CN107739339A - A kind of difunctional asphalt emulsifier and preparation method thereof - Google Patents
A kind of difunctional asphalt emulsifier and preparation method thereof Download PDFInfo
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- CN107739339A CN107739339A CN201711174314.3A CN201711174314A CN107739339A CN 107739339 A CN107739339 A CN 107739339A CN 201711174314 A CN201711174314 A CN 201711174314A CN 107739339 A CN107739339 A CN 107739339A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D233/00—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings
- C07D233/04—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member
- C07D233/06—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, directly attached to ring carbon atoms
- C07D233/08—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, directly attached to ring carbon atoms with alkyl radicals, containing more than four carbon atoms, directly attached to ring carbon atoms
- C07D233/12—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, directly attached to ring carbon atoms with alkyl radicals, containing more than four carbon atoms, directly attached to ring carbon atoms with substituted hydrocarbon radicals attached to ring nitrogen atoms
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
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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
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
- C23F11/08—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
- C23F11/10—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids using organic inhibitors
- C23F11/14—Nitrogen-containing compounds
- C23F11/149—Heterocyclic compounds containing nitrogen as hetero atom
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2395/00—Bituminous materials, e.g. asphalt, tar or pitch
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- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
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Abstract
The present invention relates to a kind of difunctional asphalt emulsifier and preparation method thereof with emulsification and corrosion inhibition, is that basic component is made in raw material first using organic polyamine, organic acid, then by mol ratio is 1:1~1.3:1 ~ 1.3 basic component, acidic components and organic aldehyde carries out reaction and the difunctional asphalt emulsifier with emulsification and corrosion inhibition is made.The difunctional asphalt emulsifier preparation method is simple; product property is stable; there is good emulsifying capacity to different pitches; contain multiple adsorption sites that suction-operated can be produced with metal surface in emulsifier molecules structure; absorption diaphragm can be formed in metal surface; delay corrosion rate; it is substantially reducing at the corrosion of acid medium in cationic emulsified bitumen production process to emulsifying, storing, conveying, the equipment such as measure; available for preparing cationic emulsified bitumen, particularly micro-surface area, slurry seal emulsified asphalt.
Description
Technical field
The present invention relates to a kind of asphalt emulsifier and preparation method thereof, has emulsification and inhibition more specifically to one kind
Difunctional asphalt emulsifier of performance and preparation method thereof.
Background technology
Traditional heated bitumen road construction technique needs pitch being heated to 160~180 DEG C, make its viscosity be down to compared with
It could carry out mixing and stirring construction with gathering materials after good mobility.In addition, gathering materials also needs to be heated to certain temperature.Due in work progress
In, pitch heat time length, temperature are high, are also easy to produce poisonous and hazardous bitumen flue gas, pitch also has certain problem of aging.Cause
This, there is the shortcomings of high energy consumption, pollution is big, construction seasons are short in traditional heated bitumen technique.Emulsified asphalt can be solved preferably
Problem above, it can construct at normal temperatures, energy consumption is low, and pollution is small, in the development and application of pavement construction and other engineering constructions, table
Good economy, environmental and social benefits are revealed.
Emulsified asphalt originate in as the application of pavement material in the 1930s, by a nearly century research and open
Hair, its type and application field have obtained tremendous development, and emulsified asphalt technology has become the most important hand of road maintenance at present
One of section.In emulsified asphalt development course, core technology of the asphalt emulsifier as production emulsified asphalt, its classification is from initial
Anionic, progressively develop into cationic, nonionic and amphoteric ion type of today etc., its cationic pitch breast
For agent due to the emulsified asphalt that it is prepared and stone surface strong adsorption force, antistrip performance is good, is widely used in micro-surface area, thin pulp
The road maintenance engineerings such as sealing, crushed stone sealing, sticking layer oil, penetration type road surface.
Now widely used cationic asphalt emulsifier, generally need to adjust emulsifier aqueous solution pH value when in use
Save to acidity, such as Li Wenhong [study on the synthesis [J] stones of Li Wenhong, Wang Wei weeks .SM type positive ion imidazoline asphalt emulsifiers
Oiling work, 1995 (5):328-330.] utilize by-product aliphatic acid with diethylenetriamine through being dehydrated addition, cyclisation and quaternized three step
Reaction is prepared for a kind of positive ion imidazoline asphalt emulsifier, need to adjust pH value to 2.5~5.5 during use.
[Li Li, Zhang Chenghong, the poplar Guo, when waiting synthesis and emulsifiability research [J] chemical industry of asphalt emulsifiers such as Li Li
Periodical, 2006,20 (8):40-41] using aphthenic acids, ethylenediamine as raw material, reacted at 160 DEG C in nitrogen, then increase the temperature to 245
Midbody compound imidazoline is obtained after DEG C, and quaterisation is carried out to it with dimethyl suflfate and obtains quaternary ammonium salt cationic
Imidazoline asphalt emulsifier.PH value need to be adjusted to 3~4 by the optimum emulsification condition of the asphalt emulsifier.
Pretty grade is opened [Zhang Qian, Zhang Tong, Wang Yuexin, to wait to split the synthesis of solidifying type cation asphalt emulgent and its performance soon slowly and grind
Study carefully [J] daily chemical industries, 2012,42 (6):432-435] with NPE, epoxychloropropane and trimethylamine
The polyoxyethylene-type cation asphalt emulgent N- [2- hydroxyl -3- NPEs (15)] third for main Material synthesis
Base trimethyl ammonium chloride, the optimum condition for preparing emulsified asphalt are oil-water ratio 6:4, emulsifier is the 3.0% of asphalt quality,
Emulsifier aqueous solution pH value is 1~2.
Wang Dongmei etc. [Wang Dongmei, An Lei, Zhang Jianzhong, waits a kind of synthesis and application of amide-type cation asphalt emulgent
[J] petrochemical industry Journal of Chinese Universities, 2015,28 (1):16-19] use stearic acid, melon seeds fatty acid oil and triethylene tetramine
A kind of synthetically prepared mixing acid amide type cation asphalt emulgent, passes through emulsified asphalt performance test and road construction, the breast
Agent has that emulsifying capacity is strong, the relatively little of feature of emulsifier.The acid amide type cation asphalt emulgent needs when in use
Emulsifier aqueous solution pH value is adjusted to 2.0.
Publication No. CN106633102A Chinese invention patent discloses a kind of system of composite cation asphalt emulsifier
Preparation Method, the invention prepare glucosides concentrate using vegetable seed degreasing enzyme deactivation and extracting, then by glucosides concentrate and epoxychloropropane
It is placed in stir in beaker with sulfuric acid and collects filtrate after the heating, be prepared into chloro glucosides, master is used as by the chloro glucosides of preparation
Body, improve the stability of emulsifying agent, be then placed in benzoyl peroxide and epoxidized soybean oil etc. in three-necked flask, stir simultaneously plus
Composite cation asphalt emulsifier is prepared after heat.The composite cation asphalt emulsifier needs pH with hydrochloric acid when in use
Value is adjusted to 2~6.
Chinese invention patent (publication number CN105968386A) discloses a kind of cation containing steric hindrance and splits fast coagulate slowly
Type asphalt emulsifier, the invention are to meet that slurry seal splits requirement solidifying soon slowly, increase steric hindrance in the hydrophilic cardinal extremity of emulsifying agent,
Delay demulsification process.The emulsifying agent needs to adjust when in use pH value to 2~6.
