CN108864718A - A kind of preparation method of high penetration bitumen regenerative agent - Google Patents
A kind of preparation method of high penetration bitumen regenerative agent Download PDFInfo
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- C08L95/00—Compositions of bituminous materials, e.g. asphalt, tar, pitch
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Abstract
The present invention relates to a kind of preparation methods of high penetration bitumen regenerative agent, belong to engineering material preparation technical field.The present invention heats octanol polyoxyethylene ether,Then dimethyldichlorosilane is put into thereto,Organosilicon structures and octanol polyoxyethylene ether are made to establish coupling channel,The present invention is by bagasse,Pork liver,The biological raw materials such as rice straw and peanut oil are placed under nitrogen protection,High temperature and pressure extracts the organic principle in biological raw material,These functional groups can form covalent bond with other particles,Hydrogen bond and intermolecular force absorption,Bamboo chip is also placed in sodium hydroxide solution high temperature and impregnated by the present invention,It is mixed into sodium sulfite and formaldehyde thereto again,Bamboo fibre is set to carry out sulfonating reaction and hydroxymethylation,Two kinds of hydrophilic functional groups being introduced into can be such that the lignosulfonates extracted in bamboo fibre are preferably scattered in bitumen regenerant,Reinforce the mechanical property of regeneration asphalt by the excellent mechanical property of bamboo fibre itself,It has broad application prospects.
Description
Technical field
The present invention relates to a kind of preparation methods of high penetration bitumen regenerative agent, belong to engineering material preparation technical field.
Background technique
Bitumen regenerant is a kind of new material early, mid-term highway maintenance suitable for bituminous pavement.The regeneration of pitch is just
It is the inverse process of aging.Regenerative agent can be usually mixed, such as mixes corn oil, lubricating oil.After mixing regenerative agent, make asphalitine is opposite to contain
Amount reduces, and improves malthene to the solvability of asphalitine, improves the compatibility of pitch, improves the needle penetration of pitch and prolongs
Degree restores it or close to original performance.
For the regenerated mechanism of pitch at present there are two types of theoretical, a kind of theory is " united Lagrangian- Eulerian method ", the theory chemically heating power
Set out, it is believed that pitch generates the reduction that the reason of aging is each component compatibility in pitch colloidal system, causes molten between component
Parameter difference is spent to increase.Reduce its solubility parameters difference as can mixing certain regenerative agent, then pitch can be restored to original property
Matter.Another theory is " composition regulation is theoretical ".The theory is that chemically component is migrated and set out, it is believed that due to migrating for component,
After ageing of asphalt, certain components are on the high side, and certain components are on the low side, and ratio is uncoordinated between each component, so leading to asphalt road
It can reduce, original property will be restored as can adjusting its component by admixture regenerative agent and surveying pitch.In fact, the two theories are
Consistent, the former is explained from the chemical energy of pitch internal structure, and the latter is explained from macroscopical chemical composition amount.
Bitumen regenerant is divided into according to regenerative process：Hot asphalt regeneration（It is mixed again including Hot-In-Plant Recycling and live heat
It is raw）And cold renewal, wherein heated tool butt-welding is more mature compared to cold recycling technology, and the bituminous concrete property regenerated is more preferable.It is existing
It is mainly made of heavy mineral oil or light oil bitumen regenerant, secondly also contains polymer, antistripping agent, stabilizer, resists
Ultraviolet light auxiliary agent and age resister.
Existing hot asphalt regenerative agent generally can only all be regenerated in regenerative process on the surface layer of aged asphalt, be difficult
Aged asphalt inner layer is penetrated into rapidly, aged asphalt property can not be made to restore comprehensively.I.e. existing hot asphalt regenerative agent is only capable of making
Aged asphalt performance obtains a degree of recovery, but comprehensively thorough not enough, makes the usability on Recycled Asphalt Pavement road surface
It can have a greatly reduced quality, shorten the service life on road surface.I.e. current bitumen regenerant penetrating power is not strong, and bond effect is bad,
The regeneration asphalt intensity difference generated simultaneously.
Therefore, invent that a kind of adhesion strength is high and the high penetration bitumen regenerative agent of good penetrability prepares skill to engineering material
Art field has positive effect.
