CN114956672B - Semi-flexible asphalt and preparation method thereof - Google Patents

Semi-flexible asphalt and preparation method thereof Download PDF

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CN114956672B
CN114956672B CN202210687705.XA CN202210687705A CN114956672B CN 114956672 B CN114956672 B CN 114956672B CN 202210687705 A CN202210687705 A CN 202210687705A CN 114956672 B CN114956672 B CN 114956672B
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asphalt
emulsified asphalt
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CN114956672A (en
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王志方
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Shandong Huachen Road And Bridge Co ltd
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Shandong Huachen Road And Bridge Co ltd
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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
    • C08L95/005—Aqueous compositions, e.g. emulsions
    • 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
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A30/00—Adapting or protecting infrastructure or their operation
    • Y02A30/30—Adapting or protecting infrastructure or their operation in transportation, e.g. on roads, waterways or railways
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A30/00—Adapting or protecting infrastructure or their operation
    • Y02A30/60—Planning or developing urban green infrastructure

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Abstract

The invention discloses semi-flexible asphalt and a preparation method thereof, and relates to the technical field of asphalt. When the semi-flexible asphalt is prepared, 3-hexenol methyl phenylacetate is emulsified into matrix asphalt to prepare emulsified asphalt; mixing vinyl p-methyl phthalonitrile and butadiene-based terephthalic acid to prepare styrene-butadiene resin; mixing styrene-butadiene resin, phosphoric acid and ceramsite, and performing hot stirring by using ammonia gas to form an interpenetrating network structure of ammonium polyphosphate and polyphenyl diamide to prepare functional ceramsite; finally, mixing the emulsified asphalt and the functionalized ceramsite to form the polyarylamide containing the dibenzo-octatomic ring structure, so as to prepare semi-flexible asphalt; the semi-flexible asphalt prepared by the invention has good flame retardance, compression resistance, rutting resistance and low-temperature cracking resistance.

Description

Semi-flexible asphalt and preparation method thereof
Technical Field
The invention relates to the technical field of asphalt, in particular to semi-flexible asphalt and a preparation method thereof.
Background
Bitumen is a black or blackish-brown solid, semi-solid or liquid mixture composed of a number of extremely complex polymeric hydrocarbons and nonmetallic derivatives of these hydrocarbons. Because of the good waterproof property and the strong binding ability with mineral mixture such as sand, stone, etc., the paved pavement is easy to maintain and is widely applied to modern road engineering.
In the use process of an asphalt road, people find that the asphalt mixture is sensitive to temperature change, the mechanical property is greatly influenced by the loading action time, and when the external environment temperature is too high, high-temperature rutting can be generated; when the temperature of the external environment is too low, low-temperature cracking can be generated. And asphalt is combustible, which is very easy to cause potential safety hazard of roads. Therefore, the preparation of asphalt with high flame retardance, rutting resistance and low-temperature cracking resistance is a technical problem to be solved in the current technical field.
The present invention addresses this problem by combining rigid ceramsite with flexible asphalt to produce semi-flexible asphalt.
Disclosure of Invention
The invention aims to provide semi-flexible asphalt and a preparation method thereof, which are used for solving the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme:
a semi-flexible asphalt is prepared by mixing emulsified asphalt and functionalized ceramsite.
Further, the emulsified asphalt is prepared by emulsifying matrix asphalt with 3-hexenol methyl phenylacetate.
Further, the functional ceramsite is prepared by mixing styrene-butadiene resin, phosphoric acid and ceramsite and stirring by ammonia bubbling heat.
Further, the styrene-butadiene resin is prepared from vinyl-p-methylphthalonitrile and butadiene-terephthalic acid.