Yao Yan etc. [Yao Yan, Zhai Zhe, Kong Xiangjun, waits that there is the synthesis of corrosion inhibitive function cation asphalt emulgent and performance to grind
Study carefully [J] Speciality Petrochemicals, 2016,33 (6):33-38] synthesize a kind of cationic asphalt emulsification with corrosion inhibitive function
Agent, the emulsifying agent obtain chain alkyl imidazoles, then with two first using laurate, TEPA as raw material through two-step reaction
Butylamine, epoxychloropropane are raw material, and absolute ethyl alcohol is solvent, stirring reaction 10 hours, is dried in vacuo 8~10 hours, obtains N-
Butyl-N, N- bis- (the chloro- 2- hydroxypropyls of 3-) butane -1- ammonium salts, then 12 are reacted in isopropanol solvent with chain alkyl imidazoline
Hour, obtain final product after solvent is evaporated off.The emulsifying agent has certain corrosion inhibitive function, is in 80 DEG C of corrosion temperature, pH values
2.0th, under the etching time etching condition of 4 hours, corrosion inhibition rate 91.62%.But the emulsifying agent preparation process is complicated, during reaction
Between it is long, cost is high, and corrosion inhibition is general.
Horse tinkling of pieces of jade etc. [Ma Ling, Li Lei, Kong Xiangjun, waits the preparation of .NE-6 cation asphalt emulgents and its grinding for Inhibitive behaviour
Study carefully [J] asphalt, 2011,25 (2):27-29] the NE-6 cationic asphalts breast using aphthenic acids, ethyleneamines as Material synthesis
Agent, the emulsifying agent have certain corrosion inhibitive function in aqueous.But the emulsifier molecules are in the adsorption potential of metal surface
Put single, and raw material aphthenic acids source and quality are unstable, and the emulsification of asphalt emulsifier product and rust inhibition can ensure.
In summary, cation asphalt emulgent is when in use generally by the pH value of emulsifier aqueous solution with hydrochloric acid, second
The pH value regulators such as acid are adjusted to 1~6, and therefore, in emulsified asphalt production process, emulsifier aqueous solution prepares holding vessel, colloid
Grinding the equipment such as bistrique, delivery pump and pipeline, emulsified asphalt storage tank, paver, flowmeter can all be exposed in acidic corrosive media,
Particularly when emulsifier aqueous solution is prepared, solution local location pH value mistake is easily caused during adding pH value conditioning agents
It is low, acid concentration is too high and causes severe local corrosion, bring potential safety hazard to emulsified asphalt production unit.Although in the prior art
The cation asphalt emulgent with certain corrosion inhibition can be used in process of production, but the building-up process of emulsifying agent is answered
Miscellaneous, production cycle length, cost is high, and corrosion inhibition is general, and raw material sources and quality are unstable.
The content of the invention
For in the prior art the defects of, an object of the present invention is to provide a kind of difunctional asphalt emulsifier, the breast
Agent also has corrosion inhibitive function concurrently while with good emulsifying capacity, contains multiple adsorption potentials in molecule, can be in metal surface
Absorption diaphragm is formed, avoids acid corrosion medium from directly being contacted with production equipment, delays corrosion rate, substantially reduce prior art
Present in Corrosion Potential.
The second object of the present invention is to provide a kind of preparation method of difunctional asphalt emulsifier, and the emulsifying agent is with organic more
Amine, organic acid are the obtained basic component of raw material, then basic component and acidic components and organic aldehyde react being made to have and delayed
Corrosion can asphalt emulsifier, without in emulsifying agent compound corrosion inhibitor composition i.e. there is corrosion inhibitive function.The synthesis of the emulsifying agent
Raw material sources are stable, and preparation method is simple, and product property is stable, and inhibition and emulsifiability are excellent.
One of technical scheme provided by the invention is to provide a kind of difunctional asphalt emulsification with emulsification and corrosion inhibition
Agent, it is characterised in that its general structure is (I)：
Wherein R1Expression-CnH2n-1Alkyl side chain, n is integer and 9≤n≤17；
-(CH2CH2NH)x- it is ethyleneamines chain, x=0,1,2,3,4；
R2ForDeng one kind in substituent.
The two of technical scheme provided by the invention are to provide a kind of preparation method of difunctional asphalt emulsifier, including as follows
Step：
1) preparation of basic component：Using mol ratio as 1:1~1.5 long chain organic acid and organic polyamine are reaction raw materials,
The solvent for accounting for 20~50wt% of reaction raw materials gross weight is added, stirring is warming up to 140~180 DEG C, and steady temperature reaction 2~4 is small
When, temperature of reaction system is then raised to 220~260 DEG C, it is 0.090-0.096MPa that vacuum is evacuated to after desolvation,
Continue reaction 2~6 hours, temperature obtains basic component after being down to 70~90 DEG C；
2) will be 1 with basic component mol ratio:1~1.3:1~1.3 acidic components and organic aldehyde are formulated as 60~
90wt% ethanol solution, add catalyst and adjust pH value to 2~6, be slowly added dropwise to the basic component obtained by step 1)
In, after being added dropwise under the conditions of 80~110 DEG C stirring reaction 1~3 hour, obtain difunctional asphalt emulsifier.
Described preferred processing condition is：Long chain organic acid is 1 with organic polyamine mol ratio:1~1.3, addition accounts for reaction
30~40wt% of raw material gross weight solvent, stirring are warming up to 160~170 DEG C, and steady temperature reacts 2.5~3.5 hours, then
Temperature of reaction system is raised under vacuum to 240~250 DEG C, continues reaction 3~5 hours, desolvation and generation
Water, basic component is obtained, after cooling the temperature to 80~85 DEG C, it is 1 to add with basic component mol ratio:1~1.2:1~1.3
Acidic components and organic aldehyde, system pH is adjusted to 2~4, stirring reaction 2~3 hours under the conditions of 90~100 DEG C, obtained double
Function asphalt emulsifier.
Described long chain organic acid is the linear saturated fatty acids that carbon chain lengths are 10~18.Described organic polyamine is second
One kind in diamines, diethylenetriamine, triethylene tetramine, TEPA, pentaethylene hexamine.
Described acidic components are one kind in acetophenone, cyclohexanone, phenol and cresols.
Described organic aldehyde is formaldehyde, formalin or the polyformaldehyde that can dissociate formaldehyde.
Described solvent is one kind in toluene, meta-xylene, ortho-xylene, paraxylene, Mixed XYLENE.
Described catalyst is one kind in hydrochloric acid, formic acid, acetic acid, phosphoric acid.
The present invention uses the asphalt emulsifier obtained by above technical scheme, special available for preparing cationic emulsified bitumen
It is not micro-surface area, slurry seal emulsified asphalt.It is compared with the prior art, the beneficial effects of the invention are as follows：
The innovative point of the present invention is the molecular structure of difunctional asphalt emulsifier, be designed to have it is multiple can be with gold
Metal surface produces the adsorption site of suction-operated, and multiple N atoms with lone pair electrons, Yi Yutie are contained such as in basic component
Atom forms coordinate bond and produces suction-operated, changes the state of charge of metal surface；To further enhance corrosion inhibition, select
Reacted containing phenyl ring, the isostructural acidic components of hexamethylene and basic component so that contain pi-electron in product molecule structure, can
Coordination is occurred by coordinate bond with the dsp tracks with iron atom hydridization, generates the stable chelate with cyclic structure
Absorption is in metal surface, the complete absorption diaphragm of formation.The presence of above-mentioned multiple adsorption sites, ensure that emulsifier,
The difunctional realization of inhibition.