Summary of the invention
The technical problems to be solved by the invention：It is not strong for current bitumen regenerant penetrating power, bond effect is bad,
The defect of the regeneration asphalt intensity difference generated simultaneously, provides a kind of preparation method of high penetration bitumen regenerative agent.
In order to solve the above technical problems, the technical solution adopted by the present invention is that：
A kind of preparation method of high penetration bitumen regenerative agent, it is characterised in that specifically preparation step is：
（1）100~150g octanol polyoxyethylene ether is put into three-necked flask, three-necked flask is heated to 50~55 DEG C,
It is mixed under constant temperature with blender, the dimethyl dichloro of octanol polyoxyethylene ether quality 30~35% is added dropwise into three-necked flask
The petroleum ether solution of silane controls drop rate, drips off in 50~60min, after being added dropwise to complete, continuation isothermal reaction 60~
Sodium hydroxide solution is added dropwise after reaction and adjusts pH value to neutrality by 70min, and obtained mixed solution is spare；
（2）According to parts by weight, 3~5 portions of bagasse, 1~2 part of pork liver, 10~12 parts of rice straws and 6~8 portions of peanuts are weighed
It in oil investment reaction kettle, is mixed with blender, is passed through nitrogen after stirring into reaction kettle and excludes air, and improve gas in kettle
Pressure；
（3）Temperature in aforesaid reaction vessel is increased after excluding air, is passed through nitrogen when reacting 10min, 15min, 20min respectively
Reactor off-gas is excluded, after 5~7h of isothermal reaction, with the cooling reaction kettle of ice water, reduces temperature in the kettle to room temperature, by gas out of kettle
Release reduces air pressure in kettle and is filtered product in kettle to standard atmospheric pressure, obtains filtrate, put the filtrate into vacuum oven
Adhesive solution is made in middle vacuum concentration, spare；
（4）The bamboo chip for weighing 500~700g, which is put into grinder, to be ground, cross 150 meshes obtain sieving powder, will sieving powder with
Distilled water in mass ratio 1:In 3 mixing investment beakers, it is mixed with blender, beaker is put into constant temperature in water-bath after stirring and is added
Sodium hydroxide solution is added dropwise into beaker for heat, adjusts pH value to 11~13, continues heated at constant temperature, mixed serum is made；
（5）2~3 times of mixed serum quality of sodium sulfite solution is added into above-mentioned beaker, places the beaker in water-bath, uses
Blender, which is mixed, is made mixed dispersion liquid, and the formalin of mixed dispersion liquid quality 10~15% is added dropwise into beaker, continues
Water bath with thermostatic control heats 2~3h and reaction solution is made；
（6）According to parts by weight, weigh 7~9 parts of spare mixed solutions, 5~7 parts of spare adhesive solutions, 3~5 parts it is above-mentioned
In reaction solution, 13~15 parts of phenol and 10~12 parts of N-Methyl pyrrolidone investment flasks, flask blender is mixed and is stirred
It mixes, flask is put into sonic oscillation instrument after stirring and is vibrated, high penetration bitumen regenerative agent is made.
Step（1）Described in three-necked flask heat temperature raising temperature to 50~55 DEG C, the revolving speed of blender is 300~
350r/min, mixing time are 20~30min, the mass fraction of the petroleum ether solution of dimethyldichlorosilane is 20~
25%, the mass fraction of sodium hydroxide solution is 15~20%.
Step（2）Described in blender revolving speed be 200~220r/min, mixing time be 30~40min, stir
Air pressure is improved to 2~3MPa in kettle.
Step（3）Described in reaction kettle in temperature be increased to 290~310 DEG C, the temperature in vacuum oven be 40~
45 DEG C, vacuum degree be 30~50Pa, the vacuum concentration time be 80~100min.
Step（4）Described in blender speed of agitator be 600~700r/min, mixing time be 30~
40min, bath temperature are 95~100 DEG C, and the heated at constant temperature time is 60~70min, and the mass fraction of sodium hydroxide solution is 15
~20%, the continuation heated at constant temperature time is 2~3h.
Step（5）Described in the mass fraction of sodium sulfite solution be 20~25%, the bath temperature of water-bath is 50~
55 DEG C, the revolving speed of blender is 200~250r/min, and mixing time is 50~60min, and the mass fraction of formalin is
3~5%.