Further, the preparation method of the semi-flexible asphalt comprises the following preparation steps:
(1) Under the conditions of high temperature and argon protection, ceramsite and phosphoric acid are mixed according to the mass ratio of 1:0.5 to 1:0.7, followed by mixing at 2-3 m from the bottom 3 Stirring for 30-50 min at 800-1000 r/min, adding phosphorus pentoxide with the mass of 1-2 times of the ceramsite, continuously stirring for 1.5-2.5 h after continuously stirring for 4-6 times of the ceramsite at 280-300 ℃, cooling to 60-80 ℃, adding styrene-butadiene resin with the mass of 0.6-0.8 times of the ceramsite, dripping concentrated sulfuric acid with the mass fraction of 0.3-0.5 times of the ceramsite at 40-60 drops/min, continuously stirring for 2-4 h, continuously stirring for 4-6 times of the ceramsite, adding nano titanium dioxide with the mass of 0.06-0.08 times of the propenyl benzoic acid, heating to 80-100 ℃, and continuously stirring for 2-4 h to obtain the functional ceramsite;
(2) Mixing 130-140 ℃ matrix asphalt with 5-7% 3-hexenol methyl phenylacetate solution according to a mass ratio of 1:0.6 to 1:0.8 is put into an emulsifying machine at 75-85 ℃ to be emulsified for 1-3 hours at 100-300 r/min, and emulsified asphalt is prepared;
(3) Under the conditions of 75-85 ℃ and argon protection, the emulsified asphalt and the functionalized ceramsite are mixed according to the mass ratio of 1:1 to 1:3, uniformly mixing, and adding the components according to the mass ratio of 1:0.4 to 1:0.6 of mixed acetic acid solution with the mass fraction of 42-44% and concentrated sulfuric acid with the mass fraction of 98%, wherein the mass of the acetic acid solution is 0.4-0.6 times of the mass of the emulsified asphalt, the temperature is raised to 110-130 ℃, the mixture is stirred for 1-2 h at 400-600 r/min, sodium hydroxide with the mass of 0.1-0.3 times of the mass of the emulsified asphalt is added, the mixture is continuously stirred for 1-3 h, phosphorus trichloride with the mass of 0.8-1 time of the mass of the emulsified asphalt is added, the mixture is continuously stirred for 11-13 h after the temperature is raised to 140-160 ℃, the temperature is lowered to 100-115 ℃, and the mixture is cooled to 1 according to the mass ratio: 0.1 to 1:0.3 adding aluminum chloride and sodium chloride, wherein the mass of the aluminum chloride is 0.7-0.9 times of that of the emulsified asphalt, continuously stirring for 5-7 h, adding sodium hydroxide solution with the mass fraction of 20-30%, cooling to 35-40 ℃, continuously stirring for 8-9 h, adding palladium carbon with the mass of 0.09-0.11 times of that of the emulsified asphalt, introducing hydrogen with the mass of 10-20 times of that of the emulsified asphalt at 90-100 ℃ and 2-3 MPa, continuously stirring for 7-8 h, heating to 115-119 ℃, continuously stirring for 4-6 h, and then under the condition of 30-50 ℃, mixing the materials according to the mass ratio of 1:4: 9-1: 5:11 adding potassium tert-butoxide, methyl triphenyl iodized phosphorus and diethyl ether, wherein the mass of the potassium tert-butoxide is 0.4-0.6 times of that of the emulsified asphalt, continuously stirring for 10-14 h, adding aluminum oxide 1-3 times of that of the emulsified asphalt, continuously stirring for 1-3 h, adding hydroxyl toluene sulfonyl iodibenzene 0.8-1 time of that of the emulsified asphalt, continuously stirring for 1-4 h at room temperature, and the mass ratio of the aluminum oxide to the emulsified asphalt is 1:1.5 to 1:3 adding lithium aluminum hydride and aluminum chloride, wherein the mass of the lithium aluminum hydride is 1-1.4 times of that of the emulsified asphalt, continuously stirring for 0.8-1.2 h, adding a 30% hydrogen peroxide solution with the mass fraction of 0.6-0.8 times of that of the emulsified asphalt at 0-4 ℃, continuously stirring for 10-18 h at room temperature, adding sodium sulfite with the mass of 3-5 times of that of the emulsified asphalt, continuously stirring for 30-50 min, and mixing according to the mass ratio of 1:0.8:3: 3-1: 1.2:5:5 adding triphenyl phosphite, calcium chloride, pyridine and dry N-methyl-2-pyrrolidone, wherein the mass of the triphenyl phosphite is 0.5 to 0.7 times that of the emulsified asphalt, and continuously stirring for 8 to 14 hours at the temperature of 100 to 150 ℃ to prepare the semi-flexible asphalt.
Further, the ceramsite in the step (1) is shale ceramsite with the particle size of 5-15 mm.
Further, the preparation method of the styrene-butadiene resin in the step (1) comprises the following steps: vinyl p-methyl phthalonitrile, n-hexane and cyclohexane are mixed according to the mass ratio of 1:4: 4-1: 6:6, then cooling to 50-70 ℃, adding n-butyllithium with the mass of 0.6-0.8 times of that of vinyl-p-methylphthalonitrile, stirring for 2-4 h at 800-1000 r/min, adding butadiene-based terephthalic acid with the mass of 0.5-0.7 times of that of vinyl-p-methylphthalonitrile, continuously stirring for 40-60 min, and steaming at 1300-1500 r/min for 40-60 min at 10-30 Pa and 70-72 ℃ to obtain the styrene-butadiene resin.
Further, the preparation method of vinyl p-methyl phthalonitrile comprises the following steps: under the protection of argon at the temperature, ethanol solution of 9-11% of chloroethylene and 4-methyl phthalonitrile are mixed according to the mass ratio of 1:0.2 to 1:0.3, adding aluminum trichloride with the mass of 0.03-0.05 times that of the 4-methyl phthalonitrile, cooling to 0-4 ℃, and stirring for 7-9 h at 800-1000 r/min to obtain the vinyl p-methyl phthalonitrile.
Further, the preparation method of the butadiene-based terephthalic acid comprises the following steps: under the protection of argon at the temperature, 2-chloro-1, 3-butadiene, terephthalic acid and dimethyl sulfoxide are mixed according to the mass ratio of 1:2: 9-1: 3:11, adding aluminum trichloride with the mass of 0.02-0.04 times of that of the 2-chloro-1, 3-butadiene, cooling to 0-4 ℃, and stirring for 7-9 h at 800-1000 r/min to obtain the butadienyl terephthalic acid.