The advantages of difunctional asphalt emulsifier of the present invention, is：The raw material sources for preparing the asphalt emulsifier are extensive
It is easy to get, there is good emulsifying capacity to different pitches, and have excellent corrosion inhibition concurrently, to metal in sour corrosion system
With corrosion inhibition, acid medium is substantially reduced in emulsified asphalt production process to emulsifying, storing, conveying, the equipment such as measuring
Corrosion, delay corrosion rate, substantially reduce Corrosion Potential present in prior art.
Embodiment
With reference to specific embodiment, the present invention is further elaborated, but the present invention is not limited to following examples.Institute
It is conventional method unless otherwise instructed to state method.The raw material can obtain from open commercial sources unless otherwise instructed.
Embodiment 1
It is 1 by mol ratio:1 capric acid is with triethylene tetramine input reactor, adding and accounting for reaction raw materials gross weight
30wt% toluene, reaction system is warming up to 150 DEG C after stirring, isothermal reaction 3.0 hours, then raises reaction system
For temperature to 240 DEG C, it is 0.090MPa that vacuum is evacuated to after desolvation, continues reaction 4.0 hours, after temperature is down to 75 DEG C
Obtain basic component；
To be 1 with basic component mol ratio:1:1 acetophenone and formaldehyde are formulated as 70wt% ethanol solution, add salt
Acid simultaneously adjusts pH value to 2.0, and above-mentioned solution is slowly added dropwise into basic component, stirred instead under the conditions of 90 DEG C after being added dropwise
Answer 2.0 hours, obtain difunctional asphalt emulsifier.
Emulsifiability test is carried out to difunctional asphalt emulsifier obtained above：The difunctional asphalt emulsifier is prepared
To account for the emulsified asphalt gross mass 1.5wt% aqueous solution, with salt acid for adjusting pH value to 2.0, colloid mill is poured into after being heated to 55 DEG C
In, after starting colloid mill, the AH-90 matrix pitches that temperature is 130 DEG C are at the uniform velocity added and fully sheared, obtain bitumen content
For 60wt% emulsified asphalt.After tested, emulsified asphalt is cationic, and volume average particle sizes are 2.6 μm, 1 day and 5 days of storage
It is respectively 0.5% and 2.7% to deposit stability, and surplus is 0.02% on sieve.
Corrosion inhibition test is carried out to difunctional asphalt emulsifier obtained above：With reference to People's Republic of China's oil day
Right gas professional standard SY/T5405-1996, the difunctional asphalt emulsifier is formulated as the 1.5wt% aqueous solution, adjusted with hydrochloric acid
PH value is saved to 2.0, after being heated to 90 DEG C, N80 corrosion coupons are positioned in solution 4.0 hours, corrosion is weighed after taking out test piece
For front and rear weightlessness to calculate corrosion rate, it is final result to take the average value tested three times, is calculated as a comparison with blank test slow
Erosion rate.The corrosion rate that wherein blank test measures is 28.39g.m-2.h-1, the corrosion rate that inhibition qualification test measures is
0.28g.m-2.h-1, corrosion inhibition rate 99.01%.
Embodiment 2
It is 1 by mol ratio:1.2 hexadecylic acid is with TEPA input reactor, adding and accounting for reaction raw materials gross weight
35wt% toluene, reaction system is warming up to 160 DEG C after stirring, isothermal reaction 4.0 hours, then raises reaction system
For temperature to 235 DEG C, it is 0.092MPa that vacuum is evacuated to after desolvation, continues reaction 4.5 hours, after temperature is down to 75 DEG C
Obtain basic component；
To be 1 with basic component mol ratio:1.1:1.1 cyclohexanone and formaldehyde are formulated as 80wt% ethanol solution, add
Enter acetic acid and adjust pH value to 4.0, above-mentioned solution is slowly added dropwise into basic component, after being added dropwise under the conditions of 95 DEG C
Stirring reaction 2.5 hours, obtains difunctional asphalt emulsifier.
Emulsifiability test is carried out to difunctional asphalt emulsifier obtained above：The difunctional asphalt emulsifier is prepared
To account for the emulsified asphalt gross mass 1.5wt% aqueous solution, with salt acid for adjusting pH value to 2.0, colloid mill is poured into after being heated to 55 DEG C
In, after starting colloid mill, the AH-90 matrix pitches that temperature is 130 DEG C are at the uniform velocity added and fully sheared, obtain bitumen content
For 60wt% emulsified asphalt.After tested, emulsified asphalt is cationic, and volume average particle sizes are 2.8 μm, 1 day and 5 days of storage
It is respectively 0.67% and 3.43% to deposit stability, and surplus is 0.04% on sieve.
Corrosion inhibition test is carried out to difunctional asphalt emulsifier obtained above：With reference to People's Republic of China's oil day
Right gas professional standard SY/T5405-1996, the difunctional asphalt emulsifier is formulated as the 1.5wt% aqueous solution, adjusted with hydrochloric acid
PH value is saved to 2.0, after being heated to 90 DEG C, N80 corrosion coupons are positioned in solution 4.0 hours, corrosion is weighed after taking out test piece
For front and rear weightlessness to calculate corrosion rate, it is final result to take the average value tested three times, is calculated as a comparison with blank test slow
Erosion rate.The corrosion rate that inhibition qualification test measures is 0.45g.m-2.h-1, corrosion inhibition rate 98.41%.
Embodiment 3
It is 1 by mol ratio:1.5 laurate is with ethylenediamine input reactor, adding and accounting for reaction raw materials gross weight
40wt% Mixed XYLENE, reaction system is warming up to 140 DEG C after stirring, isothermal reaction 2.5 hours, then rise is reacted
For system temperature to 230 DEG C, it is 0.096MPa that vacuum is evacuated to after desolvation, continues reaction 5.0 hours, temperature is down to 80
Basic component is obtained after DEG C；
To be 1 with basic component mol ratio:1.2:1.2 acetophenone and metaformaldehyde (equivalent of formaldehyde) is formulated as 85wt%
Ethanol solution, add formic acid simultaneously adjust pH value to 3.0, above-mentioned solution is slowly added dropwise into basic component, after being added dropwise
Stirring reaction 3.0 hours under the conditions of 80 DEG C, obtain difunctional asphalt emulsifier.
Emulsifiability test is carried out to difunctional asphalt emulsifier obtained above：The difunctional asphalt emulsifier is prepared
To account for the emulsified asphalt gross mass 1.5wt% aqueous solution, with salt acid for adjusting pH value to 2.0, colloid mill is poured into after being heated to 55 DEG C
In, after starting colloid mill, the AH-90 matrix pitches that temperature is 130 DEG C are at the uniform velocity added and fully sheared, obtain bitumen content
For 60wt% emulsified asphalt.After tested, emulsified asphalt is cationic, and volume average particle sizes are 2.4 μm, 1 day and 5 days of storage
It is respectively 0.35% and 2.98% to deposit stability, and surplus is 0.03% on sieve.
Corrosion inhibition test is carried out to difunctional asphalt emulsifier obtained above：With reference to People's Republic of China's oil day
Right gas professional standard SY/T5405-1996, the difunctional asphalt emulsifier is formulated as the 1.5wt% aqueous solution, adjusted with hydrochloric acid
PH value is saved to 2.0, after being heated to 90 DEG C, N80 corrosion coupons are positioned in solution 4 hours, before weighing corrosion after taking-up test piece
For weightlessness to calculate corrosion rate, it is final result to take the average value tested three times, and inhibition is calculated as a comparison with blank test afterwards
Rate.The corrosion rate that inhibition qualification test measures is 0.36g.m-2.h-1, corrosion inhibition rate 98.73%.