Step（6）Described in blender revolving speed be 200~220r/min, mixing time be 20~30min, surpass
Supersonic frequency in sound oscillation instrument is 30~35kHz, and duration of oscillation is 12~14h.
The method have the benefit that：
（1）First mixed solution is made in octanol polyoxyethylene ether and dimethyldichlorosilane hybrid reaction by the present invention, then with sweet
Bagasse, pork liver, rice straw and peanut oil are that adhesive solution is made in raw material under conditions of completely cutting off air and high temperature and pressure, then
Bamboo chip is crushed and water rushes exchange into bamboo pulp, lye heating reaction is added, then sequentially adds sodium sulfite and formaldehyde generates instead
Solution is answered, finally mixed solution, spare adhesive solution, reaction solution, phenol and N-Methyl pyrrolidone are mixed and made
High penetration bitumen regenerative agent is obtained, the present invention heats octanol polyoxyethylene ether, dimethyldichlorosilane is then put into thereto,
Silicon unit is introduced into octanol polyoxyethylene ether, so that organosilicon structures and octanol polyoxyethylene ether is established coupling channel, makes product
Thermal stability and chemical stability be improved, and reduce surface tension, reduce the generation of bubble in solution, make octanol polyoxy
The penetrating power of vinethene enhances, so that bitumen regenerant be made to have good permeability, improves pitch power of regeneration；
（2）The present invention places the biological raw materials such as bagasse, pork liver, rice straw and peanut oil under nitrogen protection, and high temperature is high
Pressure extracts organic principle in biological raw material, have in these organic principles ester group, phenolic hydroxyl group, amino, epoxy group and
Other organo-functional groups, these functional groups can form covalent bond, hydrogen bond and intermolecular force with other particles and adsorb, add
Strong bonding effect, make to act between each molecule in pitch it is even closer, while wherein have lignin fibre, can use wooden
The stable chemical property of cellulose fiber itself reinforces the thermal stability and weatherability of regenerative agent to a certain extent, and the present invention is also by bamboo chip
Be placed in the immersion of sodium hydroxide solution high temperature, then be mixed into sodium sulfite and formaldehyde thereto, make bamboo fibre carry out sulfonating reaction with
Hydroxymethylation, two kinds of hydrophilic functional groups being introduced into can be such that the lignosulfonates extracted in bamboo fibre preferably disperse
In bitumen regenerant, bond bamboo fibre preferably with particle each in pitch, it is excellent by bamboo fibre itself
Mechanical property reinforces the mechanical property of regeneration asphalt, has broad application prospects.
Specific embodiment
100~150g octanol polyoxyethylene ether is put into three-necked flask, three-necked flask is heated to 50~55 DEG C,
20~30min is mixed with the revolving speed of 300~350r/min with blender under constant temperature, octanol polyoxy is added dropwise into three-necked flask
Speed is added dropwise in the petroleum ether solution for the dimethyldichlorosilane that the mass fraction of vinethene quality 30~35% is 20~25%, control
Rate drips off in 50~60min, after being added dropwise to complete, continues 60~70min of isothermal reaction, mass fraction is added dropwise after reaction
PH value is adjusted to neutrality for 15~20% sodium hydroxide solution, and obtained mixed solution is spare；According to parts by weight, 3~5 are weighed
In part bagasse, 1~2 part of pork liver, 10~12 parts of rice straws and 6~8 parts of peanut oil investment reaction kettles, with blender with 200
30~40min is mixed in the revolving speed of~220r/min, is passed through nitrogen after stirring into reaction kettle and excludes air, and improves in kettle
Air pressure is to 2~3MPa；Temperature in aforesaid reaction vessel is increased to 290~310 DEG C after excluding air, respectively reaction 10min,
It is passed through nitrogen when 15min, 20min and excludes reactor off-gas, after 5~7h of isothermal reaction, with the cooling reaction kettle of ice water, reduces temperature in kettle
To room temperature, gas is discharged out of kettle reduces air pressure in kettle is filtered product in kettle, is filtered to standard atmospheric pressure degree
Liquid is put the filtrate into vacuum oven, is concentrated in vacuo 80 under conditions of temperature is 40~45 DEG C, vacuum degree is 30~50Pa
Adhesive solution is made in~100min, spare；The bamboo chip for weighing 500~700g, which is put into grinder, to be ground, and is crossed 150 meshes and is obtained