Further, the preparation method of the 3-hexenol methyl phenylacetate in the step (2) comprises the following steps: at room temperature, 3-hexene-1, 6-diol and 2-methyl phenylacetic acid are mixed according to the mass ratio of 1:0.6 to 1:0.8, adding concentrated sulfuric acid with the mass fraction of 98% which is 1.3-1.5 times of the mass of 3-hexene-1, 6-diol, and refluxing for 2-4 hours at the temperature of 80-100 ℃ to obtain the 3-hexenol methyl phenylacetate.
Compared with the prior art, the invention has the following beneficial effects:
when the semi-flexible asphalt is prepared, 3-hexenol methyl phenylacetate is emulsified into matrix asphalt to prepare emulsified asphalt; mixing styrene-butadiene resin, phosphoric acid and ceramsite, and performing hot stirring by using ammonia bubbling to prepare functionalized ceramsite; finally, mixing the emulsified asphalt and the functionalized ceramsite to prepare semi-flexible asphalt; wherein the styrene-butadiene resin is prepared from vinyl p-methyl phthalonitrile and butadiene-based terephthalic acid.
Firstly, partially phosphoric acid acidizes the surface of the ceramsite, a large number of free radicals such as hydroxyl groups are formed on the surface of the ceramsite, and after the partial phosphoric acid reacts with the hydroxyl groups on the surface of the ceramsite, the partial phosphoric acid reacts with ammonia gas to polymerize to form ammonium polyphosphate, so that the flame retardant property of the functionalized ceramsite is enhanced; and part of carboxyl on the styrene-butadiene resin reacts with hydroxyl on the ceramsite, part of carboxyl reacts with ammonia gas and amino on ammonium polyphosphate to crosslink, so that the polyphenyl diamide is formed, an interpenetrating network structure is formed with the ammonium polyphosphate, and the compressive strength of the functionalized ceramsite is increased.
Secondly, ammonium polyphosphate in the functionalized ceramsite reacts with active groups such as hydroxyl, carboxyl, imino and the like in emulsified asphalt molecules to block aggregation of asphaltene, and the asphaltene micelle with larger size is dispersed into smaller asphaltene units, so that the functionalized ceramsite is uniformly dispersed in the emulsified asphalt, and the rutting resistance of the semi-flexible asphalt is enhanced; part of 3-hexenol methyl phenylacetate in the emulsified asphalt is hydrolyzed to form methyl phenylacetic acid, cyano groups on the functionalized ceramsite are hydrolyzed to form methyl phthalic acid, the methyl phthalic acid and the methyl phenylacetic acid react and then are hydrolyzed and reduced to form 2- (2-phenethyl) benzoic acid, the 2- (2-phenethyl) benzoic acid is dehydrated and cyclized under the action of ammonium polyphosphate to form dibenzosuberone, the dibenzosuberone rearranges and is reduced to form a dibenzosubelement ring structure, hydrogen peroxide is introduced to oxidize methyl groups on the dibenzosubelement ring structure into carboxyl groups, the carboxyl groups react with the polyphenyl diamide on the functionalized ceramsite to form polyarylamide, and when the temperature is reduced, the asphalt is contracted, and the polyarylamide containing the dibenzosubelement ring structure is expanded, so that the low-temperature cracking resistance of the semi-flexible asphalt is enhanced.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In order to more clearly illustrate the method provided by the invention, the following examples are used for describing the detailed description, and the test methods of each index of the semi-flexible asphalt prepared in the following examples are as follows:
resistance to compression and rut: the marshall stability and dynamic stability were measured according to JTG E20 to determine the compression resistance and rutting resistance of the semi-flexible asphalt prepared in examples and comparative examples of the same quality.
Low temperature cracking resistance: the semi-flexible asphalt prepared in the examples and comparative examples of the same quality was tested for low temperature cracking resistance by measuring flexural tensile strength according to the GB/T38948 standard method.