Embodiment 4
It is 1 by mol ratio:1.1 stearic acid is with pentaethylene hexamine input reactor, adding and accounting for reaction raw materials gross weight
45wt% Mixed XYLENE, reaction system is warming up to 180 DEG C after stirring, isothermal reaction 2.0 hours, then rise is reacted
For system temperature to 220 DEG C, it is 0.093MPa that vacuum is evacuated to after desolvation, continues reaction 6.0 hours, temperature is down to 70
Basic component is obtained after DEG C；
To be 1 with basic component mol ratio:1:1 phenol and formaldehyde are formulated as 60wt% ethanol solution, add phosphoric acid
And adjust pH value to 5.0, above-mentioned solution is slowly added dropwise into basic component, after being added dropwise under the conditions of 85 DEG C stirring reaction
1.5 hours, obtain difunctional asphalt emulsifier.
Emulsifiability test is carried out to difunctional asphalt emulsifier obtained above：The difunctional asphalt emulsifier is prepared
To account for the emulsified asphalt gross mass 1.5wt% aqueous solution, with salt acid for adjusting pH value to 2.0, colloid mill is poured into after being heated to 55 DEG C
In, after starting colloid mill, the AH-90 matrix pitches that temperature is 130 DEG C are at the uniform velocity added and fully sheared, obtain bitumen content
For 60wt% emulsified asphalt.After tested, emulsified asphalt is cationic, and volume average particle sizes are 3.1 μm, 1 day and 5 days of storage
It is respectively 0.55% and 3.64% to deposit stability, and surplus is 0.06% on sieve.
Corrosion inhibition test is carried out to difunctional asphalt emulsifier obtained above：With reference to People's Republic of China's oil day
Right gas professional standard SY/T5405-1996, the difunctional asphalt emulsifier is formulated as the 1.5wt% aqueous solution, adjusted with hydrochloric acid
PH value is saved to 2.0, after being heated to 90 DEG C, N80 corrosion coupons are positioned in solution 4.0 hours, corrosion is weighed after taking out test piece
For front and rear weightlessness to calculate corrosion rate, it is final result to take the average value tested three times, is calculated as a comparison with blank test slow
Erosion rate.The corrosion rate that inhibition qualification test measures is 0.32g.m-2.h-1, corrosion inhibition rate 98.87%.
Embodiment 5
It is 1 by mol ratio:1.3 tetradecylic acid is with diethylenetriamine input reactor, adding and accounting for reaction raw materials gross weight
50wt% paraxylene, reaction system is warming up to 170 DEG C after stirring, isothermal reaction 3.5 hours, then rise is reacted
For system temperature to 225 DEG C, it is 0.091MPa that vacuum is evacuated to after desolvation, continues reaction 5.5 hours, temperature is down to 75
Basic component is obtained after DEG C；
To be 1 with basic component mol ratio:1.1:1.1 cresols and metaformaldehyde (equivalent of formaldehyde) is formulated as 65wt%'s
Ethanol solution, add acetic acid and adjust pH value to 4.0, above-mentioned solution is slowly added dropwise into basic component, after being added dropwise
Stirring reaction 2.0 hours under the conditions of 90 DEG C, obtain difunctional asphalt emulsifier.
Emulsifiability test is carried out to difunctional asphalt emulsifier obtained above：The difunctional asphalt emulsifier is prepared
To account for the emulsified asphalt gross mass 1.5wt% aqueous solution, with salt acid for adjusting pH value to 2.0, colloid mill is poured into after being heated to 55 DEG C
In, after starting colloid mill, the AH-90 matrix pitches that temperature is 130 DEG C are at the uniform velocity added and fully sheared, obtain bitumen content
For 60wt% emulsified asphalt.After tested, emulsified asphalt is cationic, and volume average particle sizes are 3.4 μm, 1 day and 5 days of storage
It is respectively 0.53% and 3.39% to deposit stability, and surplus is 0.05% on sieve.
Corrosion inhibition test is carried out to difunctional asphalt emulsifier obtained above：With reference to People's Republic of China's oil day
Right gas professional standard SY/T5405-1996, the difunctional asphalt emulsifier is formulated as the 1.5wt% aqueous solution, adjusted with hydrochloric acid
PH value is saved to 2.0, after being heated to 90 DEG C, N80 corrosion coupons are positioned in solution 4.0 hours, corrosion is weighed after taking out test piece
For front and rear weightlessness to calculate corrosion rate, it is final result to take the average value tested three times, is calculated as a comparison with blank test slow
Erosion rate.The corrosion rate that inhibition qualification test measures is 0.41g.m-2.h-1, corrosion inhibition rate 98.56%.
Embodiment 6
It is 1 by mol ratio:1.2 laurate is with triethylene tetramine input reactor, adding and accounting for reaction raw materials gross weight
30wt% ortho-xylene, reaction system is warming up to 145 DEG C after stirring, isothermal reaction 4.0 hours, then rise is reacted
For system temperature to 245 DEG C, it is 0.092MPa that vacuum is evacuated to after desolvation, continues reaction 3.5 hours, temperature is down to 85
Basic component is obtained after DEG C；
To be 1 with basic component mol ratio:1.3:1.3 cyclohexanone and formaldehyde are formulated as 70wt% ethanol solution, add
Enter hydrochloric acid and adjust pH value to 3.0, above-mentioned solution is slowly added dropwise into basic component, after being added dropwise under the conditions of 110 DEG C
Stirring reaction 1.0 hours, obtains difunctional asphalt emulsifier.
Emulsifiability test is carried out to difunctional asphalt emulsifier obtained above：The difunctional asphalt emulsifier is prepared
To account for the emulsified asphalt gross mass 1.5wt% aqueous solution, with salt acid for adjusting pH value to 2.0, colloid mill is poured into after being heated to 55 DEG C
In, after starting colloid mill, the AH-90 matrix pitches that temperature is 130 DEG C are at the uniform velocity added and fully sheared, obtain bitumen content
For 60wt% emulsified asphalt.After tested, emulsified asphalt is cationic, and volume average particle sizes are 2.8 μm, 1 day and 5 days of storage
It is respectively 0.36% and 3.02% to deposit stability, and surplus is 0.03% on sieve.
Corrosion inhibition test is carried out to difunctional asphalt emulsifier obtained above：With reference to People's Republic of China's oil day
Right gas professional standard SY/T5405-1996, the difunctional asphalt emulsifier is formulated as the 1.5wt% aqueous solution, adjusted with hydrochloric acid
PH value is saved to 2.0, after being heated to 90 DEG C, N80 corrosion coupons are positioned in solution 4.0 hours, corrosion is weighed after taking out test piece
For front and rear weightlessness to calculate corrosion rate, it is final result to take the average value tested three times, is calculated as a comparison with blank test slow
Erosion rate.The corrosion rate that inhibition qualification test measures is 0.56g.m-2.h-1, corrosion inhibition rate 98.03%.
