stop plus
Heat, and cooled to room temperature, add isocyanates, continue to be stirred to react 10~15min, and discharging obtains expansion pitch.It is described
Crosslinking agent is the chromium nitrate solution that mass fraction is 6~8%.The anionic polyacrylamide is that molecular weight is 600~8,000,000
Anionic polyacrylamide.The pitch particle preparation process is：After asphalt Freezing smashing, 60~80 mesh sieve is crossed,
Obtain pitch particle.The isocyanates is：Methyl diphenylene diisocyanate, dicyclohexyl methyl hydride diisocyanate or different Fo Er
Any one in ketone diisocyanate.
Example 1
It is 1 in mass ratio by chitosan and water：15 mixing are poured into No. 1 beaker, after being stirred 15min with glass bar, in room
Under the conditions of temperature, after standing swelling 5h, the chitosan enzyme of 0.08 times of chitosan mass is added, No. 1 beaker is then moved into digital display
Test the speed constant temperature blender with magnetic force, is 35 DEG C in temperature, under the conditions of rotating speed is 500r/min, constant temperature stirring digests 60min, then at temperature
Under the conditions of degree is 90 DEG C, after keeping the temperature enzyme deactivation 15min, material in No. 1 beaker is transferred to Rotary Evaporators, is 85 DEG C in temperature, presses
Power be 550kPa under the conditions of, be concentrated under reduced pressure 2h, obtain concentrate, then concentrate is transferred in baking oven, in temperature be 110 DEG C of conditions
Under, it is dry to constant weight, obtain enzymolysis chitosan；It counts in parts by weight, takes 20 parts of starch octenyl succinate anhydrides, 10 parts of enzymolysis successively
Starch octenyl succinate anhydride, enzymolysis chitosan and water are first mixed and pour into No. 2 burnings by chitosan, 200 parts of water, 6 parts of linoleic acid
Cup after being stirred 10min with glass bar, under room temperature, stands swelling 5h, then beaker immigration digital display is tested the speed constant temperature magnetic
Power blender is 70 DEG C in temperature, and under the conditions of rotating speed is 1200r/min, heating stirring disperses 2h, obtains dispersion liquid, then to dispersion
Linoleic acid is added in liquid, continues to be stirred 45min with 500r/min rotating speeds, obtains emulsified dispersed liquid；It counts in parts by weight, successively
Take 60 parts of emulsified dispersed liquids, 10 parts of polyethyleneimines, 8 parts of crosslinking agents that band first is added in emulsified dispersed liquid and polyethyleneimine and is stirred
The three-necked flask for mixing device is passed through dioxy into three-necked flask under the conditions of speed of agitator is 600r/min with 120mL/min rates
Change carbon gas, after being continually fed into 3h, stopping is passed through carbon dioxide gas, and crosslinking agent is added, and continuation is stirred with 600r/min rotating speeds
Mixing 45min is mixed, function additive is obtained；It counts in parts by weight, takes 50 parts of function additives, the silicon that 10 parts of mass fractions are 10% successively
Acid sodium solution, 15 parts of anionic polyacrylamide, 150 parts of water, 500 parts of pitch particles, 8 parts of isocyanates, first by function additive,
Sodium silicate solution, water and pitch particle are stirred 45min under the conditions of rotating speed is 800r/min, under stirring, with
1.5 DEG C/min rate programs are warming up to 70 DEG C, after insulated and stirred reacts 45min, and continuation is warming up to 4 DEG C/min rate programs
185 DEG C, after thermal insulation foaming 45min, stops heating, and cooled to room temperature, add isocyanates, continue to be stirred to react
15min, discharging, obtains expansion pitch.The crosslinking agent is the chromium nitrate solution that mass fraction is 8%.The anion pp acyl
Amine is the anionic polyacrylamide that molecular weight is 650~7,500,000.The pitch particle preparation process is：Asphalt is cold
After agar is broken, 80 mesh sieve is crossed, pitch particle is obtained.The isocyanates is：Methyl diphenylene diisocyanate.