Example 1
(1) Under the protection of argon at the temperature, 2-chloro-1, 3-butadiene, terephthalic acid and dimethyl sulfoxide are mixed according to the mass ratio of 1:2:9, uniformly mixing, adding aluminum trichloride with the mass of 0.02 times that of 2-chloro-1, 3-butadiene, cooling to 0 ℃, and stirring for 7h at 800r/min to obtain butadiene-based terephthalic acid; under the protection of argon at the temperature, an ethanol solution of 9% of chloroethylene and 4-methyl phthalonitrile are mixed according to the mass ratio of 1:0.2, adding aluminum trichloride with the mass of 0.03 times that of the 4-methyl phthalonitrile, cooling to 0 ℃, and stirring for 7 hours at 800r/min to obtain vinyl p-methyl phthalonitrile; vinyl p-methyl phthalonitrile, n-hexane and cyclohexane are mixed according to the mass ratio of 1:4:4, uniformly mixing, then cooling to 50 ℃, adding n-butyllithium with the mass of 0.6 times of that of vinyl-p-methylphthalonitrile, stirring for 2 hours at 800r/min, adding butadiene-based terephthalic acid with the mass of 0.5 times of that of vinyl-p-methylphthalonitrile, continuously stirring for 40 minutes, and performing rotary steaming at 1300r/min for 40 minutes at 10Pa and 70 ℃ to obtain styrene-butadiene resin;
(2) Under the conditions of the temperature and the argon protection, shale ceramsite with the grain diameter of 5mm and phosphoric acid are mixed according to the mass ratio of 1:0.5 and then mixed at 2m from the bottom 3 Stirring for 30min at 800r/min, adding phosphorus pentoxide 1 times of the mass of the ceramsite, continuously stirring for 1.5h after heating to 280 deg.C, cooling to 60 deg.C, adding styrene-butadiene resin 0.6 times of the mass of the ceramsite, dropwise adding 98% concentrated sulfuric acid at 40 drops/min, continuously stirring for 2h,continuously bubbling ammonia with the mass 4 times of that of the ceramsite, adding nano titanium dioxide with the mass 0.06 time of that of the propenyl benzoic acid, heating to 80 ℃, and continuously stirring for 2 hours to obtain the functional ceramsite;
(3) At room temperature, 3-hexene-1, 6-diol and 2-methyl phenylacetic acid are mixed according to the mass ratio of 1:0.6, adding concentrated sulfuric acid with the mass fraction of 98% which is 1.3 times that of 3-hexene-1, 6-diol, and refluxing for 2 hours at 80 ℃ to prepare 3-hexenol methyl phenylacetate; mixing 130 ℃ matrix asphalt with 5% 3-hexenol methyl phenylacetate solution according to a mass ratio of 1:0.6 is put into an emulsifying machine at 75 ℃ to be emulsified for 1h at 100r/min, and emulsified asphalt is prepared;
(4) Under the conditions of 75 ℃ and argon protection, the emulsified asphalt and the functionalized ceramsite are mixed according to the mass ratio of 1:1, mixing uniformly, and adding the components according to the mass ratio of 1:0.4 mixing acetic acid solution with the mass fraction of 42% and concentrated sulfuric acid with the mass fraction of 98%, wherein the mass of the acetic acid solution is 0.4 times that of emulsified asphalt, heating to 110 ℃, stirring for 1h at 400r/min, adding sodium hydroxide with the mass of 0.1 times that of the emulsified asphalt, continuously stirring for 1h, then adding phosphorus trichloride with the mass of 0.8 times that of the emulsified asphalt, heating to 140 ℃, continuously stirring for 11h, cooling to 100 ℃, and mixing according to the mass ratio of 1:0.1 adding aluminum chloride and sodium chloride, wherein the mass of the aluminum chloride is 0.7 times of that of the emulsified asphalt, continuously stirring for 5 hours, adding sodium hydroxide solution with the mass fraction of 20%, cooling to 35 ℃, continuously stirring for 8 hours, adding palladium-carbon with the mass of 0.09 times of that of the emulsified asphalt, introducing hydrogen with the mass of 10 times of that of the emulsified asphalt at 90 ℃ and 2MPa, continuously stirring for 7 hours, continuously stirring for 4 hours after heating to 115 ℃, and then under the condition of 30 ℃, according to the mass ratio of 1:4:9 adding potassium tert-butoxide, methyl triphenyl iodized phosphorus and diethyl ether, wherein the mass of the potassium tert-butoxide is 0.4 time of that of the emulsified asphalt, continuously stirring for 10 hours, adding aluminum oxide 1 time of that of the emulsified asphalt, continuously stirring for 1 hour, adding hydroxyl toluene sulfonyl iodobenzene 0.8 time of that of the emulsified asphalt, continuously stirring for 1 hour at room temperature, and mixing according to the mass ratio of 1:1.5 adding lithium aluminum hydride and aluminum chloride, wherein the mass of the lithium aluminum hydride is 1 time of that of the emulsified asphalt, continuously stirring for 0.8h, adding hydrogen peroxide solution with the mass fraction of 30% and 0.6 time of that of the emulsified asphalt at 0 ℃, continuously stirring for 10h at room temperature, adding sodium sulfite with the mass of 3 times of that of the emulsified asphalt, continuously stirring for 30min, and mixing according to the mass ratio of 1:0.8:3:3 adding triphenyl phosphite, calcium chloride, pyridine and dry N-methyl-2-pyrrolidone, wherein the mass of the triphenyl phosphite is 0.5 times that of the emulsified asphalt, and stirring is continued for 8 hours at 100 ℃ to prepare the semi-flexible asphalt.