Be sieved powder, by sieving powder and distilled water in mass ratio 1:In 3 mixing investment beakers, with blender with 600~700r/min
Revolving speed 30~40min is mixed, after stirring by beaker be put into temperature be heated at constant temperature 60 in 95~100 DEG C of water-bath~
The sodium hydroxide solution that mass fraction is 15~20% is added dropwise into beaker by 70min, adjusts pH value to 11~13, continues constant temperature and add
Mixed serum is made in 2~3h of heat；The mass fraction that 2~3 times of mixed serum quality are added into above-mentioned beaker is 20~25%
Sodium sulfite solution places the beaker in the water-bath that bath temperature is 50~55 DEG C, with blender with 200~250r/min's
50~60min is mixed in revolving speed, and mixed dispersion liquid is made, and the quality of mixed dispersion liquid quality 10~15% is added dropwise into beaker
The formalin that score is 3~5% continues water bath with thermostatic control and heats the obtained reaction solution of 2~3h；According to parts by weight, it weighs spare
7~9 parts of mixed solutions, 5~7 parts of spare adhesive solutions, 3~5 parts of above-mentioned reaction solutions, 13~15 parts of phenol and 10~12
In part N-Methyl pyrrolidone investment flask, flask blender is mixed 20 with the revolving speed of 200~220r/min~
Flask is put into sonic oscillation instrument by 30min after stirring, and 12~14h is vibrated under conditions of supersonic frequency is 30~35kHz,
High penetration bitumen regenerative agent is made.
Example 1
100g octanol polyoxyethylene ether is put into three-necked flask, three-necked flask is heated to 50 DEG C, with stirring under constant temperature
20min is mixed with the revolving speed of 300r/min in device, and the quality point of octanol polyoxyethylene ether quality 30% is added dropwise into three-necked flask
The petroleum ether solution for the dimethyldichlorosilane that number is 20% controls drop rate, drips off in 50min, after being added dropwise to complete, after
The sodium hydroxide solution that mass fraction is 15% is added dropwise after reaction and adjusts pH value to neutrality, is made by continuous isothermal reaction 60min
Mixed solution, it is spare；According to parts by weight, 3 portions of bagasse, 1 part of pork liver, 10 parts of rice straws and 6 parts of peanut oil investments are weighed
In reaction kettle, 30min is mixed with the revolving speed of 200r/min with blender, nitrogen is passed through after stirring into reaction kettle and excludes sky
Gas, and air pressure is improved in kettle to 2MPa；Temperature in aforesaid reaction vessel is increased to 290 DEG C after exclusion air, is being reacted respectively
It is passed through nitrogen when 10min, 15min, 20min and excludes reactor off-gas, after isothermal reaction 5h, with the cooling reaction kettle of ice water, reduces kettle
To room temperature, gas is discharged out of kettle reduces air pressure in kettle is filtered product in kettle, obtains to standard atmospheric pressure interior temperature
Filtrate puts the filtrate into vacuum oven, is concentrated in vacuo 80min under conditions of temperature is 40 DEG C, vacuum degree is 30Pa, system
Adhesive solution is obtained, it is spare；The bamboo chip for weighing 500g, which is put into grinder, to be ground, and is crossed 150 meshes and is obtained sieving powder, by the powder that is sieved
End and distilled water in mass ratio 1:In 3 mixing investment beakers, 30min is mixed with the revolving speed of 600r/min with blender, is stirred
Beaker is put into heated at constant temperature 60min in the water-bath that temperature is 95 DEG C after mixing, the hydrogen-oxygen that mass fraction is 15% is added dropwise into beaker
Change sodium solution, adjusts pH value to 11, continue heated at constant temperature 2h, mixed serum is made；Mixed serum matter is added into above-mentioned beaker
The sodium sulfite solution that the mass fraction of 2 times of amount is 20% places the beaker in the water-bath that bath temperature is 50 DEG C, with stirring
50min is mixed with the revolving speed of 200r/min in device, and mixed dispersion liquid is made, and mixed dispersion liquid quality 10% is added dropwise into beaker
Mass fraction be 3% formalin, continue water bath with thermostatic control heating 2h be made reaction solution；According to parts by weight, it weighs spare
7 parts of mixed solutions, 5 parts of spare adhesive solutions, 3 parts of above-mentioned reaction solutions, 13 parts of phenol and 10 parts of N-Methyl pyrrolidones
It puts into flask, 20min is mixed with the revolving speed of 200r/min in flask blender, flask is put into ultrasonic vibration after stirring
It swings in instrument, vibrates 12h under conditions of supersonic frequency is 30kHz, high penetration bitumen regenerative agent is made.
