CN108485288A - A kind of heat resistance modified pitch of macromolecule and preparation method thereof - Google Patents
A kind of heat resistance modified pitch of macromolecule and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L95/00—Compositions of bituminous materials, e.g. asphalt, tar, pitch
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/28—Nitrogen-containing compounds
- C08K2003/282—Binary compounds of nitrogen with aluminium
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention discloses heat resistance modified pitches of a kind of macromolecule and preparation method thereof, and in particular to pitch chemical technology field, ingredient include：Pitch, modifying agent, sea sand, concrete, silane, vinyl pyrrolidone vinyl acetate copolymer, polyether Glycols, polyglyceryl fatty acid ester, octamethylcy-clotetrasiloxane, octaphenyl POSS, dimethylacetylamide, octyl phenyl cyclotetrasiloxane, 20 25% ammonium hydroxide, dispersant, pyromellitic acid anhydride, N methyl pyrrolidones, aluminium nitride, reinforcing bar slag, vinyl carboxylate, benzotriazole, Diacetone Acrylamide, polyvinylbenzenesulfonic acid, ammonium polyphosphate；When the heat resistance modified pitch of macromolecule prepared by the present invention is used for road pavement road surface, have compared with strong structure stability, high temperature resistant, low-temperature resistance, rutting resistance；The anti-fatigue ability on road surface is improved, road surface permanent deformation is reduced；Cementitiousness is strong, can be obviously improved road surface and meet the tensile capacity after water, and greatly improve the stability of pitch.
Description
Technical field：
The present invention relates to pitch chemical technology fields, and in particular to a kind of heat resistance modified pitch of macromolecule and its preparation side
Method.
Background technology：
The dark brown complex mixture that pitch is made of the hydrocarbon and its non metallic derivatives of different molecular weight,
It is one kind of high viscosity organic liquid, is in a liquid state, surface is in black, dissolves in carbon disulfide.It is dripped including bitumen, oil
Four kinds of green, shale tar pitch and coal tar asphalt etc..Main component is asphalitine and resin, is that one kind is waterproof and dampproof and corrosion-resistant has
Machine cementitious material.For coatings, plastics, rubber and other industries and the pavement etc..Next has higher boiling mineral oil and a small amount of
The compound of oxygen, sulphur and chlorine.It is glossy, it is in liquid, semisolid or solid state, matter is crisp when low temperature, caking property and antiseptic property
Well.
Many variations occur for highroad and road：The magnitude of traffic flow and traveling frequency sharp increase, the axis weight of freight is not
It is disconnected to increase, generally carry out divided lane one-way traffic, it is desirable that further increase road surface resistance to flow, i.e., the energy of Rut resistance under high temperature
Power；Improve flexible and elasticity, i.e., the ability of cracking resistance under low temperature；It improves abrasion performance ability and prolongs the service life.Modern architecture
Object generally uses large-span prestressed roof boarding, it is desirable that roof waterpoof material adapts to big displacement, more tolerant to harsh height wet
Time condition, durability is more preferable, there is tack, facilitates construction, reduces maintenance load.These variations that use environment occurs are to stone
The performance of oil asphalt proposes stern challenge.To petroleum asphalt modified, above-mentioned harsh requirement is adapted it to, people is caused
Attention.It is researched and developed by many decades, modified pavement asphalt various in style, waterproof roll and coating has occurred, showed
Go out certain Practical effect.But, user pair usually 2~7 times higher than common petroleum pitch in view of modified material price
Material engineering performance not yet can fully be held, and modified pitch increase of production is slow.Modified pavement asphalt be mainly used for airfield runway,
The application of mating formation of the special occasions such as waterproofing bridge floor, parking lot, sports ground, heavy traffic road surface, intersection and road surface turning.
Invention content：
Technical problem to be solved by the present invention lies in a kind of heat resistance modified pitches of macromolecule of offer and preparation method thereof, resist
Mobility, i.e., the ability of Rut resistance under high temperature；Improve flexible and elasticity, i.e., the ability of cracking resistance under low temperature；Improve wear-resisting energy consumption
Power and prolong the service life.Modern building generally uses large-span prestressed roof boarding, it is desirable that roof waterpoof material adapts to big
Displacement, more tolerant to harsh high/low temperature weather conditions, durability is more preferable, there is tack, facilitates construction, reduces maintenance load.