Example 2
(1) Under the protection of argon at the temperature, 2-chloro-1, 3-butadiene, terephthalic acid and dimethyl sulfoxide are mixed according to the mass ratio of 1:2.5:10, uniformly mixing, adding aluminum trichloride with the mass of 0.03 times that of 2-chloro-1, 3-butadiene, cooling to 2 ℃, and stirring for 8 hours at 900r/min to obtain butadiene-based terephthalic acid; under the protection of argon at the temperature, ethanol solution of chloroethylene with the mass fraction of 10 percent and 4-methyl phthalonitrile are mixed according to the mass ratio of 1:0.5, adding aluminum trichloride with the mass of 0.04 times that of the 4-methyl phthalonitrile, cooling to 2 ℃, and stirring for 8 hours at 900r/min to prepare vinyl p-methyl phthalonitrile; vinyl p-methyl phthalonitrile, n-hexane and cyclohexane are mixed according to the mass ratio of 1:5:5, uniformly mixing, then cooling to 60 ℃, adding n-butyllithium with the mass of 0.7 times of that of vinyl-p-methylphthalonitrile, stirring for 3 hours at 900r/min, adding butadiene-based terephthalic acid with the mass of 0.6 times of that of vinyl-p-methylphthalonitrile, continuously stirring for 50 minutes, and performing rotary steaming at 1400r/min for 50 minutes at 20Pa and 71 ℃ to obtain styrene-butadiene resin;
(2) Under the conditions of the temperature and the argon protection, shale ceramsite with the particle size of 10mm and phosphoric acid are mixed according to the mass ratio of 1:0.6 and then 2.5m from the bottom 3 Stirring for 40min at 900r/min, adding phosphorus pentoxide at 1.5 times of the mass of the ceramsite, continuously stirring for 2h after heating to 290 ℃, cooling to 70 ℃, adding styrene-butadiene resin at 0.7 times of the mass of the ceramsite, dropwise adding concentrated sulfuric acid at 0.4 times of the mass of the ceramsite at 50 drops/min, continuously stirring for 3h, continuously stirring for 5 times of the mass of the ammonia, adding nano titanium dioxide at 0.07 times of the mass of the propenyl benzoic acid, heating to 90 ℃, and continuously stirring for 3h to obtain the functional ceramsite;
(3) At room temperature, 3-hexene-1, 6-diol and 2-methyl phenylacetic acid are mixed according to the mass ratio of 1:0.7, adding concentrated sulfuric acid with the mass fraction of 98% which is 1.4 times that of 3-hexene-1, 6-diol, and refluxing for 3 hours at 90 ℃ to prepare 3-hexenol methyl phenylacetate; mixing 135 ℃ matrix asphalt with 6 mass percent 3-hexenol methyl phenylacetate solution according to the mass ratio of 1:0.7 is put into an emulsifying machine at 80 ℃ to be emulsified for 2 hours at 200r/min, and emulsified asphalt is prepared;
(4) Under the conditions of 80 ℃ and argon protection, the emulsified asphalt and the functionalized ceramsite are mixed according to the mass ratio of 1:2, uniformly mixing, and adding the components according to the mass ratio of 1:0.5 of mixed acetic acid solution with the mass fraction of 43% and concentrated sulfuric acid with the mass fraction of 98%, wherein the mass of the acetic acid solution is 0.5 times of that of emulsified asphalt, the mixture is stirred for 1.5 hours at 500r/min after the temperature is raised to 120 ℃, then sodium hydroxide with the mass of 0.2 times of that of the emulsified asphalt is added, the mixture is continuously stirred for 2 hours, then phosphorus trichloride with the mass of 0.9 times of that of the emulsified asphalt is added, the mixture is continuously stirred for 12 hours after the temperature is raised to 150 ℃, and then the temperature is lowered to 108 ℃ according to the mass ratio of 1:0.2 adding aluminum chloride and sodium chloride, wherein the mass of the aluminum chloride is 0.8 times of that of the emulsified asphalt, continuously stirring for 6 hours, adding sodium hydroxide solution with the mass fraction of 25%, cooling to 37 ℃, continuously stirring for 8.5 hours, adding palladium-carbon with the mass of 0.1 times of that of the emulsified asphalt, introducing hydrogen with the mass of 15 times of that of the emulsified asphalt at 95 ℃ and 2.5MPa, continuously stirring for 7.5 hours, continuously stirring for 5 hours after heating to 117 ℃, and then stirring for 1 according to the mass ratio under the condition of 40 ℃): 4.5:10 adding potassium tert-butoxide, methyl triphenyl iodized phosphorus and diethyl ether, wherein the mass of the potassium tert-butoxide is 0.5 time of that of the emulsified asphalt, continuously stirring for 12 hours, adding aluminum oxide 2 times of that of the emulsified asphalt, continuously stirring for 2 hours, adding hydroxyl toluene sulfonyl iodobenzene 0.9 time of that of the emulsified asphalt, continuously stirring for 2.5 hours at room temperature, and mixing according to the mass ratio of 1:2 adding lithium aluminum hydride and aluminum chloride, wherein the mass of the lithium aluminum hydride is 1.2 times of that of the emulsified asphalt, continuously stirring for 1h, adding hydrogen peroxide solution with the mass fraction of 30% and the mass of 0.7 times of that of the emulsified asphalt at 2 ℃, continuously stirring for 14h at room temperature, adding sodium sulfite with the mass of 4 times of that of the emulsified asphalt, continuously stirring for 40min, and mixing according to the mass ratio of 1:1:4:4 adding triphenyl phosphite, calcium chloride, pyridine and dry N-methyl-2-pyrrolidone, wherein the mass of the triphenyl phosphite is 0.6 times of that of the emulsified asphalt, and stirring is continued for 11 hours at 125 ℃ to prepare the semi-flexible asphalt.