Example 2
125g octanol polyoxyethylene ether is put into three-necked flask, three-necked flask is heated to 52 DEG C, with stirring under constant temperature
25min is mixed with the revolving speed of 320r/min in device, and the quality point of octanol polyoxyethylene ether quality 32% is added dropwise into three-necked flask
The petroleum ether solution for the dimethyldichlorosilane that number is 22% controls drop rate, drips off in 55min, after being added dropwise to complete, after
The sodium hydroxide solution that mass fraction is 17% is added dropwise after reaction and adjusts pH value to neutrality, is made by continuous isothermal reaction 65min
Mixed solution, it is spare；According to parts by weight, 4 portions of bagasse, 1 part of pork liver, 11 parts of rice straws and 7 parts of peanut oil investments are weighed
In reaction kettle, 35min is mixed with the revolving speed of 210r/min with blender, nitrogen is passed through after stirring into reaction kettle and excludes sky
Gas, and air pressure is improved in kettle to 2MPa；Temperature in aforesaid reaction vessel is increased to 300 DEG C after exclusion air, is being reacted respectively
It is passed through nitrogen when 10min, 15min, 20min and excludes reactor off-gas, after isothermal reaction 6h, with the cooling reaction kettle of ice water, reduces kettle
To room temperature, gas is discharged out of kettle reduces air pressure in kettle is filtered product in kettle, obtains to standard atmospheric pressure interior temperature
Filtrate puts the filtrate into vacuum oven, is concentrated in vacuo 90min under conditions of temperature is 42 DEG C, vacuum degree is 40Pa, system
Adhesive solution is obtained, it is spare；The bamboo chip for weighing 600g, which is put into grinder, to be ground, and is crossed 150 meshes and is obtained sieving powder, by the powder that is sieved
End and distilled water in mass ratio 1:In 3 mixing investment beakers, 35min is mixed with the revolving speed of 650r/min with blender, is stirred
Beaker is put into heated at constant temperature 65min in the water-bath that temperature is 97 DEG C after mixing, the hydrogen-oxygen that mass fraction is 17% is added dropwise into beaker
Change sodium solution, adjusts pH value to 12, continue heated at constant temperature 2.5h, mixed serum is made；Mixed serum is added into above-mentioned beaker
The sodium sulfite solution that the mass fraction that 2 times of quality is 22%, placing the beaker bath temperature is in 52 DEG C of water-bath, with stirring
It mixes device and 55min is mixed with the revolving speed of 220r/min, mixed dispersion liquid is made, mixed dispersion liquid quality is added dropwise into beaker
The formalin that 12% mass fraction is 4% continues water bath with thermostatic control heating 2.5h and reaction solution is made；According to parts by weight, claim
Take 8 parts of spare mixed solutions, 6 parts of spare adhesive solutions, 4 parts of above-mentioned reaction solutions, 14 parts of phenol and 11 parts of N- methyl pyrroles
Pyrrolidone is put into flask, and 25min is mixed with the revolving speed of 210r/min in flask blender, is put into flask after stirring
In sonic oscillation instrument, 13h is vibrated under conditions of supersonic frequency is 32kHz, high penetration bitumen regenerative agent is made.