The technical problems to be solved by the invention are realized using technical solution below：
A kind of heat resistance modified pitch of macromolecule and preparation method thereof, includes the raw material of following number：
59-100 parts of pitch, 11-23 parts of modifying agent, 13-25 parts of sea sand, 35-55 parts of concrete, 13-21 parts of silane, ethylene
Base pyrrolidones -24-57 parts of vinyl acetate copolymer, 2-5 parts of polyether Glycols, 0.7-1 parts of polyglyceryl fatty acid ester, prestox
5-7 parts of cyclotetrasiloxane ,-POSS2-5 parts of octaphenyl, 30-40 parts of dimethylacetylamide, 1-3 parts of octyl phenyl cyclotetrasiloxane,
70-80 parts of 46-50 parts of 3-7 parts of 2-6 parts of ammonium hydroxide, dispersant, pyromellitic acid anhydride, N-Methyl pyrrolidone, the nitrogen of 20-25%
Change 3-7 parts of aluminium, 10-14 parts of reinforcing bar slag, 3-7 parts of vinyl carboxylate, 0.4-1 parts of benzotriazole, Diacetone Acrylamide 1-
1.7 parts, 2-8 parts of polyvinylbenzenesulfonic acid, 2-6 parts of ammonium polyphosphate.
Wherein modifying agent includes：13-24 parts of vinyl-vinyl acetate copolymer, 12-25 parts of butyl acrylate, buergerite
0.2-1.5 parts 0.5-3 parts of type boron nitride, polymerization of diamond nanoparticles stick；Preparation method：Into vinyl-vinyl acetate copolymer
The microwave treatment 5min under microwave frequency 2450MHz, power 700W is added after butyl acrylate is sufficiently mixed, after standing 30min
Continue microwave treatment 3min, adds wurtzite BN and polymerization diamond nanoparticles stick, be then heated to 115-200 DEG C of heat preservation
15min is mixed, gained mixture is cooled with the speed of 10-15 DEG C/min, is kept the temperature and is stood after temperature is down to 35-40 DEG C
30min stands 3h then to 5-10 25 DEG C of warm water of part are added in mixture after being sufficiently mixed, be finally sent into freeze drier,
Powder is ground into after well-dried to get modifying agent.
Wherein dispersant includes：The raw material composition of following parts by weight：7-15 parts of Sorbitan Palmitate, polyoxyethylene-polyoxy
8-12 parts of propylene copolymer, 13-26 parts of ethylenediamine tetra-acetic acid, 80001-10 parts of macrogol, 2-20 parts of ethyl alcohol；Its preparation side
Method is：Sorbitan Palmitate is added in ethyl alcohol and is impregnated 1-8 hours, rear blender of being sent into fully dissolves stirring, adds after heating
Enter Pluronic F68, ethylenediamine tetra-acetic acid, macrogol 8000, add ethyl alcohol after precooling, startup is stirred
Device is mixed, 60-200rpm/min stirs 20min, afterwards up to dispersant after placement room temperature natural cooling.