Example 2
It is 1 in mass ratio by chitosan and water：15 mixing are poured into No. 1 beaker, after being stirred 15min with glass bar, in room
Under the conditions of temperature, after standing swelling 5h, the chitosan enzyme of 0.08 times of chitosan mass is added, No. 1 beaker is then moved into digital display
Test the speed constant temperature blender with magnetic force, is 35 DEG C in temperature, under the conditions of rotating speed is 500r/min, constant temperature stirring digests 60min, then at temperature
Under the conditions of degree is 90 DEG C, after keeping the temperature enzyme deactivation 15min, material in No. 1 beaker is transferred to Rotary Evaporators, is 85 DEG C in temperature, presses
Power be 550kPa under the conditions of, be concentrated under reduced pressure 2h, obtain concentrate, then concentrate is transferred in baking oven, in temperature be 110 DEG C of conditions
Under, it is dry to constant weight, obtain enzymolysis chitosan；It counts in parts by weight, takes 10 parts of enzymolysis chitosans, 200 parts of water, 6 parts of sub- oil successively
Enzymolysis chitosan and water are first mixed and pour into No. 2 beakers by acid, quiet under room temperature after being stirred 10min with glass bar
Swelling 5h is set, then beaker immigration digital display is tested the speed constant temperature blender with magnetic force, is 70 DEG C in temperature, rotating speed is 1200r/min conditions
Under, heating stirring disperses 2h, obtains dispersion liquid, then linoleic acid is added into dispersion liquid, and continuation is stirred with 500r/min rotating speeds
45min obtains emulsified dispersed liquid；It counts in parts by weight, takes 60 parts of emulsified dispersed liquids, 10 parts of polyethyleneimines, 8 parts of crosslinkings successively
The three-necked flask of belt stirrer is first added in emulsified dispersed liquid and polyethyleneimine by agent, in speed of agitator be 600r/min conditions
Under, carbon dioxide gas is passed through into three-necked flask with 120mL/min rates, after being continually fed into 3h, stopping is passed through carbon dioxide
Gas, and crosslinking agent is added, continue to be stirred 45min with 600r/min rotating speeds, obtains function additive；It counts in parts by weight, according to
Sodium silicate solution secondary to take 50 parts of function additives, that 10 parts of mass fractions are 10%, 15 parts of anionic polyacrylamide, 150 parts of water,
500 parts of pitch particles, 8 parts of isocyanates, first by function additive, sodium silicate solution, water and pitch particle in rotating speed be 800r/
Under the conditions of min, it is stirred 45min, under stirring, is warming up to 70 DEG C with 1.5 DEG C/min rate programs, insulated and stirred
After reacting 45min, continue to be warming up to 185 DEG C with 4 DEG C/min rate programs, after thermal insulation foaming 45min, stops heating, and natural
It is cooled to room temperature, adds isocyanates, continue to be stirred to react 15min, discharge, obtain expansion pitch.The crosslinking agent is quality
The chromium nitrate solution that score is 8%.The anionic polyacrylamide is the anion pp acyl that molecular weight is 650~7,500,000
Amine.The pitch particle preparation process is：After asphalt Freezing smashing, 80 mesh sieve is crossed, pitch particle is obtained.The isocyanic acid
Ester is：Methyl diphenylene diisocyanate.