Example 3
(1) Under the protection of argon at the temperature, 2-chloro-1, 3-butadiene, terephthalic acid and dimethyl sulfoxide are mixed according to the mass ratio of 1:3:11, adding aluminum trichloride with the mass of 0.04 times that of 2-chloro-1, 3-butadiene, cooling to 4 ℃, and stirring for 9 hours at 1000r/min to obtain butadiene-based terephthalic acid; under the protection of argon at the temperature, ethanol solution of 11 percent of chloroethylene and 4-methyl phthalonitrile are mixed according to the mass ratio of 1:0.3, adding aluminum trichloride with the mass of 0.05 times that of the 4-methyl phthalonitrile, cooling to 4 ℃, and stirring for 9 hours at 1000r/min to prepare vinyl p-methyl phthalonitrile; vinyl p-methyl phthalonitrile, n-hexane and cyclohexane are mixed according to the mass ratio of 1:6:6, uniformly mixing, then cooling to 70 ℃, adding n-butyllithium with the mass of 0.8 times of that of vinyl-p-methylphthalonitrile, stirring for 4 hours at 1000r/min, adding butadiene-based terephthalic acid with the mass of 0.7 times of that of vinyl-p-methylphthalonitrile, continuously stirring for 60 minutes, and performing rotary steaming at 1500r/min for 60 minutes at 30Pa and 72 ℃ to obtain styrene-butadiene resin;
(2) Under the conditions of the temperature and the argon protection, shale ceramsite with the grain diameter of 15mm and phosphoric acid are mixed according to the mass ratio of 1:0.7, followed by 3m from the bottom 3 Stirring for 50min at 1000r/min, adding phosphorus pentoxide at 2 times of the mass of the ceramsite, continuously stirring for 2.5h after heating to 300 ℃, cooling to 80 ℃, adding styrene-butadiene resin at 0.8 times of the mass of the ceramsite, dropwise adding concentrated sulfuric acid at 0.5 times of the mass of the ceramsite at 60 drops/min, continuously stirring for 4h, continuously stirring for 6h, adding nano titanium dioxide at 0.08 times of the mass of the propenyl benzoic acid, heating to 100 ℃, and continuously stirring for 4h to obtain the functional ceramsite;
(3) At room temperature, 3-hexene-1, 6-diol and 2-methyl phenylacetic acid are mixed according to the mass ratio of 1:0.8, adding concentrated sulfuric acid with the mass fraction of 98% which is 1.5 times that of 3-hexene-1, 6-diol, and refluxing for 4 hours at 100 ℃ to prepare 3-hexenol methyl phenylacetate; mixing matrix asphalt at 140 ℃ with a 7% 3-hexenol methyl phenylacetate solution according to a mass ratio of 1:0.8 is put into an emulsifying machine at 85 ℃ to be emulsified for 3 hours at 300r/min, and emulsified asphalt is prepared;
(4) Under the conditions of 85 ℃ and argon protection, the emulsified asphalt and the functionalized ceramsite are mixed according to the mass ratio of 1:3, uniformly mixing, and adding the components according to the mass ratio of 1:0.6 of mixed acetic acid solution with the mass fraction of 44% and concentrated sulfuric acid with the mass fraction of 98%, wherein the mass of the acetic acid solution is 0.6 times of that of emulsified asphalt, the mixture is stirred for 2 hours at 600r/min after the temperature is raised to 130 ℃, sodium hydroxide with the mass of 0.3 times of that of the emulsified asphalt is added, the mixture is continuously stirred for 3 hours, phosphorus trichloride with the mass of 1 time of that of the emulsified asphalt is added, the mixture is continuously stirred for 13 hours after the temperature is raised to 160 ℃, and the temperature is reduced to 115 ℃ according to the mass ratio of 1:0.3 adding aluminum chloride and sodium chloride, wherein the mass of the aluminum chloride is 0.9 times of that of the emulsified asphalt, continuously stirring for 7 hours, adding sodium hydroxide solution with the mass fraction of 30%, cooling to 40 ℃, continuously stirring for 9 hours, adding palladium-carbon with the mass of 0.11 times of that of the emulsified asphalt, introducing hydrogen with the mass of 20 times of that of the emulsified asphalt at 100 ℃ and 3MPa, continuously stirring for 8 hours, continuously stirring for 6 hours after heating to 119 ℃, and then under the condition of 50 ℃, stirring according to the mass ratio of 1:5:11 adding potassium tert-butoxide, methyl triphenyl iodized phosphorus and diethyl ether, wherein the mass of the potassium tert-butoxide is 0.6 times of that of the emulsified asphalt, continuously stirring for 14h, adding aluminum oxide 3 times of that of the emulsified asphalt, continuously stirring for 3h, adding hydroxyl toluene sulfonyl iodibenzene 1 time of that of the emulsified asphalt, continuously stirring for 4h at room temperature, and mixing according to the mass ratio of 1:3 adding lithium aluminum hydride and aluminum chloride, wherein the mass of the lithium aluminum hydride is 1.4 times of that of the emulsified asphalt, continuously stirring for 1.2 hours, adding hydrogen peroxide solution with the mass fraction of 30% and 0.8 time of that of the emulsified asphalt at the temperature of 4 ℃, continuously stirring for 18 hours at room temperature, adding sodium sulfite with the mass of 5 times of that of the emulsified asphalt, continuously stirring for 50 minutes, and mixing according to the mass ratio of 1:1.2:5:5 adding triphenyl phosphite, calcium chloride, pyridine and dry N-methyl-2-pyrrolidone, wherein the mass of the triphenyl phosphite is 0.7 times that of the emulsified asphalt, and stirring is continued for 14 hours at 150 ℃ to prepare the semi-flexible asphalt.