Preferably, preparation method is as follows：
(1) reinforcing bar slag, vinyl pyrrolidone-vinyl acetate copolymer are added in 30% pitch, in blender
10-30min is kept the temperature after being sufficiently mixed when being heated to 40-50 DEG C, adds modifying agent, is continued heating and is uniformly mixed, stands cold
But to room temperature to get material I；
(2) 10-15% for taking above-mentioned octamethylcy-clotetrasiloxane weight, mixes with Diacetone Acrylamide, is passed through nitrogen,
Insulation reaction 2-3 hours at 90-95 DEG C, it is room temperature slowly to reduce temperature, obtains alkaline-sol；
(3) remaining octamethylcy-clotetrasiloxane, octyl benzene is added in the 10-15% for taking above-mentioned dimethylacetylamide weight
Basic ring tetrasiloxane, octaphenyl-POSS, stir evenly, are passed through nitrogen, and above-mentioned alkaline-sol is added, in 90-95 DEG C of insulated and stirred
30-40 minutes, stopping was passed through nitrogen, kept the temperature 2-3 hours, and it is 150-160 DEG C to increase temperature, keeps the temperature 27-30 minutes, cooling,
It is dried in vacuo 1-2 hours at 60-65 DEG C, obtains cross linking polysiloxane；
(4) above-mentioned pyromellitic acid anhydride is added in 36-40 times of its weight, 15-17% sulfuric acid solution, is added
The ammonium hydroxide of above-mentioned 20-25% stands 1-2 hours, and precipitation is washed with deionized water 3-4 times for filtering, and vacuum is dry at 60-70 DEG C
It is 4-5 hours dry, obtain refined phthalic anhydride；
(5) above-mentioned polyglyceryl fatty acid ester is added in the deionized water of 17-20 times of its weight, is stirred evenly, is added
Ammonium polyphosphate, it is 2-3 minutes ultrasonic, obtain polyglycerol fatty acid ammonium salt solution；
(6) above-mentioned refined phthalic anhydride, polyglycerol fatty acid ammonium, cross linking polysiloxane are mixed, benzotriazole, stirring is added
Uniformly, it is sent into ice-water bath, is passed through nitrogen, is stirred to react 2-3 hours, discharge, product is added in amide aqueous solution, room temperature
4-5 days are stood, filtering obtains precrosslink polyimides；
(7) above-mentioned aluminium nitride is added in N-Methyl pyrrolidone, it is 2-3 minutes ultrasonic, obtain aluminium nitride dispersion liquid；
(8) above-mentioned precrosslink polyimides and polyether Glycols, vinyl carboxylate are added in aluminium nitride dispersion liquid,
It is 20-30 minutes ultrasonic, above-mentioned polyether Glycols are added, stir evenly, filter, it is small that vacuum drying 3-5 at 76-80 DEG C will be deposited in
When, fine powder is worn into, is heated 6-7 hours, discharging cooling obtains cross-linking modified polyimides；
(9) by remaining pitch, concrete, silane, sea sand, cross-linking modified polyimides be added dispersant in, blender with
500-2000rpm/min is uniformly mixed, and remaining pitch is added while stirring, stands place 10-30min after mixing,
Up to material II；
(10) polyvinylbenzenesulfonic acid is added in material I and material II, 20-60min is stood after stirring evenly, is finally utilized
Sand mill is sanded into uniform, careful grain size powder, and powder exists with cream form；
(11) paste mixture is uniformly laid on road surface by paver, bituminous paving thickness in 0.5-6.0cm, after
It is firm with road roller by effecting HMA compaction.
The beneficial effects of the invention are as follows：
1, there are good high temperature resistant, anti-seismic design in the larger area of the temperature difference；
2, there are preferable rutting resistance, elasticity and good toughness；
3, the anti-fatigue ability on road surface is improved, especially there is good answer on big flow, the serious highway of overload
Change ability can reduce the permanent deformation on road surface；
4, cementitiousness is especially strong, can be obviously improved road surface and meet the tensile capacity after water, and significantly improve the steady of pitch
It is qualitative；
5 present invention are introduced in the strand of polyimides with hydrophobic Si-O-Si structures, pass through polyimides
To the shearing force of cross linking polysiloxane, polysiloxanes can be dispersed into smaller particle, polyamides can be uniformly coated on
The surface of imines particle, so as to improve its dispersing uniformity in mixing material；The cross linking polysiloxane of the present invention also has
There are good thermal stability and structural stability, improves the compatibility of mixing material；The present invention by precrosslink polyimides with
Aluminium nitride suspension mixes, and the mixed material of formation combines the respective advantage of polyimides and aluminium nitride, has high heat conduction, low
Expansion, the excellent performance such as high temperature resistant.
Specific implementation mode：
In order to make the technical means, the creative features, the aims and the efficiencies achieved by the present invention be easy to understand, tie below
Specific embodiment is closed, the present invention is further explained.