Example 3
It is 1 in mass ratio by chitosan and water：15 mixing are poured into No. 1 beaker, after being stirred 15min with glass bar, in room
Under the conditions of temperature, after standing swelling 5h, the chitosan enzyme of 0.08 times of chitosan mass is added, No. 1 beaker is then moved into digital display
Test the speed constant temperature blender with magnetic force, is 35 DEG C in temperature, under the conditions of rotating speed is 500r/min, constant temperature stirring digests 60min, then at temperature
Under the conditions of degree is 90 DEG C, after keeping the temperature enzyme deactivation 15min, material in No. 1 beaker is transferred to Rotary Evaporators, is 85 DEG C in temperature, presses
Power be 550kPa under the conditions of, be concentrated under reduced pressure 2h, obtain concentrate, then concentrate is transferred in baking oven, in temperature be 110 DEG C of conditions
Under, it is dry to constant weight, obtain enzymolysis chitosan；It counts in parts by weight, takes 20 parts of starch octenyl succinate anhydrides, 10 parts of enzymolysis successively
Starch octenyl succinate anhydride, enzymolysis chitosan and water are first mixed and pour into No. 2 burnings by chitosan, 200 parts of water, 6 parts of linoleic acid
Cup after being stirred 10min with glass bar, under room temperature, stands swelling 5h, then beaker immigration digital display is tested the speed constant temperature magnetic
Power blender is 70 DEG C in temperature, and under the conditions of rotating speed is 1200r/min, heating stirring disperses 2h, obtains dispersion liquid, then to dispersion
Linoleic acid is added in liquid, continues to be stirred 45min with 500r/min rotating speeds, obtains emulsified dispersed liquid；It counts in parts by weight, successively
Take 60 parts of emulsified dispersed liquids, 10 parts of polyethyleneimines, 8 parts of crosslinking agents that band first is added in emulsified dispersed liquid and polyethyleneimine and is stirred
The three-necked flask for mixing device is passed through dioxy into three-necked flask under the conditions of speed of agitator is 600r/min with 120mL/min rates
Change carbon gas, after being continually fed into 3h, stopping is passed through carbon dioxide gas, and crosslinking agent is added, and continuation is stirred with 600r/min rotating speeds
Mixing 45min is mixed, function additive is obtained；It counts in parts by weight, takes 50 parts of function additives, the silicon that 10 parts of mass fractions are 10% successively
Acid sodium solution, 150 parts of water, 500 parts of pitch particles, 8 parts of isocyanates are first broken by function additive, sodium silicate solution, water and pitch
Expect under the conditions of rotating speed is 800r/min, be stirred 45min, under stirring, is heated up with 1.5 DEG C/min rate programs
To 70 DEG C, after insulated and stirred reacts 45min, continue to be warming up to 185 DEG C with 4 DEG C/min rate programs, after thermal insulation foaming 45min,
Stop heating, and cooled to room temperature, add isocyanates, continue to be stirred to react 15min, discharges, obtain expansion pitch.Institute
It is the chromium nitrate solution that mass fraction is 8% to state crosslinking agent.The pitch particle preparation process is：By asphalt Freezing smashing
Afterwards, 80 mesh sieve is crossed, pitch particle is obtained.The isocyanates is：Methyl diphenylene diisocyanate.
Example 4
It counts in parts by weight, takes 20 parts of starch octenyl succinate anhydrides, 200 parts of water, 6 parts of linoleic acid, first by octenyl amber successively
No. 2 beakers are poured into amber acid-starch ester and water mixing, after being stirred 10min with glass bar, under room temperature, stand swelling
5h, then beaker immigration digital display is tested the speed constant temperature blender with magnetic force, in temperature be 70 DEG C, under the conditions of rotating speed is 1200r/min, heating
It is dispersed with stirring 2h, obtains dispersion liquid, then linoleic acid is added into dispersion liquid, continues to be stirred 45min with 500r/min rotating speeds, obtain
Emulsified dispersed liquid；It counts in parts by weight, takes 60 parts of emulsified dispersed liquids successively, 10 parts of polyethyleneimines, 8 parts of crosslinking agents first will be newborn
Change dispersion liquid and the three-necked flask of belt stirrer is added in polyethyleneimine, under the conditions of speed of agitator is 600r/min, with
120mL/min rates are passed through carbon dioxide gas into three-necked flask, and after being continually fed into 3h, stopping is passed through carbon dioxide gas,
And crosslinking agent is added, continue to be stirred 45min with 600r/min rotating speeds, obtains function additive；It counts in parts by weight, takes 50 successively
Part function additive, the sodium silicate solution that 10 parts of mass fractions are 10%, 15 parts of anionic polyacrylamide, 150 parts of water, 500 parts of drips
Green particle, 8 parts of isocyanates, first by function additive, sodium silicate solution, water and pitch particle in rotating speed be 800r/min conditions
Under, it is stirred 45min, under stirring, is warming up to 70 DEG C with 1.5 DEG C/min rate programs, insulated and stirred reaction
After 45min, continue to be warming up to 185 DEG C with 4 DEG C/min rate programs, after thermal insulation foaming 45min, stops heating, and natural cooling
To room temperature, isocyanates is added, continues to be stirred to react 15min, discharges, obtains expansion pitch.The crosslinking agent is mass fraction
For 8% chromium nitrate solution.The anionic polyacrylamide is the anionic polyacrylamide that molecular weight is 650~7,500,000.