Embodiment 7
It is 1 by mol ratio:1.4 palmitic acid is with TEPA input reactor, adding and accounting for reaction raw materials gross weight
35wt% toluene, reaction system is warming up to 140 DEG C after stirring, isothermal reaction 4.0 hours, then raises reaction system
For temperature to 235 DEG C, it is 0.092MPa that vacuum is evacuated to after desolvation, continues reaction 3.5 hours, after temperature is down to 80 DEG C
Obtain basic component；
To be 1 with basic component mol ratio:1.2:1.2 acetophenone and formaldehyde are formulated as 85wt% ethanol solution, add
Enter hydrochloric acid and adjust pH value to 3.0, above-mentioned solution is slowly added dropwise into basic component, after being added dropwise under the conditions of 90 DEG C
Stirring reaction 1.5 hours, obtains difunctional asphalt emulsifier.
Emulsifiability test is carried out to difunctional asphalt emulsifier obtained above：The difunctional asphalt emulsifier is prepared
To account for the emulsified asphalt gross mass 1.5wt% aqueous solution, with salt acid for adjusting pH value to 2.0, colloid mill is poured into after being heated to 55 DEG C
In, after starting colloid mill, the AH-90 matrix pitches that temperature is 130 DEG C are at the uniform velocity added and fully sheared, obtain bitumen content
For 60wt% emulsified asphalt.After tested, emulsified asphalt is cationic, and volume average particle sizes are 2.7 μm, 1 day and 5 days of storage
It is respectively 0.31% and 2.49% to deposit stability, and surplus is 0.02% on sieve.
Corrosion inhibition test is carried out to difunctional asphalt emulsifier obtained above：With reference to People's Republic of China's oil day
Right gas professional standard SY/T5405-1996, the difunctional asphalt emulsifier is formulated as the 1.5wt% aqueous solution, adjusted with hydrochloric acid
PH value is saved to 2.0, after being heated to 90 DEG C, N80 corrosion coupons are positioned in solution 4.0 hours, corrosion is weighed after taking out test piece
For front and rear weightlessness to calculate corrosion rate, it is final result to take the average value tested three times, is calculated as a comparison with blank test slow
Erosion rate.The corrosion rate that inhibition qualification test measures is 0.32g.m-2.h-1, corrosion inhibition rate 98.87%.
Embodiment 8
It is 1 by mol ratio:1.1 capric acid is with ethylenediamine input reactor, adding and accounting for reaction raw materials gross weight 25wt%
Mixed XYLENE, reaction system is warming up to 150 DEG C after stirring, isothermal reaction 3.5 hours, then raises reaction system temperature
For degree to 250 DEG C, it is 0.094MPa that vacuum is evacuated to after desolvation, continues reaction 3.0 hours, and temperature obtains after being down to 90 DEG C
To basic component；
To be 1 with basic component mol ratio:1.1:1.1 cyclohexanone and formaldehyde are formulated as 80wt% ethanol solution, add
Enter acetic acid and adjust pH value to 5.0, above-mentioned solution is slowly added dropwise into basic component, after being added dropwise under the conditions of 95 DEG C
Stirring reaction 2.5 hours, obtains difunctional asphalt emulsifier.
Emulsifiability test is carried out to difunctional asphalt emulsifier obtained above：The difunctional asphalt emulsifier is prepared
To account for the emulsified asphalt gross mass 1.5wt% aqueous solution, with salt acid for adjusting pH value to 2.0, colloid mill is poured into after being heated to 55 DEG C
In, after starting colloid mill, the AH-90 matrix pitches that temperature is 130 DEG C are at the uniform velocity added and fully sheared, obtain bitumen content
For 60wt% emulsified asphalt.After tested, emulsified asphalt is cationic, and volume average particle sizes are 2.8 μm, 1 day and 5 days of storage
It is respectively 0.39% and 2.87% to deposit stability, and surplus is 0.03% on sieve.
Corrosion inhibition test is carried out to difunctional asphalt emulsifier obtained above：With reference to People's Republic of China's oil day
Right gas professional standard SY/T5405-1996, the difunctional asphalt emulsifier is formulated as the 1.5wt% aqueous solution, adjusted with hydrochloric acid
PH value is saved to 2.0, after being heated to 90 DEG C, N80 corrosion coupons are positioned in solution 4.0 hours, corrosion is weighed after taking out test piece
For front and rear weightlessness to calculate corrosion rate, it is final result to take the average value tested three times, is calculated as a comparison with blank test slow
Erosion rate.The corrosion rate that inhibition qualification test measures is 0.21g.m-2.h-1, corrosion inhibition rate 99.26%.
Embodiment 9
It is 1 by mol ratio:1.2 stearic acid is with diethylenetriamine input reactor, adding and accounting for reaction raw materials gross weight
20wt% ortho-xylene, reaction system is warming up to 155 DEG C after stirring, isothermal reaction 3.5 hours, then rise is reacted
For system temperature to 255 DEG C, it is 0.096MPa that vacuum is evacuated to after desolvation, continues reaction 2.5 hours, temperature is down to 70
Basic component is obtained after DEG C；
To be 1 with basic component mol ratio:1:1 cresols and formaldehyde are formulated as 90wt% ethanol solution, add hydrochloric acid
And adjust pH value to 6.0, above-mentioned solution is slowly added dropwise into basic component, after being added dropwise under the conditions of 85 DEG C stirring reaction
3.0 hours, obtain difunctional asphalt emulsifier.
Emulsifiability test is carried out to difunctional asphalt emulsifier obtained above：The difunctional asphalt emulsifier is prepared
To account for the emulsified asphalt gross mass 1.5wt% aqueous solution, with salt acid for adjusting pH value to 2.0, colloid mill is poured into after being heated to 55 DEG C
In, after starting colloid mill, the AH-90 matrix pitches that temperature is 130 DEG C are at the uniform velocity added and fully sheared, obtain bitumen content
For 60wt% emulsified asphalt.After tested, emulsified asphalt is cationic, and volume average particle sizes are 3.0 μm, 1 day and 5 days of storage
It is respectively 0.47% and 3.36% to deposit stability, and surplus is 0.06% on sieve.
Corrosion inhibition test is carried out to difunctional asphalt emulsifier obtained above：With reference to People's Republic of China's oil day
Right gas professional standard SY/T5405-1996, the difunctional asphalt emulsifier is formulated as the 1.5wt% aqueous solution, adjusted with hydrochloric acid
PH value is saved to 2.0, after being heated to 90 DEG C, N80 corrosion coupons are positioned in solution 4.0 hours, corrosion is weighed after taking out test piece
For front and rear weightlessness to calculate corrosion rate, it is final result to take the average value tested three times, is calculated as a comparison with blank test slow
Erosion rate.The corrosion rate that inhibition qualification test measures is 0.29g.m-2.h-1, corrosion inhibition rate 98.98%.
Embodiment 10
It is 1 by mol ratio:1.5 tetradecylic acid is with pentaethylene hexamine input reactor, adding and accounting for reaction raw materials gross weight
35wt% paraxylene, reaction system is warming up to 155 DEG C after stirring, isothermal reaction 3.5 hours, then rise is reacted
For system temperature to 260 DEG C, it is 0.092MPa that vacuum is evacuated to after desolvation, continues reaction 2.0 hours, temperature is down to 75
Basic component is obtained after DEG C；
To be 1 with basic component mol ratio:1.2:1.2 phenol and formaldehyde are formulated as 80wt% ethanol solution, add
Acetic acid simultaneously adjusts pH value to 3.0, and above-mentioned solution is slowly added dropwise into basic component, stirred after being added dropwise under the conditions of 95 DEG C
Reaction 2.0 hours, obtains difunctional asphalt emulsifier.