Embodiment 1：
A kind of heat resistance modified pitch of macromolecule and preparation method thereof, includes the raw material of following number：
95 parts of pitch, 13 parts of modifying agent, 15 parts of sea sand, 35 parts of concrete, 13 parts of silane, vinyl pyrrolidone-acetic acid
27 parts of ethenyl copolymer, 5 parts of polyether Glycols, 1 part of polyglyceryl fatty acid ester, 5 parts of octamethylcy-clotetrasiloxane, octaphenyl-
POSS5 parts, 30 parts of dimethylacetylamide, 3 parts of octyl phenyl cyclotetrasiloxane, 20-25% 4 parts of 5 parts of ammonium hydroxide, dispersant,
46 parts of pyromellitic dianhydride, 70 parts of N-Methyl pyrrolidone, 7 parts of aluminium nitride, 10 parts of reinforcing bar slag, 4 parts of vinyl carboxylate, benzene a pair of horses going side by side
0.5 part of triazole, 1.5 parts of Diacetone Acrylamide, 4 parts of polyvinylbenzenesulfonic acid, 5 parts of ammonium polyphosphate.
Wherein modifying agent includes：14 parts of vinyl-vinyl acetate copolymer, 17 parts of butyl acrylate, wurtzite-type nitridation
1.5 parts of boron, 0.7 part of polymerization diamond nanoparticles stick；Preparation method：Acrylic acid fourth is added into vinyl-vinyl acetate copolymer
Ester be sufficiently mixed after under microwave frequency 2450MHz, power 700W microwave treatment 5min, stand 30min after continue microwave treatment
3min adds wurtzite BN and polymerization diamond nanoparticles stick, is then heated to 115-200 DEG C of heat preservation mixing 15min, institute
It obtains mixture to cool with the speed of 10 DEG C/min, the heat preservation standing 30min after temperature is down to 35 DEG C, then in mixture
5 parts of 25 DEG C of warm water are added, 3h is stood after being sufficiently mixed, is finally sent into freeze drier, powder is ground into after well-dried,
Up to modifying agent.
Wherein dispersant includes：The raw material composition of following parts by weight：8 parts of Sorbitan Palmitate, PULLRONIC F68
0 part of copolymer 1,16 parts of ethylenediamine tetra-acetic acid, 80005 parts of macrogol, 12 parts of ethyl alcohol；Preparation method is：By palm mountain
Pears tanga, which enters in ethyl alcohol, to be impregnated 6 hours, and rear blender of being sent into fully dissolves stirring, and polyoxyethylene-polyoxy is added after heating
Propylene copolymer, ethylenediamine tetra-acetic acid, macrogol 8000 add ethyl alcohol after precooling, start agitating device, 200rpm/
Min stirs 20min, afterwards up to dispersant after placement room temperature natural cooling.
Preferably, preparation method is as follows：
(1) reinforcing bar slag, vinyl pyrrolidone-vinyl acetate copolymer are added in 30% pitch, in blender
15min is kept the temperature after being sufficiently mixed when being heated to 50 DEG C, adds modifying agent, continues heating and is uniformly mixed, standing is cooled to room
Temperature is to get material I；
(2) the 10% of above-mentioned octamethylcy-clotetrasiloxane weight is taken, is mixed with Diacetone Acrylamide, is passed through nitrogen,
Insulation reaction 3 hours at 95 DEG C, it is room temperature slowly to reduce temperature, obtains alkaline-sol；
(3) the 15% of above-mentioned dimethylacetylamide weight is taken, remaining octamethylcy-clotetrasiloxane, octyl phenyl ring is added
Tetrasiloxane, octaphenyl-POSS, stir evenly, are passed through nitrogen, and above-mentioned alkaline-sol is added, and in 95 DEG C of insulated and stirreds 30 minutes, stop
It is only passed through nitrogen, keeps the temperature 2-3 hours, it is 150 DEG C to increase temperature, keeps the temperature 30 minutes, cooling, is dried in vacuo 2 hours at 65 DEG C,
Obtain cross linking polysiloxane；
(4) above-mentioned pyromellitic acid anhydride is added in 40 times of its weight, 17% sulfuric acid solution, is added above-mentioned
20% ammonium hydroxide stands 2 hours, and precipitation is washed with deionized water 3 times, is dried in vacuo 5 hours, obtains refined at 65 DEG C by filtering
Phthalic anhydride；
(5) above-mentioned polyglyceryl fatty acid ester is added in the deionized water of 17 times of its weight, is stirred evenly, poly- phosphorus is added