The pitch particle preparation process is：After asphalt Freezing smashing, 80 mesh sieve is crossed, pitch particle is obtained.The isocyanates
For：Methyl diphenylene diisocyanate.
Example 5
It is 1 in mass ratio by chitosan and water：15 mixing are poured into No. 1 beaker, after being stirred 15min with glass bar, in room
Under the conditions of temperature, after standing swelling 5h, the chitosan enzyme of 0.08 times of chitosan mass is added, No. 1 beaker is then moved into digital display
Test the speed constant temperature blender with magnetic force, is 35 DEG C in temperature, under the conditions of rotating speed is 500r/min, constant temperature stirring digests 60min, then at temperature
Under the conditions of degree is 90 DEG C, after keeping the temperature enzyme deactivation 15min, material in No. 1 beaker is transferred to Rotary Evaporators, is 85 DEG C in temperature, presses
Power be 550kPa under the conditions of, be concentrated under reduced pressure 2h, obtain concentrate, then concentrate is transferred in baking oven, in temperature be 110 DEG C of conditions
Under, it is dry to constant weight, obtain enzymolysis chitosan；It counts in parts by weight, takes 20 parts of starch octenyl succinate anhydrides, 10 parts of enzymolysis successively
Starch octenyl succinate anhydride, enzymolysis chitosan and water are first mixed and pour into No. 2 burnings by chitosan, 200 parts of water, 6 parts of linoleic acid
Cup after being stirred 10min with glass bar, under room temperature, stands swelling 5h, then beaker immigration digital display is tested the speed constant temperature magnetic
Power blender is 70 DEG C in temperature, and under the conditions of rotating speed is 1200r/min, heating stirring disperses 2h, obtains dispersion liquid, then to dispersion
Linoleic acid is added in liquid, continues to be stirred 45min with 500r/min rotating speeds, obtains emulsified dispersed liquid；It counts in parts by weight, successively
Take 60 parts of emulsified dispersed liquids, 10 parts of polyethyleneimines, 8 parts of crosslinking agents that band first is added in emulsified dispersed liquid and polyethyleneimine and is stirred
The three-necked flask for mixing device is passed through dioxy into three-necked flask under the conditions of speed of agitator is 600r/min with 120mL/min rates
Change carbon gas, after being continually fed into 3h, stopping is passed through carbon dioxide gas, and crosslinking agent is added, and continuation is stirred with 600r/min rotating speeds
Mixing 45min is mixed, function additive is obtained；It counts in parts by weight, takes 50 parts of function additives, the silicon that 10 parts of mass fractions are 10% successively
Acid sodium solution, 15 parts of anionic polyacrylamide, 150 parts of water, 500 parts of pitch particles, 8 parts of isocyanates, first by function additive,
Sodium silicate solution, water and pitch particle are stirred 45min under the conditions of rotating speed is 800r/min, under stirring, with
1.5 DEG C/min rate programs are warming up to 70 DEG C, after insulated and stirred reacts 45min, and continuation is warming up to 4 DEG C/min rate programs
185 DEG C, after thermal insulation foaming 45min, stops heating, and cooled to room temperature, add isocyanates, continue to be stirred to react
15min, discharging, obtains expansion pitch.The crosslinking agent is the calcium nitrate solution that mass fraction is 8%.The anion pp acyl
Amine is the anionic polyacrylamide that molecular weight is 650~7,500,000.The pitch particle preparation process is：Asphalt is cold
After agar is broken, 80 mesh sieve is crossed, pitch particle is obtained.The isocyanates is：Methyl diphenylene diisocyanate.