Emulsifiability test is carried out to difunctional asphalt emulsifier obtained above：The difunctional asphalt emulsifier is prepared
To account for the emulsified asphalt gross mass 1.5wt% aqueous solution, with salt acid for adjusting pH value to 2.0, colloid mill is poured into after being heated to 55 DEG C
In, after starting colloid mill, the AH-90 matrix pitches that temperature is 130 DEG C are at the uniform velocity added and fully sheared, obtain bitumen content
For 60wt% emulsified asphalt.After tested, emulsified asphalt is cationic, and volume average particle sizes are 2.8 μm, 1 day and 5 days of storage
It is respectively 0.39% and 2.87% to deposit stability, and surplus is 0.03% on sieve.
Corrosion inhibition test is carried out to difunctional asphalt emulsifier obtained above：With reference to People's Republic of China's oil day
Right gas professional standard SY/T5405-1996, the difunctional asphalt emulsifier is formulated as the 1.5wt% aqueous solution, adjusted with hydrochloric acid
PH value is saved to 2.0, after being heated to 90 DEG C, N80 corrosion coupons are positioned in solution 4.0 hours, corrosion is weighed after taking out test piece
For front and rear weightlessness to calculate corrosion rate, it is final result to take the average value tested three times, is calculated as a comparison with blank test slow
Erosion rate.The corrosion rate that inhibition qualification test measures is 0.34g.m-2.h-1, corrosion inhibition rate 98.80%.
Embodiment 11
It is 1 by mol ratio:1 tetradecylic acid is with ethylenediamine input reactor, adding and accounting for reaction raw materials gross weight 35wt%
Meta-xylene, reaction system is warming up to 160 DEG C after stirring, isothermal reaction 3.0 hours, then raises reaction system temperature
For degree to 240 DEG C, it is 0.093MPa that vacuum is evacuated to after desolvation, continues reaction 3.5 hours, and temperature obtains after being down to 70 DEG C
To basic component；
To be 1 with basic component mol ratio:1.1:1.1 acetophenone and formaldehyde are formulated as 75wt% ethanol solution, add
Enter acetic acid and adjust pH value to 4.0, above-mentioned solution is slowly added dropwise into basic component, after being added dropwise under the conditions of 105 DEG C
Stirring reaction 1.5 hours, obtains difunctional asphalt emulsifier.
Emulsifiability test is carried out to difunctional asphalt emulsifier obtained above：The difunctional asphalt emulsifier is prepared
To account for the emulsified asphalt gross mass 1.5wt% aqueous solution, with salt acid for adjusting pH value to 2.0, colloid mill is poured into after being heated to 55 DEG C
In, after starting colloid mill, the AH-90 matrix pitches that temperature is 130 DEG C are at the uniform velocity added and fully sheared, obtain bitumen content
For 60wt% emulsified asphalt.After tested, emulsified asphalt is cationic, and volume average particle sizes are 2.4 μm, 1 day and 5 days of storage
It is respectively 0.69% and 4.03% to deposit stability, and surplus is 0.08% on sieve.
Corrosion inhibition test is carried out to difunctional asphalt emulsifier obtained above：With reference to People's Republic of China's oil day
Right gas professional standard SY/T5405-1996, the difunctional asphalt emulsifier is formulated as the 1.5wt% aqueous solution, adjusted with hydrochloric acid
PH value is saved to 2.0, after being heated to 90 DEG C, N80 corrosion coupons are positioned in solution 4.0 hours, corrosion is weighed after taking out test piece
For front and rear weightlessness to calculate corrosion rate, it is final result to take the average value tested three times, is calculated as a comparison with blank test slow
Erosion rate.The corrosion rate that inhibition qualification test measures is 0.38g.m-2.h-1, corrosion inhibition rate 98.66%.
Embodiment 12
It is 1 by mol ratio:1 palmitic acid is with triethylene tetramine input reactor, adding and accounting for reaction raw materials gross weight
40wt% Mixed XYLENE, reaction system is warming up to 165 DEG C after stirring, isothermal reaction 2.5 hours, then rise is reacted
For system temperature to 235 DEG C, it is 0.095MPa that vacuum is evacuated to after desolvation, continues reaction 4.0 hours, temperature is down to 80
Basic component is obtained after DEG C；
To be 1 with basic component mol ratio:1:1 cyclohexanone and formaldehyde are formulated as 75wt% ethanol solution, add salt
Acid simultaneously adjusts pH value to 2.0, and above-mentioned solution is slowly added dropwise into basic component, stirred after being added dropwise under the conditions of 110 DEG C
Reaction 1.5 hours, obtains difunctional asphalt emulsifier.
Emulsifiability test is carried out to difunctional asphalt emulsifier obtained above：The difunctional asphalt emulsifier is prepared
To account for the emulsified asphalt gross mass 1.5wt% aqueous solution, with salt acid for adjusting pH value to 2.0, colloid mill is poured into after being heated to 55 DEG C
In, after starting colloid mill, the AH-90 matrix pitches that temperature is 130 DEG C are at the uniform velocity added and fully sheared, obtain bitumen content
For 60wt% emulsified asphalt.After tested, emulsified asphalt is cationic, and volume average particle sizes are 2.5 μm, 1 day and 5 days of storage
It is respectively 0.24% and 2.12% to deposit stability, and surplus is 0.02% on sieve.
Corrosion inhibition test is carried out to difunctional asphalt emulsifier obtained above：With reference to People's Republic of China's oil day
Right gas professional standard SY/T5405-1996, the difunctional asphalt emulsifier is formulated as the 1.5wt% aqueous solution, adjusted with hydrochloric acid
PH value is saved to 2.0, after being heated to 90 DEG C, N80 corrosion coupons are positioned in solution 4.0 hours, corrosion is weighed after taking out test piece
For front and rear weightlessness to calculate corrosion rate, it is final result to take the average value tested three times, is calculated as a comparison with blank test slow
Erosion rate.The corrosion rate that inhibition qualification test measures is 0.43g.m-2.h-1, corrosion inhibition rate 98.49%.
Embodiment 13
It is 1 by mol ratio:1.1 laurate is with diethylenetriamine input reactor, adding and accounting for reaction raw materials gross weight
40wt% Mixed XYLENE, reaction system is warming up to 170 DEG C after stirring, isothermal reaction 2.5 hours, then rise is reacted
For system temperature to 240 DEG C, it is 0.094MPa that vacuum is evacuated to after desolvation, continues reaction 4.0 hours, temperature is down to 85
Basic component is obtained after DEG C；
To be 1 with basic component mol ratio:1.3:1.3 acetophenone and formaldehyde are formulated as 80wt% ethanol solution, add
Enter hydrochloric acid and adjust pH value to 3.0, above-mentioned solution is slowly added dropwise into basic component, after being added dropwise under the conditions of 100 DEG C
Stirring reaction 2.0 hours, obtains difunctional asphalt emulsifier.
Emulsifiability test is carried out to difunctional asphalt emulsifier obtained above：The difunctional asphalt emulsifier is prepared
To account for the emulsified asphalt gross mass 1.5wt% aqueous solution, with salt acid for adjusting pH value to 2.0, colloid mill is poured into after being heated to 55 DEG C
In, after starting colloid mill, the AH-90 matrix pitches that temperature is 130 DEG C are at the uniform velocity added and fully sheared, obtain bitumen content
For 60wt% emulsified asphalt.After tested, emulsified asphalt is cationic, and volume average particle sizes are 3.1 μm, 1 day and 5 days of storage
It is respectively 0.74% and 4.02% to deposit stability, and surplus is 0.08% on sieve.