Sour ammonium, ultrasound 3 minutes, obtains polyglycerol fatty acid ammonium salt solution；
(6) above-mentioned refined phthalic anhydride, polyglycerol fatty acid ammonium, cross linking polysiloxane are mixed, benzotriazole, stirring is added
Uniformly, it is sent into ice-water bath, is passed through nitrogen, is stirred to react 2 hours, discharge, product is added in amide aqueous solution, room temperature is quiet
It sets 4-5 days, filters, obtain precrosslink polyimides；
(7) above-mentioned aluminium nitride is added in N-Methyl pyrrolidone, ultrasound 3 minutes obtains aluminium nitride dispersion liquid；
(8) above-mentioned precrosslink polyimides and polyether Glycols, vinyl carboxylate are added in aluminium nitride dispersion liquid,
Ultrasound 30 minutes, is added above-mentioned polyether Glycols, stirs evenly, and filters, will be deposited at 76 DEG C and be dried in vacuo 3 hours, wear into
Fine powder heats 6 hours, and discharging cooling obtains cross-linking modified polyimides；
(9) by remaining pitch, concrete, silane, sea sand, cross-linking modified polyimides be added dispersant in, blender with
1000rpm/min is uniformly mixed, and remaining pitch is added while stirring, stands place 20min to get material after mixing
Ⅱ；
(10) polyvinylbenzenesulfonic acid is added in material I and material II, 30min is stood after stirring evenly, finally utilize sand
Grinding machine is sanded into uniform, careful grain size powder, and powder exists with cream form；
(11) paste mixture is uniformly laid on road surface by paver, bituminous paving thickness is in 4.0cm, rear pressure
Road machine is firm by effecting HMA compaction.
Embodiment 2：
A kind of heat resistance modified pitch of macromolecule and preparation method thereof, includes the raw material of following number：
86 parts of pitch, 13 parts of modifying agent, 16 parts of sea sand, 45 parts of concrete, 15 parts of silane, vinyl pyrrolidone-acetic acid
27 parts of ethenyl copolymer, 4 parts of polyether Glycols, 0.7 part of polyglyceryl fatty acid ester, 5 parts of octamethylcy-clotetrasiloxane, octaphenyl-
POSS2 parts, 30 parts of dimethylacetylamide, 2 parts of octyl phenyl cyclotetrasiloxane, 20-25% 5 parts of 4 parts of ammonium hydroxide, dispersant,
46 parts of pyromellitic dianhydride, 70 parts of N-Methyl pyrrolidone, 6 parts of aluminium nitride, 11 parts of reinforcing bar slag, 5 parts of vinyl carboxylate, benzene a pair of horses going side by side
0.6 part of triazole, 1 part of Diacetone Acrylamide, 5 parts of polyvinylbenzenesulfonic acid, 4 parts of ammonium polyphosphate.
Wherein modifying agent includes：14 parts of vinyl-vinyl acetate copolymer, 15 parts of butyl acrylate, wurtzite-type nitridation
1.5 parts of boron, 0.8 part of polymerization diamond nanoparticles stick；Preparation method：Acrylic acid fourth is added into vinyl-vinyl acetate copolymer
Ester be sufficiently mixed after under microwave frequency 2450MHz, power 700W microwave treatment 5min, stand 30min after continue microwave treatment
3min adds wurtzite BN and polymerization diamond nanoparticles stick, is then heated to 145 DEG C of heat preservation mixing 15min, and gained is mixed
Object is closed to cool with the speed of 12 DEG C/min, after temperature is down to 40 DEG C heat preservation stand 30min, then to being added in mixture
6 parts of 25 DEG C of warm water, stand 3h after being sufficiently mixed, finally be sent into freeze drier in, be ground into after well-dried powder to get
Modifying agent.
Wherein dispersant includes：The raw material composition of following parts by weight：15 parts of Sorbitan Palmitate, polyoxyethylene-polyoxy third
8 parts of alkene copolymer, 13 parts of ethylenediamine tetra-acetic acid, 80004 parts of macrogol, 10 parts of ethyl alcohol；Preparation method is：By palm mountain
Pears tanga, which enters in ethyl alcohol, to be impregnated 5 hours, and rear blender of being sent into fully dissolves stirring, and polyoxyethylene-polyoxy is added after heating
Propylene copolymer, ethylenediamine tetra-acetic acid, macrogol 8000 add ethyl alcohol after precooling, start agitating device, 200rpm/
Min stirs 20min, afterwards up to dispersant after placement room temperature natural cooling.