Example 6
It is 1 in mass ratio by chitosan and water：15 mixing are poured into No. 1 beaker, after being stirred 15min with glass bar, in room
Under the conditions of temperature, after standing swelling 5h, the chitosan enzyme of 0.08 times of chitosan mass is added, No. 1 beaker is then moved into digital display
Test the speed constant temperature blender with magnetic force, is 35 DEG C in temperature, under the conditions of rotating speed is 500r/min, constant temperature stirring digests 60min, then at temperature
Under the conditions of degree is 90 DEG C, after keeping the temperature enzyme deactivation 15min, material in No. 1 beaker is transferred to Rotary Evaporators, is 85 DEG C in temperature, presses
Power be 550kPa under the conditions of, be concentrated under reduced pressure 2h, obtain concentrate, then concentrate is transferred in baking oven, in temperature be 110 DEG C of conditions
Under, it is dry to constant weight, obtain enzymolysis chitosan；It counts in parts by weight, takes 20 parts of starch octenyl succinate anhydrides, 10 parts of enzymolysis successively
Starch octenyl succinate anhydride, enzymolysis chitosan and water are first mixed and pour into No. 2 burnings by chitosan, 200 parts of water, 6 parts of linoleic acid
Cup after being stirred 10min with glass bar, under room temperature, stands swelling 5h, then beaker immigration digital display is tested the speed constant temperature magnetic
Power blender is 70 DEG C in temperature, and under the conditions of rotating speed is 1200r/min, heating stirring disperses 2h, obtains dispersion liquid, then to dispersion
Linoleic acid is added in liquid, continues to be stirred 45min with 500r/min rotating speeds, obtains emulsified dispersed liquid；It counts in parts by weight, successively
Take 60 parts of emulsified dispersed liquids, 8 parts of crosslinking agents that emulsified dispersed liquid is first added to the three-necked flask of belt stirrer, is in speed of agitator
Under the conditions of 600r/min, carbon dioxide gas is passed through into three-necked flask with 120mL/min rates, after being continually fed into 3h, is stopped
It is passed through carbon dioxide gas, and crosslinking agent is added, continues to be stirred 45min with 600r/min rotating speeds, obtains function additive；By weight
Number meter is measured, takes 50 parts of function additives, the sodium silicate solution that 10 parts of mass fractions are 10%, 15 parts of anion pp acyls successively
Amine, 150 parts of water, 500 parts of pitch particles, 8 parts of isocyanates, first by function additive, sodium silicate solution, water and pitch particle in turn
Under the conditions of speed is 800r/min, it is stirred 45min, under stirring, 70 are warming up to 1.5 DEG C/min rate programs
DEG C, after insulated and stirred reacts 45min, continue to be warming up to 185 DEG C with 4 DEG C/min rate programs, after thermal insulation foaming 45min, stop
Heating, and cooled to room temperature, add isocyanates, continue to be stirred to react 15min, discharge, obtain expansion pitch.The friendship
Connection agent is the chromium nitrate solution that mass fraction is 8%.The anionic polyacrylamide be molecular weight be 650~7,500,000 it is cloudy from
Sub- polyacrylamide.The pitch particle preparation process is：After asphalt Freezing smashing, 80 mesh sieve is crossed, pitch particle is obtained.
The isocyanates is：Methyl diphenylene diisocyanate.
Example 7
It is 1 in mass ratio by chitosan and water：15 mixing are poured into No. 1 beaker, after being stirred 15min with glass bar, in room
Under the conditions of temperature, after standing swelling 5h, the chitosan enzyme of 0.08 times of chitosan mass is added, No. 1 beaker is then moved into digital display
Test the speed constant temperature blender with magnetic force, is 35 DEG C in temperature, under the conditions of rotating speed is 500r/min, constant temperature stirring digests 60min, then at temperature
Under the conditions of degree is 90 DEG C, after keeping the temperature enzyme deactivation 15min, material in No. 1 beaker is transferred to Rotary Evaporators, is 85 DEG C in temperature, presses
Power be 550kPa under the conditions of, be concentrated under reduced pressure 2h, obtain concentrate, then concentrate is transferred in baking oven, in temperature be 110 DEG C of conditions
Under, it is dry to constant weight, obtain enzymolysis chitosan；It counts in parts by weight, takes 20 parts of starch octenyl succinate anhydrides, 10 parts of enzymolysis successively
Starch octenyl succinate anhydride, enzymolysis chitosan and water are first mixed and pour into No. 2 burnings by chitosan, 200 parts of water, 6 parts of linoleic acid
Cup after being stirred 10min with glass bar, under room temperature, stands swelling 5h, then beaker immigration digital display is tested the speed constant temperature magnetic
Power blender is 70 DEG C in temperature, and under the conditions of rotating speed is 1200r/min, heating stirring disperses 2h, obtains dispersion liquid, then to dispersion
Linoleic acid is added in liquid, continues to be stirred 45min with 500r/min rotating speeds, obtains emulsified dispersed liquid；It counts in parts by weight, successively