Example 3
150g octanol polyoxyethylene ether is put into three-necked flask, three-necked flask is heated to 55 DEG C, with stirring under constant temperature
30min is mixed with the revolving speed of 350r/min in device, and the quality point of octanol polyoxyethylene ether quality 35% is added dropwise into three-necked flask
The petroleum ether solution for the dimethyldichlorosilane that number is 25% controls drop rate, drips off in 60min, after being added dropwise to complete, after
The sodium hydroxide solution that mass fraction is 20% is added dropwise after reaction and adjusts pH value to neutrality, is made by continuous isothermal reaction 70min
Mixed solution, it is spare；According to parts by weight, 5 portions of bagasse, 2 parts of pork livers, 12 parts of rice straws and 8 parts of peanut oil investments are weighed
In reaction kettle, 40min is mixed with the revolving speed of 220r/min with blender, nitrogen is passed through after stirring into reaction kettle and excludes sky
Gas, and air pressure is improved in kettle to 3MPa；Temperature in aforesaid reaction vessel is increased to 310 DEG C after exclusion air, is being reacted respectively
It is passed through nitrogen when 10min, 15min, 20min and excludes reactor off-gas, after isothermal reaction 7h, with the cooling reaction kettle of ice water, reduces kettle
To room temperature, gas is discharged out of kettle reduces air pressure in kettle is filtered product in kettle, obtains to standard atmospheric pressure interior temperature
Filtrate puts the filtrate into vacuum oven, is concentrated in vacuo 100min under conditions of temperature is 45 DEG C, vacuum degree is 50Pa,
Adhesive solution is made, it is spare；The bamboo chip for weighing 700g, which is put into grinder, to be ground, and is crossed 150 meshes and is obtained sieving powder, will be sieved
Powder and distilled water in mass ratio 1:In 3 mixing investment beakers, 40min is mixed with the revolving speed of 700r/min with blender,
Beaker is put into heated at constant temperature 70min in the water-bath that temperature is 100 DEG C after stirring, it is 20% that mass fraction is added dropwise into beaker
Sodium hydroxide solution adjusts pH value to 13, continues heated at constant temperature 3h, mixed serum is made；Mixing slurry is added into above-mentioned beaker
The sodium sulfite solution that the mass fraction that 3 times of liquid quality is 25% is placed the beaker in the water-bath that bath temperature is 55 DEG C, is used
60min is mixed with the revolving speed of 250r/min in blender, and mixed dispersion liquid is made, and mixed dispersion liquid quality is added dropwise into beaker
The formalin that 15% mass fraction is 5% continues water bath with thermostatic control heating 3h and reaction solution is made；According to parts by weight, it weighs
Spare 9 parts of mixed solutions, 7 parts of spare adhesive solutions, 5 parts of above-mentioned reaction solutions, 15 parts of phenol and 12 parts of N- methylpyrroles
Alkanone is put into flask, and 30min is mixed with the revolving speed of 220r/min in flask blender, is put into flask after stirring super
In sound oscillation instrument, 14h is vibrated under conditions of supersonic frequency is 35kHz, high penetration bitumen regenerative agent is made.
Comparative example
With the high penetration bitumen regenerative agent of Hangzhou company production as a comparison case to high penetration bitumen produced by the present invention
High penetration bitumen regenerative agent in regenerative agent and comparative example carries out performance detection, and testing result is as shown in table 1：
Test method：
Viscosity：The viscosity that pitch is tested using DV-11+Pro type Bu Shi rotational viscometer, according to《Highway engineering pitch and pitch
Test mixture regulation》Specified in method tested, 135 DEG C of the temperature of test.
Penetration test is detected by the standard of T0604-2011.
Ductility test is detected by the standard of T0605-2011.
Dynamic stability test is detected by GB T 25033-2010 standard.
The test of Marshall modulus is detected using Marshall stability apparatus.
Compression strength and tensile splitting strength test are detected by GB 11968-2006 standard.
1 bitumen regenerant performance measurement result of table
Good, needle penetration and ductility according to the high penetration bitumen regenerative agent bond effect produced by the present invention of data among the above
Height, Marshall modulus is high, and compression strength and tensile splitting strength are high, and the regeneration asphalt intensity of generation is high, and penetrating power is good, has
Wide application prospect.