Preferably, preparation method is as follows：
(1) reinforcing bar slag, vinyl pyrrolidone-vinyl acetate copolymer are added in 30% pitch, in blender
15min is kept the temperature after being sufficiently mixed when being heated to 40 DEG C, adds modifying agent, continues heating and is uniformly mixed, standing is cooled to room
Temperature is to get material I；
(2) the 15% of above-mentioned octamethylcy-clotetrasiloxane weight is taken, is mixed with Diacetone Acrylamide, is passed through nitrogen,
Insulation reaction 2 hours at 90-95 DEG C, it is room temperature slowly to reduce temperature, obtains alkaline-sol；
(3) the 10% of above-mentioned dimethylacetylamide weight is taken, remaining octamethylcy-clotetrasiloxane, octyl phenyl ring is added
Tetrasiloxane, octaphenyl-POSS, stir evenly, are passed through nitrogen, and above-mentioned alkaline-sol is added, and in 95 DEG C of insulated and stirreds 40 minutes, stop
It is only passed through nitrogen, keeps the temperature 2 hours, it is 150 DEG C to increase temperature, keeps the temperature 27 minutes, cooling, is dried in vacuo 2 hours, obtains at 60 DEG C
Cross linking polysiloxane；
(4) above-mentioned pyromellitic acid anhydride is added in 36 times of its weight, 15% sulfuric acid solution, is added above-mentioned
20% ammonium hydroxide stands 2 hours, and precipitation is washed with deionized water 3 times, is dried in vacuo 4 hours, obtains refined at 60 DEG C by filtering
Phthalic anhydride；
(5) above-mentioned polyglyceryl fatty acid ester is added in the deionized water of 17 times of its weight, is stirred evenly, poly- phosphorus is added
Sour ammonium, ultrasound 3 minutes, obtains polyglycerol fatty acid ammonium salt solution；
(6) above-mentioned refined phthalic anhydride, polyglycerol fatty acid ammonium, cross linking polysiloxane are mixed, benzotriazole, stirring is added
Uniformly, it is sent into ice-water bath, is passed through nitrogen, is stirred to react 3 hours, discharge, product is added in amide aqueous solution, room temperature is quiet
It sets 4 days, filters, obtain precrosslink polyimides；
(7) above-mentioned aluminium nitride is added in N-Methyl pyrrolidone, ultrasound 3 minutes obtains aluminium nitride dispersion liquid；
(8) above-mentioned precrosslink polyimides and polyether Glycols, vinyl carboxylate are added in aluminium nitride dispersion liquid,
Ultrasound 20 minutes, is added above-mentioned polyether Glycols, stirs evenly, and filters, will be deposited at 76 DEG C and be dried in vacuo 3 hours, wear into
Fine powder heats 6 hours, and discharging cooling obtains cross-linking modified polyimides；
(9) by remaining pitch, concrete, silane, sea sand, cross-linking modified polyimides be added dispersant in, blender with
1500rpm/min is uniformly mixed, and remaining pitch is added while stirring, stands place 20min to get material after mixing
Ⅱ；
(10) polyvinylbenzenesulfonic acid is added in material I and material II, 35min is stood after stirring evenly, finally utilize sand
Grinding machine is sanded into uniform, careful grain size powder, and powder exists with cream form；
(11) paste mixture is uniformly laid on road surface by paver, bituminous paving thickness is in 3.5cm, rear pressure
Road machine is firm by effecting HMA compaction.
It is to carrying out experiment investigation respectively in embodiment provided by the invention, embodiment 1 and 2 made macromolecule of embodiment is resistance to
Heat modification pitch is tested for the property, and the results are shown in Table 1.
The performance test results of the heat resistance modified pitch of 1 macromolecule of table
It is obtained by the above testing result：The performance detection index of the heat resistance modified pitch of macromolecule is better than plain asphalt index,
And when applied to road pavement road surface, there are good high temperature resistant, anti-seismic design；Have a preferable rutting resistance, elasticity and
Good toughness；The anti-fatigue ability on road surface is improved, especially there is good strain energy on big flow, the serious highway of overload
Power can reduce the permanent deformation on road surface；Cementitiousness is especially strong, hence it is evident that improves road surface and meets the tensile capacity after water, and greatly
Improve the stability of pitch.