Comparative example 1
Comparative example 1 differs from example 2 only in the difference of step (2), the step (2) was modified as: under the conditions of the temperature and the argon protection, shale ceramsite with the particle size of 10mm and styrene-butadiene resin are mixed according to the mass ratio of 1:0.7, heating to 70 ℃, dropwise adding concentrated sulfuric acid with the mass fraction of 98% and the mass fraction of 0.4 times of that of the ceramsite at 50 drops/min, continuously stirring for 3 hours, continuously blowing ammonia with the mass of 5 times of that of the ceramsite, then adding nano titanium dioxide with the mass of 0.07 times of that of propenyl benzoic acid, heating to 90 ℃, and continuously stirring for 3 hours to obtain the functionalized ceramsite. The remaining preparation steps were the same as in example 2.
Comparative example 2
Comparative example 2 differs from example 2 only in the difference of step (2), the step (2) was modified as: under the conditions of the temperature and the argon protection, shale ceramsite with the particle size of 10mm and phosphoric acid are mixed according to the mass ratio of 1:0.6 and then 2.5m from the bottom 3 And (3) bubbling ammonia gas with the mass of 0.35 times of that of the ceramsite in the reactor per minute, stirring for 40 minutes at 900r/min, adding phosphorus pentoxide with the mass of 1.5 times of that of the ceramsite, continuously bubbling ammonia gas with the mass of 5 times of that of the ceramsite, heating to 290 ℃, and continuously stirring for 2 hours to obtain the functional ceramsite. The remaining preparation steps were the same as in example 2.
Comparative example 3
Comparative example 3 differs from example 2 only in the difference of step (2), the modification of step (2) to: under the conditions of the temperature and the argon protection, shale ceramsite with the particle size of 10mm and phosphoric acid are mixed according to the mass ratio of 1: mixing 0.6, stirring for 40min at 900r/min, adding phosphorus pentoxide with the mass of 1.5 times of that of the ceramsite, heating to 290 ℃, continuously stirring for 2h, cooling to 70 ℃, adding styrene-butadiene resin with the mass of 0.7 times of that of the ceramsite, dripping concentrated sulfuric acid with the mass fraction of 98% with the mass of 0.4 times of that of the ceramsite at 50 drops/min, continuously stirring for 3h, adding nano titanium dioxide with the mass of 0.07 times of that of propenyl benzoic acid, heating to 90 ℃, and continuously stirring for 3h to obtain the functional ceramsite. The remaining preparation steps were the same as in example 2.
Comparative example 4
Comparative example 4 differs from example 2 only in the difference of step (4), the modification of step (4) to: under the conditions of 80 ℃ and argon protection, the mass ratio of the matrix asphalt to the functionalized ceramsite is 1:2, uniformly mixing, and adding the components according to the mass ratio of 1:0.5 of mixed acetic acid solution with the mass fraction of 43% and concentrated sulfuric acid with the mass fraction of 98%, wherein the mass of the acetic acid solution is 0.5 times of the mass of matrix asphalt, the mixture is stirred for 1.5 hours at 500r/min after the temperature is raised to 120 ℃, then sodium hydroxide with the mass of 0.2 times of the mass of the matrix asphalt is added, the mixture is continuously stirred for 2 hours, then phosphorus trichloride with the mass of 0.9 times of the mass of the matrix asphalt is added, the mixture is continuously stirred for 12 hours after the temperature is raised to 150 ℃, and then the temperature is lowered to 108 ℃ according to the mass ratio of 1:0.2 adding aluminum chloride and sodium chloride, wherein the mass of the aluminum chloride is 0.8 times of that of the matrix asphalt, continuously stirring for 6 hours, adding sodium hydroxide solution with the mass fraction of 25%, cooling to 37 ℃, continuously stirring for 8.5 hours, adding palladium-carbon with the mass of 0.1 times of that of the matrix asphalt, introducing hydrogen with the mass of 15 times of that of the matrix asphalt at 95 ℃ and 2.5MPa, continuously stirring for 7.5 hours, continuously stirring for 5 hours after heating to 117 ℃, and then stirring for 1 according to the mass ratio under the condition of 40 ℃): 4.5:10 adding potassium tert-butoxide, methyl triphenyl iodized phosphorus and diethyl ether, wherein the mass of the potassium tert-butoxide is 0.5 times of that of the matrix asphalt, continuously stirring for 12 hours, adding aluminum oxide with the mass of 2 times of that of the matrix asphalt, continuously stirring for 2 hours, adding hydroxyl toluene sulfonyl iodobenzene with the mass of 0.9 times of that of the matrix asphalt, continuously stirring for 2.5 hours at room temperature, and mixing according to the mass ratio of 1:2 adding lithium aluminum hydride and aluminum chloride, wherein the mass of the lithium aluminum hydride is 1.2 times of that of the matrix asphalt, continuously stirring for 1h, adding hydrogen peroxide solution with the mass fraction of 30% and 0.7 time of that of the matrix asphalt at 2 ℃, continuously stirring for 14h at room temperature, adding sodium sulfite with the mass of 4 times of that of the matrix asphalt, continuously stirring for 40min, and mixing according to the mass ratio of 1:1:4:4 adding triphenyl phosphite, calcium chloride, pyridine and dry N-methyl-2-pyrrolidone, wherein the mass of the triphenyl phosphite is 0.6 times of that of the matrix asphalt, and stirring is continued for 11 hours at 125 ℃ to prepare the semi-flexible asphalt. The remaining preparation steps were the same as in example 2.