Corrosion inhibition test is carried out to difunctional asphalt emulsifier obtained above：With reference to People's Republic of China's oil day
Right gas professional standard SY/T5405-1996, the difunctional asphalt emulsifier is formulated as the 1.5wt% aqueous solution, adjusted with hydrochloric acid
PH value is saved to 2.0, after being heated to 90 DEG C, N80 corrosion coupons are positioned in solution 4.0 hours, corrosion is weighed after taking out test piece
For front and rear weightlessness to calculate corrosion rate, it is final result to take the average value tested three times, is calculated as a comparison with blank test slow
Erosion rate.The corrosion rate that inhibition qualification test measures is 0.47g.m-2.h-1, corrosion inhibition rate 98.34%.
Embodiment 14
It is 1 by mol ratio:1.3 palmitic acid is with ethylenediamine input reactor, adding and accounting for reaction raw materials gross weight
45wt% Mixed XYLENE, reaction system is warming up to 160 DEG C after stirring, isothermal reaction 3.0 hours, then rise is reacted
For system temperature to 245 DEG C, it is 0.092MPa that vacuum is evacuated to after desolvation, continues reaction 3.5 hours, temperature is down to 80
Basic component is obtained after DEG C；
To be 1 with basic component mol ratio:1.3:1.3 cresols and formaldehyde are formulated as 65wt% ethanol solution, add
Hydrochloric acid simultaneously adjusts pH value to 3.0, and above-mentioned solution is slowly added dropwise into basic component, stirred after being added dropwise under the conditions of 105 DEG C
Reaction 2.5 hours is mixed, obtains difunctional asphalt emulsifier.
Emulsifiability test is carried out to difunctional asphalt emulsifier obtained above：The difunctional asphalt emulsifier is prepared
To account for the emulsified asphalt gross mass 1.5wt% aqueous solution, with salt acid for adjusting pH value to 2.0, colloid mill is poured into after being heated to 55 DEG C
In, after starting colloid mill, the AH-90 matrix pitches that temperature is 130 DEG C are at the uniform velocity added and fully sheared, obtain bitumen content
For 60wt% emulsified asphalt.After tested, emulsified asphalt is cationic, and volume average particle sizes are 2.6 μm, 1 day and 5 days of storage
It is respectively 0.34% and 2.55% to deposit stability, and surplus is 0.03% on sieve.
Corrosion inhibition test is carried out to difunctional asphalt emulsifier obtained above：With reference to People's Republic of China's oil day
Right gas professional standard SY/T5405-1996, the difunctional asphalt emulsifier is formulated as the 1.5wt% aqueous solution, adjusted with hydrochloric acid
PH value is saved to 2.0, after being heated to 90 DEG C, N80 corrosion coupons are positioned in solution 4.0 hours, corrosion is weighed after taking out test piece
For front and rear weightlessness to calculate corrosion rate, it is final result to take the average value tested three times, is calculated as a comparison with blank test slow
Erosion rate.The corrosion rate that inhibition qualification test measures is 0.56g.m-2.h-1, corrosion inhibition rate 98.03%.
Embodiment 15
It is 1 by mol ratio:1.5 capric acid is with triethylene tetramine input reactor, adding and accounting for reaction raw materials gross weight
50wt% Mixed XYLENE, reaction system is warming up to 180 DEG C after stirring, isothermal reaction 2.0 hours, then rise is reacted
For system temperature to 240 DEG C, it is 0.091MPa that vacuum is evacuated to after desolvation, continues reaction 3.5 hours, temperature is down to 75
Basic component is obtained after DEG C；
To be 1 with basic component mol ratio:1.2:1.2 acetophenone and formaldehyde are formulated as 75wt% ethanol solution, add
Enter acetic acid and adjust pH value to 4.0, above-mentioned solution is slowly added dropwise into basic component, after being added dropwise under the conditions of 105 DEG C
Stirring reaction 1.0 hours, obtains difunctional asphalt emulsifier.
Emulsifiability test is carried out to difunctional asphalt emulsifier obtained above：The difunctional asphalt emulsifier is prepared
To account for the emulsified asphalt gross mass 1.5wt% aqueous solution, with salt acid for adjusting pH value to 2.0, colloid mill is poured into after being heated to 55 DEG C
In, after starting colloid mill, the AH-90 matrix pitches that temperature is 130 DEG C are at the uniform velocity added and fully sheared, obtain bitumen content
For 60wt% emulsified asphalt.After tested, emulsified asphalt is cationic, and volume average particle sizes are 2.4 μm, 1 day and 5 days of storage
It is respectively 0.31% and 2.23% to deposit stability, and surplus is 0.03% on sieve.
Corrosion inhibition test is carried out to difunctional asphalt emulsifier obtained above：With reference to People's Republic of China's oil day
Right gas professional standard SY/T5405-1996, the difunctional asphalt emulsifier is formulated as the 1.5wt% aqueous solution, adjusted with hydrochloric acid
PH value is saved to 2.0, after being heated to 90 DEG C, N80 corrosion coupons are positioned in solution 4.0 hours, corrosion is weighed after taking out test piece
For front and rear weightlessness to calculate corrosion rate, it is final result to take the average value tested three times, is calculated as a comparison with blank test slow
Erosion rate.The corrosion rate that inhibition qualification test measures is 0.59g.m-2.h-1, corrosion inhibition rate 97.92%.
Embodiment 16
It is 1 by mol ratio:1.2 stearic acid is with TEPA input reactor, adding and accounting for reaction raw materials gross weight
50wt% Mixed XYLENE, reaction system is warming up to 175 DEG C after stirring, isothermal reaction 2.0 hours, then rise is reacted
For system temperature to 235 DEG C, it is 0.090MPa that vacuum is evacuated to after desolvation, continues reaction 5.5 hours, temperature is down to 70
Basic component is obtained after DEG C；
To be 1 with basic component mol ratio:1:1 cyclohexanone and formaldehyde are formulated as 70wt% ethanol solution, add salt
Acid simultaneously adjusts pH value to 2.0, and above-mentioned solution is slowly added dropwise into basic component, stirred instead under the conditions of 98 DEG C after being added dropwise
Answer 1.5 hours, obtain difunctional asphalt emulsifier.
Emulsifiability test is carried out to difunctional asphalt emulsifier obtained above：The difunctional asphalt emulsifier is prepared
To account for the emulsified asphalt gross mass 1.5wt% aqueous solution, with salt acid for adjusting pH value to 2.0, colloid mill is poured into after being heated to 55 DEG C
In, after starting colloid mill, the AH-90 matrix pitches that temperature is 130 DEG C are at the uniform velocity added and fully sheared, obtain bitumen content
For 60wt% emulsified asphalt.After tested, emulsified asphalt is cationic, and volume average particle sizes are 2.3 μm, 1 day and 5 days of storage
It is respectively 0.18% and 1.96% to deposit stability, and surplus is 0.01% on sieve.
Corrosion inhibition test is carried out to difunctional asphalt emulsifier obtained above：With reference to People's Republic of China's oil day
Right gas professional standard SY/T5405-1996, the difunctional asphalt emulsifier is formulated as the 1.5wt% aqueous solution, adjusted with hydrochloric acid
PH value is saved to 2.0, after being heated to 90 DEG C, N80 corrosion coupons are positioned in solution 4.0 hours, corrosion is weighed after taking out test piece
For front and rear weightlessness to calculate corrosion rate, it is final result to take the average value tested three times, is calculated as a comparison with blank test slow
Erosion rate.The corrosion rate that inhibition qualification test measures is 0.40g.m-2.h-1, corrosion inhibition rate 98.59%.