Claims (7)
1. a kind of preparation method of high penetration bitumen regenerative agent, it is characterised in that specifically preparation step is：
（1）100~150g octanol polyoxyethylene ether is put into three-necked flask, three-necked flask is heated to 50~55 DEG C,
It is mixed under constant temperature with blender, the dimethyl dichloro of octanol polyoxyethylene ether quality 30~35% is added dropwise into three-necked flask
The petroleum ether solution of silane controls drop rate, drips off in 50~60min, after being added dropwise to complete, continuation isothermal reaction 60~
Sodium hydroxide solution is added dropwise after reaction and adjusts pH value to neutrality by 70min, and obtained mixed solution is spare；
（2）According to parts by weight, 3~5 portions of bagasse, 1~2 part of pork liver, 10~12 parts of rice straws and 6~8 portions of peanuts are weighed
It in oil investment reaction kettle, is mixed with blender, is passed through nitrogen after stirring into reaction kettle and excludes air, and improve gas in kettle
Pressure；
（3）Temperature in aforesaid reaction vessel is increased after excluding air, is passed through nitrogen when reacting 10min, 15min, 20min respectively
Reactor off-gas is excluded, after 5~7h of isothermal reaction, with the cooling reaction kettle of ice water, reduces temperature in the kettle to room temperature, by gas out of kettle
Release reduces air pressure in kettle and is filtered product in kettle to standard atmospheric pressure, obtains filtrate, put the filtrate into vacuum oven
Adhesive solution is made in middle vacuum concentration, spare；
（4）The bamboo chip for weighing 500~700g, which is put into grinder, to be ground, cross 150 meshes obtain sieving powder, will sieving powder with
Distilled water in mass ratio 1:In 3 mixing investment beakers, it is mixed with blender, beaker is put into constant temperature in water-bath after stirring and is added
Sodium hydroxide solution is added dropwise into beaker for heat, adjusts pH value to 11~13, continues heated at constant temperature, mixed serum is made；
（5）2~3 times of mixed serum quality of sodium sulfite solution is added into above-mentioned beaker, places the beaker in water-bath, uses
Blender, which is mixed, is made mixed dispersion liquid, and the formalin of mixed dispersion liquid quality 10~15% is added dropwise into beaker, continues
Water bath with thermostatic control heats 2~3h and reaction solution is made；
（6）According to parts by weight, weigh 7~9 parts of spare mixed solutions, 5~7 parts of spare adhesive solutions, 3~5 parts it is above-mentioned
In reaction solution, 13~15 parts of phenol and 10~12 parts of N-Methyl pyrrolidone investment flasks, flask blender is mixed and is stirred
It mixes, flask is put into sonic oscillation instrument after stirring and is vibrated, high penetration bitumen regenerative agent is made.
2. a kind of preparation method of high penetration bitumen regenerative agent according to claim 1, it is characterised in that：Step（1）
Described in three-necked flask heat temperature raising temperature to 50~55 DEG C, the revolving speed of blender is 300~350r/min, when mixing
Between be 20~30min, the mass fraction of the petroleum ether solution of dimethyldichlorosilane is 20~25%, the matter of sodium hydroxide solution
Measuring score is 15~20%.
3. a kind of preparation method of high penetration bitumen regenerative agent according to claim 1, it is characterised in that：Step（2）
Described in blender revolving speed be 200~220r/min, mixing time be 30~40min, stir air pressure in kettle and improve to 2
~3MPa.
4. a kind of preparation method of high penetration bitumen regenerative agent according to claim 1, it is characterised in that：Step（3）
Described in reaction kettle in temperature be increased to 290~310 DEG C, the temperature in vacuum oven is 40~45 DEG C, vacuum degree 30
~50Pa, vacuum concentration time are 80~100min.
5. a kind of preparation method of high penetration bitumen regenerative agent according to claim 1, it is characterised in that：Step（4）
Described in blender speed of agitator be 600~700r/min, mixing time be 30~40min, bath temperature 95
~100 DEG C, the heated at constant temperature time is 60~70min, and the mass fraction of sodium hydroxide solution is 15~20%, continues heated at constant temperature
Time is 2~3h.
6. a kind of preparation method of high penetration bitumen regenerative agent according to claim 1, it is characterised in that：Step（5）
Described in the mass fraction of sodium sulfite solution be 20~25%, the bath temperature of water-bath is 50~55 DEG C, and blender turns
Speed is 200~250r/min, and mixing time is 50~60min, and the mass fraction of formalin is 3~5%.
7. a kind of preparation method of high penetration bitumen regenerative agent according to claim 1, it is characterised in that：Step（6）
Described in the revolving speed of blender be 200~220r/min, mixing time is 20~30min, super in sonic oscillation instrument
Acoustic frequency is 30~35kHz, and duration of oscillation is 12~14h.
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