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (2)
1. a kind of heat resistance modified pitch of macromolecule, it is characterised in that：The heat resistance modified pitch of macromolecule includes the raw material of following number：
59-100 parts of pitch, 11-23 parts of modifying agent, 13-25 parts of sea sand, 35-55 parts of concrete, 13-21 parts of silane, vinylpyridine
Pyrrolidone -24-57 parts of vinyl acetate copolymer, 2-5 parts of polyether Glycols, 0.7-1 parts of polyglyceryl fatty acid ester, prestox ring four
5-7 parts of siloxanes ,-POSS2-5 parts of octaphenyl, 30-40 parts of dimethylacetylamide, 1-3 parts of octyl phenyl cyclotetrasiloxane, 20-
25% 2-6 parts of ammonium hydroxide, 46-50 parts of pyromellitic acid anhydride, 70-80 parts of N-Methyl pyrrolidone, nitrogenizes 3-7 parts of dispersant
3-7 parts of aluminium, 10-14 parts of reinforcing bar slag, 3-7 parts of vinyl carboxylate, 0.4-1 parts of benzotriazole, Diacetone Acrylamide 1-1.7
Part, 2-8 parts of polyvinylbenzenesulfonic acid, 2-6 parts of ammonium polyphosphate.
2. the heat resistance modified pitch of macromolecule according to claim 1, it is characterised in that：It is prepared by the heat resistance modified pitch of macromolecule
Method is as follows：
(1) reinforcing bar slag, vinyl pyrrolidone-vinyl acetate copolymer are added in 30% pitch, side adds in blender
Heat keeps the temperature 10-30min after being sufficiently mixed to 40-50 DEG C of side, adds modifying agent, continues heating and is uniformly mixed, standing is cooled to
Room temperature is to get material I；
(2) 10-15% for taking above-mentioned octamethylcy-clotetrasiloxane weight, mixes with Diacetone Acrylamide, is passed through nitrogen,
Insulation reaction 2-3 hours at 90-95 DEG C, it is room temperature slowly to reduce temperature, obtains alkaline-sol；
(3) remaining octamethylcy-clotetrasiloxane, octyl phenyl ring is added in the 10-15% for taking above-mentioned dimethylacetylamide weight
Tetrasiloxane, octaphenyl-POSS, stir evenly, are passed through nitrogen, and above-mentioned alkaline-sol is added, in 90-95 DEG C of insulated and stirred 30-40
Minute, stopping is passed through nitrogen, keeps the temperature 2-3 hours, and it is 150-160 DEG C to increase temperature, keeps the temperature 27-30 minutes, cooling, in 60-65
It is dried in vacuo 1-2 hours at DEG C, obtains cross linking polysiloxane；
(4) above-mentioned pyromellitic acid anhydride is added in 36-40 times of its weight, 15-17% sulfuric acid solution, is added above-mentioned
The ammonium hydroxide of 20-25% stands 1-2 hours, and precipitation is washed with deionized water 3-4 times, 4-5 is dried in vacuo at 60-70 DEG C by filtering
Hour, obtain refined phthalic anhydride；
(5) above-mentioned polyglyceryl fatty acid ester is added in the deionized water of 17-20 times of its weight, is stirred evenly, poly- phosphorus is added
Sour ammonium, it is 2-3 minutes ultrasonic, obtain polyglycerol fatty acid ammonium salt solution；
(6) above-mentioned refined phthalic anhydride, polyglycerol fatty acid ammonium, cross linking polysiloxane are mixed, benzotriazole is added, stirring is equal
It is even, it is sent into ice-water bath, is passed through nitrogen, is stirred to react 2-3 hours, discharge, product is added in amide aqueous solution, room temperature is quiet
It sets 4-5 days, filters, obtain precrosslink polyimides；
(7) above-mentioned aluminium nitride is added in N-Methyl pyrrolidone, it is 2-3 minutes ultrasonic, obtain aluminium nitride dispersion liquid；
(8) above-mentioned precrosslink polyimides and polyether Glycols, vinyl carboxylate are added in aluminium nitride dispersion liquid, ultrasound