Take 60 parts of emulsified dispersed liquids, 10 parts of polyethyleneimines, 8 parts of crosslinking agents that band first is added in emulsified dispersed liquid and polyethyleneimine and is stirred
The three-necked flask for mixing device is passed through dioxy into three-necked flask under the conditions of speed of agitator is 600r/min with 120mL/min rates
Change carbon gas, after being continually fed into 3h, stopping is passed through carbon dioxide gas, and crosslinking agent is added, and continuation is stirred with 600r/min rotating speeds
Mixing 45min is mixed, function additive is obtained；It counts in parts by weight, takes 50 parts of function additives successively, 15 parts of anionic polyacrylamide,
150 parts of water, 500 parts of pitch particles, 8 parts of isocyanates, first by function additive, water and pitch particle in rotating speed be 800r/min items
Under part, it is stirred 45min, under stirring, is warming up to 70 DEG C with 1.5 DEG C/min rate programs, insulated and stirred reaction
After 45min, continue to be warming up to 185 DEG C with 4 DEG C/min rate programs, after thermal insulation foaming 45min, stops heating, and natural cooling
To room temperature, isocyanates is added, continues to be stirred to react 15min, discharges, obtains expansion pitch.The crosslinking agent is mass fraction
For 8% chromium nitrate solution.The anionic polyacrylamide is the anionic polyacrylamide that molecular weight is 650~7,500,000.
The pitch particle preparation process is：After asphalt Freezing smashing, 80 mesh sieve is crossed, pitch particle is obtained.The isocyanates
For：Methyl diphenylene diisocyanate.
Example 8
It is 1 in mass ratio by chitosan and water：15 mixing are poured into No. 1 beaker, after being stirred 15min with glass bar, in room
Under the conditions of temperature, after standing swelling 5h, the chitosan enzyme of 0.08 times of chitosan mass is added, No. 1 beaker is then moved into digital display
Test the speed constant temperature blender with magnetic force, is 35 DEG C in temperature, under the conditions of rotating speed is 500r/min, constant temperature stirring digests 60min, then at temperature
Under the conditions of degree is 90 DEG C, after keeping the temperature enzyme deactivation 15min, material in No. 1 beaker is transferred to Rotary Evaporators, is 85 DEG C in temperature, presses
Power be 550kPa under the conditions of, be concentrated under reduced pressure 2h, obtain concentrate, then concentrate is transferred in baking oven, in temperature be 110 DEG C of conditions
Under, it is dry to constant weight, obtain enzymolysis chitosan；It counts in parts by weight, takes 20 parts of starch octenyl succinate anhydrides, 10 parts of enzymolysis successively
Starch octenyl succinate anhydride, enzymolysis chitosan and water are first mixed and pour into No. 2 burnings by chitosan, 200 parts of water, 6 parts of linoleic acid
Cup after being stirred 10min with glass bar, under room temperature, stands swelling 5h, then beaker immigration digital display is tested the speed constant temperature magnetic
Power blender is 70 DEG C in temperature, and under the conditions of rotating speed is 1200r/min, heating stirring disperses 2h, obtains dispersion liquid, then to dispersion
Linoleic acid is added in liquid, continues to be stirred 45min with 500r/min rotating speeds, obtains emulsified dispersed liquid；It counts in parts by weight, successively
Take 60 parts of emulsified dispersed liquids, 10 parts of polyethyleneimines, 8 parts of crosslinking agents that band first is added in emulsified dispersed liquid and polyethyleneimine and is stirred
The three-necked flask for mixing device is passed through dioxy into three-necked flask under the conditions of speed of agitator is 600r/min with 120mL/min rates
Change carbon gas, after being continually fed into 3h, stopping is passed through carbon dioxide gas, and crosslinking agent is added, and continuation is stirred with 600r/min rotating speeds
Mixing 45min is mixed, function additive is obtained；It counts in parts by weight, takes 50 parts of function additives, the silicon that 10 parts of mass fractions are 10% successively
Acid sodium solution, 15 parts of anionic polyacrylamide, 150 parts of water, 500 parts of pitch particles, first by function additive, sodium silicate solution,
Water and pitch particle are stirred 45min under the conditions of rotating speed is 800r/min, under stirring, with 1.5 DEG C/min speed
Rate temperature programming is to 70 DEG C, after insulated and stirred reacts 45min, continues to be warming up to 185 DEG C with 4 DEG C/min rate programs, heat preservation hair
After steeping 45min, stop heating, and cooled to room temperature, discharging obtains expansion pitch.The crosslinking agent is that mass fraction is 8%
Chromium nitrate solution.The anionic polyacrylamide is the anionic polyacrylamide that molecular weight is 650~7,500,000.It is described
Pitch particle preparation process is：After asphalt Freezing smashing, 80 mesh sieve is crossed, pitch particle is obtained.