Embodiment 17
It is 1 by mol ratio:1.1 tetradecylic acid is with pentaethylene hexamine input reactor, adding and accounting for reaction raw materials gross weight
25wt% paraxylene, reaction system is warming up to 165 DEG C after stirring, isothermal reaction 3.0 hours, then rise is reacted
For system temperature to 235 DEG C, it is 0.092MPa that vacuum is evacuated to after desolvation, continues reaction 5.0 hours, temperature is down to 90
Basic component is obtained after DEG C；
To be 1 with basic component mol ratio:1.1:1.1 phenol and formaldehyde are formulated as 75wt% ethanol solution, add
Hydrochloric acid simultaneously adjusts pH value to 5.0, and above-mentioned solution is slowly added dropwise into basic component, stirred after being added dropwise under the conditions of 100 DEG C
Reaction 2.0 hours is mixed, obtains difunctional asphalt emulsifier.
Emulsifiability test is carried out to difunctional asphalt emulsifier obtained above：The difunctional asphalt emulsifier is prepared
To account for the emulsified asphalt gross mass 1.5wt% aqueous solution, with salt acid for adjusting pH value to 2.0, colloid mill is poured into after being heated to 55 DEG C
In, after starting colloid mill, the AH-90 matrix pitches that temperature is 130 DEG C are at the uniform velocity added and fully sheared, obtain bitumen content
For 60wt% emulsified asphalt.After tested, emulsified asphalt is cationic, and volume average particle sizes are 2.8 μm, 1 day and 5 days of storage
It is respectively 0.39% and 2.87% to deposit stability, and surplus is 0.03% on sieve.
Corrosion inhibition test is carried out to difunctional asphalt emulsifier obtained above：With reference to People's Republic of China's oil day
Right gas professional standard SY/T5405-1996, the difunctional asphalt emulsifier is formulated as the 1.5wt% aqueous solution, adjusted with hydrochloric acid
PH value is saved to 2.0, after being heated to 90 DEG C, N80 corrosion coupons are positioned in solution 4.0 hours, corrosion is weighed after taking out test piece
For front and rear weightlessness to calculate corrosion rate, it is final result to take the average value tested three times, is calculated as a comparison with blank test slow
Erosion rate.The corrosion rate that inhibition qualification test measures is 0.42g.m-2.h-1, corrosion inhibition rate 98.52%.
Embodiment 18
It is 1 by mol ratio:1.3 palmitic acid is with TEPA input reactor, adding and accounting for reaction raw materials gross weight
30wt% Mixed XYLENE, reaction system is warming up to 170 DEG C after stirring, isothermal reaction 2.5 hours, then rise is reacted
For system temperature to 225 DEG C, it is 0.094MPa that vacuum is evacuated to after desolvation, continues reaction 5.5 hours, temperature is down to 75
Basic component is obtained after DEG C；
To be 1 with basic component mol ratio:1.1:1.1 acetophenone and formaldehyde are formulated as 80wt% ethanol solution, add
Enter acetic acid and adjust pH value to 6.0, above-mentioned solution is slowly added dropwise into basic component, after being added dropwise under the conditions of 85 DEG C
Stirring reaction 2.5 hours, obtains difunctional asphalt emulsifier.
Emulsifiability test is carried out to difunctional asphalt emulsifier obtained above：The difunctional asphalt emulsifier is prepared
To account for the emulsified asphalt gross mass 1.5wt% aqueous solution, with salt acid for adjusting pH value to 2.0, colloid mill is poured into after being heated to 55 DEG C
In, after starting colloid mill, the AH-90 matrix pitches that temperature is 130 DEG C are at the uniform velocity added and fully sheared, obtain bitumen content
For 60wt% emulsified asphalt.After tested, emulsified asphalt is cationic, and volume average particle sizes are 3.2 μm, 1 day and 5 days of storage
It is respectively 0.84% and 4.51% to deposit stability, and surplus is 0.08% on sieve.
Corrosion inhibition test is carried out to difunctional asphalt emulsifier obtained above：With reference to People's Republic of China's oil day
Right gas professional standard SY/T5405-1996, the difunctional asphalt emulsifier is formulated as the 1.5wt% aqueous solution, adjusted with hydrochloric acid
PH value is saved to 2.0, after being heated to 90 DEG C, N80 corrosion coupons are positioned in solution 4.0 hours, corrosion is weighed after taking out test piece
For front and rear weightlessness to calculate corrosion rate, it is final result to take the average value tested three times, is calculated as a comparison with blank test slow
Erosion rate.The corrosion rate that inhibition qualification test measures is 0.61g.m-2.h-1, corrosion inhibition rate 97.85%.
Claims (8)
1. a kind of have emulsification and the difunctional asphalt emulsifier of inhibition, it is characterised in that its general structure is (I)：
Wherein R1Expression-CnH2n-1Alkyl side chain, n is integer and 9≤n≤17；
-(CH2CH2NH)x- it is ethyleneamines chain, x=0,1,2,3,4；
R2ForA kind of substituent in.
2. a kind of general structure prepared described in claim 1 is the method for the difunctional asphalt emulsifier of (I), including as follows
Step：
1) preparation of basic component：Using mol ratio as 1:1~1.5 long chain organic acid and organic polyamine are reaction raw materials, are added
Account for 20~50wt% of reaction raw materials gross weight solvent, stirring is warming up to 140~180 DEG C, and steady temperature reacts 2~4 hours, so
Temperature of reaction system is raised afterwards to 220~260 DEG C, and it is 0.090~0.096MPa that vacuum is evacuated to after desolvation, is continued
Reaction 2~6 hours, temperature is down to 70~90 DEG C, obtains basic component；
2) will be 1 with basic component mol ratio:1~1.3:1~1.3 acidic components and organic aldehyde are formulated as 60~90wt%'s
Ethanol solution, add catalyst and adjust pH value to 2~6, be slowly added dropwise into the basic component obtained by step 1), drip
Finish after under the conditions of 80~110 DEG C stirring reaction 1~3 hour, obtain difunctional asphalt emulsifier.
3. difunctional asphalt emulsifier according to claim 1 or 2, it is characterised in that：Described long chain organic acid is carbon
Chain length is 10~18 linear saturated fatty acids.
4. difunctional asphalt emulsifier according to claim 1 or 2, it is characterised in that：Described organic polyamine is second two
One kind in amine, diethylenetriamine, triethylene tetramine, TEPA, pentaethylene hexamine.
5. the preparation method of difunctional asphalt emulsifier according to claim 2, it is characterised in that：Described acidic components
For one kind in acetophenone, cyclohexanone, phenol and cresols.
6. the preparation method of difunctional asphalt emulsifier according to claim 2, it is characterised in that：Described organic aldehyde is
Formaldehyde, formalin or the polyformaldehyde that formaldehyde can be dissociateed.
7. the preparation method of difunctional asphalt emulsifier according to claim 2, it is characterised in that：Described solvent is first
One kind in benzene, meta-xylene, ortho-xylene, paraxylene, Mixed XYLENE.
8. the preparation method of difunctional asphalt emulsifier according to claim 2, it is characterised in that：Described catalyst is
One kind in hydrochloric acid, formic acid, acetic acid, phosphoric acid.
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| CN112920311A (en) * | 2021-01-27 | 2021-06-08 | 山东交通学院 | High-molecular asphalt emulsifier and preparation method and application thereof |
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