20-30 minutes, above-mentioned polyether Glycols are added, stir evenly, filters, will be deposited at 76-80 DEG C and be dried in vacuo 3-5 hours,
Fine powder is worn into, is heated 6-7 hours, discharging cooling obtains cross-linking modified polyimides；
(9) remaining pitch, concrete, silane, sea sand, cross-linking modified polyimides are added in dispersant, blender is with 500-
2000rpm/min is uniformly mixed, and remaining pitch is added while stirring, stand after mixing place 10-30min to get
Material II；
(10) polyvinylbenzenesulfonic acid is added in material I and material II, 20-60min is stood after stirring evenly, finally utilize sand milling
Machine is sanded into uniform, careful grain size powder, and powder exists with cream form；
(11) paste mixture is uniformly laid on road surface by paver, bituminous paving thickness is in 0.5-6.0cm, rear pressure
Road machine is firm by effecting HMA compaction.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109970979A (en) * | 2019-04-02 | 2019-07-05 | 中国水利水电科学研究院 | A kind of siloxy group bituminous concrete antistripping agent and preparation method thereof |
| CN110540853A (en) * | 2019-08-12 | 2019-12-06 | 中国科学院山西煤炭化学研究所 | Method for preparing spinnable asphalt from pyromellitic dianhydride and polystyrene modified coal pitch |
| CN110684206A (en) * | 2019-11-27 | 2020-01-14 | 上海海事大学 | Preparation method of asphalt modified emulsified asphalt without sticking wheel rock |
| CN115572543A (en) * | 2022-09-30 | 2023-01-06 | 中建材苏州防水研究院有限公司 | Non-cured asphalt waterproof coating and preparation method and application thereof |
| CN116143463A (en) * | 2023-03-04 | 2023-05-23 | 四川精益达工程检测有限责任公司 | Reactive powder concrete and preparation process thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106084396A (en) * | 2016-06-22 | 2016-11-09 | 安徽电信器材贸易工业有限责任公司 | A kind of macromolecule heat-resistant cable material and preparation method thereof |
| CN106995612A (en) * | 2017-05-08 | 2017-08-01 | 安徽海德石油化工有限公司 | A kind of modified pitch |
-
2018
- 2018-02-11 CN CN201810142353.3A patent/CN108485288A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106084396A (en) * | 2016-06-22 | 2016-11-09 | 安徽电信器材贸易工业有限责任公司 | A kind of macromolecule heat-resistant cable material and preparation method thereof |
| CN106995612A (en) * | 2017-05-08 | 2017-08-01 | 安徽海德石油化工有限公司 | A kind of modified pitch |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109970979A (en) * | 2019-04-02 | 2019-07-05 | 中国水利水电科学研究院 | A kind of siloxy group bituminous concrete antistripping agent and preparation method thereof |
| CN110540853A (en) * | 2019-08-12 | 2019-12-06 | 中国科学院山西煤炭化学研究所 | Method for preparing spinnable asphalt from pyromellitic dianhydride and polystyrene modified coal pitch |
| CN110540853B (en) * | 2019-08-12 | 2021-03-26 | 中国科学院山西煤炭化学研究所 | Method for preparing spinnable asphalt from pyromellitic dianhydride and polystyrene modified coal pitch |
| CN110684206A (en) * | 2019-11-27 | 2020-01-14 | 上海海事大学 | Preparation method of asphalt modified emulsified asphalt without sticking wheel rock |
| CN110684206B (en) * | 2019-11-27 | 2022-07-01 | 上海海事大学 | Preparation method of asphalt modified emulsified asphalt without sticking wheel rock |
| CN115572543A (en) * | 2022-09-30 | 2023-01-06 | 中建材苏州防水研究院有限公司 | Non-cured asphalt waterproof coating and preparation method and application thereof |
| CN115572543B (en) * | 2022-09-30 | 2023-11-07 | 中建材苏州防水研究院有限公司 | Non-cured asphalt waterproof paint and preparation method and application thereof |
| CN116143463A (en) * | 2023-03-04 | 2023-05-23 | 四川精益达工程检测有限责任公司 | Reactive powder concrete and preparation process thereof |
| CN116143463B (en) * | 2023-03-04 | 2024-08-09 | 四川精益达工程检测有限责任公司 | Reactive powder concrete and preparation process thereof |
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