Comparative example：The expansion pitch of Jiangsu Construction Company Limited production.
The expansion pitch of 1 to 8 gained of example and comparative example product are subjected to performance detection, specific detection method is as follows：
Mechanical property：15 DEG C of cleavage strengths of test specimen are detected according to DB13/T 2513；
Specific testing result is as shown in table 1：
Table 1
| Detection project | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Example 7 | Example 8 | Comparative example |
| Cleavage strength/MPa | 0.78 | 0.71 | 0.68 | 0.66 | 0.67 | 0.63 | 0.57 | 0.54 | 0.43 |
By 1 testing result of table it is found that expansion pitch prepared by technical solution of the present invention has the characteristics that excellent mechanical property,
It has broad prospects in the development of paving materials industry.
Claims (6)
1. a kind of preparation method of expansion pitch, it is characterised in that specifically preparation process is：
（1）It counts in parts by weight, takes 10~20 parts of starch octenyl succinate anhydrides successively, 8~10 parts of enzymolysis chitosans, 150~
200 parts of water, 4~6 parts of linoleic acid, after first starch octenyl succinate anhydride, enzymolysis chitosan and water are mixed, swelling, then through adding
Thermal agitation disperses, and obtains dispersion liquid, adds linoleic acid, be stirred, obtains emulsified dispersed liquid；
（2）It counts in parts by weight, takes 40~60 parts of emulsified dispersed liquids successively, 8~10 parts of polyethyleneimines, 3~8 parts of crosslinking agents,
First emulsified dispersed liquid and polyethyleneimine are stirred, and carbon dioxide is passed through during being stirred, is then added and hands over
Join agent, continues to be stirred, obtain function additive；
（3）It counts in parts by weight, 30~50 parts of function additives, 8~10 parts of sodium silicate solutions, 10~15 parts of anion is taken to gather successively
Acrylamide, 100~150 parts of water, 300~500 parts of pitch particles, 4~8 parts of isocyanates are first molten by function additive, sodium metasilicate
After liquid, water and the mixing of pitch particle, under stirring, 60~70 DEG C is warming up to 0.8~1.5 DEG C/min rate programs, is protected
After 30~45min of temperature reaction, continue to be warming up to 180~185 DEG C with 2~4 DEG C/min rate programs, 30~45min of thermal insulation foaming
Afterwards, cooled to room temperature adds isocyanates, continues to be stirred to react 10~15min, discharging is to get expansion pitch.
2. a kind of preparation method of expansion pitch according to claim 1, which is characterized in that step（1）The enzymolysis shell
Glycan preparation process is：It is 1 in mass ratio by chitosan and water：10~1：After 15 are stirred, swelling is stood, it is poly- to add shell
The chitosan enzyme that 0.06~0.08 times of saccharic amount, after constant temperature stirring digests, enzyme deactivation concentrates, dry, obtains enzymolysis chitosan.
3. a kind of preparation method of expansion pitch according to claim 1, which is characterized in that step（2）The crosslinking agent
The chromium nitrate solution for being 6~8% for mass fraction.
4. a kind of preparation method of expansion pitch according to claim 1, which is characterized in that step（3）The anion
Polyacrylamide is the anionic polyacrylamide that molecular weight is 600~8,000,000.
5. a kind of preparation method of expansion pitch according to claim 1, which is characterized in that step（3）The pitch is broken
Expect that preparation process is：After asphalt Freezing smashing, 60~80 mesh sieve is crossed, pitch particle is obtained.
6. a kind of preparation method of expansion pitch according to claim 1, which is characterized in that step（3）The isocyanic acid
Ester is：It is arbitrary in methyl diphenylene diisocyanate, dicyclohexyl methyl hydride diisocyanate or isophorone diisocyanate
It is a kind of.
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