Effect example
The following table 1 shows the results of analysis of the compressive resistance, rutting resistance and low temperature cracking resistance of the semi-flexible asphalt prepared by using examples 1 to 3 of the present invention and comparative examples 1 to 4.
TABLE 1
From Table 1, it can be found that the semi-flexible asphalt prepared in examples 1, 2 and 3 is strong in compression resistance, rutting resistance and low-temperature cracking resistance; from comparison of experimental data of examples 1, 2 and 3 and comparative example 1, it can be found that ammonium phosphate can be formed by preparing functionalized ceramsite by using phosphoric acid, and then the semi-flexible asphalt can be prepared into the polyamide containing dibenzo-octamembered ring structure, so that the prepared semi-flexible asphalt has stronger compression resistance, rutting resistance and low-temperature cracking resistance; from the experimental data of examples 1, 2 and 3 and comparative example 2, it can be found that the use of styrene-butadiene resin to prepare functionalized ceramsite can form ammonium phosphate, and when semi-flexible asphalt is prepared subsequently, the semi-flexible asphalt can form polyarylamide containing dibenzo-octamembered ring structure, and the prepared semi-flexible asphalt has stronger compression resistance and low temperature cracking resistance; from the experimental data of examples 1, 2 and 3 and comparative example 3, it can be found that ammonium phosphate can be formed by preparing semi-flexible asphalt using functionalized ceramsite prepared by ammonia bubbling and hot mixing, and then, when the semi-flexible asphalt is prepared, a poly (aryl amide) containing dibenzo-octant ring structure can be formed, so that the compression resistance and the low-temperature cracking resistance are stronger; from the experimental data of examples 1, 2, 3 and comparative example 4, it was found that a semi-flexible asphalt prepared using emulsified asphalt can form a polyarylamide having a dibenzo-octamembered ring structure, and the prepared asphalt has a strong rutting resistance and a strong low-temperature cracking resistance.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.

Claims (1)

1. The semi-flexible asphalt is characterized by being prepared by mixing emulsified asphalt and functionalized ceramsite;
the emulsified asphalt is prepared by the following method: mixing 130-140 ℃ matrix asphalt with 5-7% of 3-hexenol methyl phenylacetate solution according to a mass ratio of 1: 0.6-1: 0.8 is put into an emulsifying machine at the temperature of 75-85 ℃ to be emulsified for 1-3 hours at the speed of 100-300 r/min, so that emulsified asphalt is prepared;
the 3-hexenol methyl phenylacetate is prepared by the following steps of: 0.6-1: 0.8, uniformly mixing, adding concentrated sulfuric acid with the mass fraction of 98% which is 1.3-1.5 times that of 3-hexene-1, 6-diol, and refluxing at 80-100 ℃ for 2-4 hours to obtain 3-hexenol methyl phenylacetate;
the functional ceramsite is prepared by mixing styrene-butadiene resin, phosphoric acid and ceramsite and stirring by using ammonia bubbling heat;
the styrene-butadiene resin is prepared by the following method, and under the conditions of room temperature and argon protection, an ethanol solution of 9-11% of chloroethylene and 4-methyl phthalonitrile are mixed according to the mass ratio of 1: 0.2-1: 0.3, uniformly mixing, adding aluminum trichloride with the mass which is 0.03-0.05 times that of 4-methyl phthalonitrile, cooling to 0-4 ℃, and stirring for 7-9 hours at 800-1000 r/min to obtain vinyl p-methyl phthalonitrile; under the protection of argon at the temperature, 2-chloro-1, 3-butadiene, terephthalic acid and dimethyl sulfoxide are mixed according to the mass ratio of 1:2:9~1:3:11, adding aluminum trichloride with the mass of 0.02-0.04 times of that of 2-chloro-1, 3-butadiene, cooling to 0-4 ℃, and stirring for 7-9 hours at 800-1000 r/min to obtain butadiene-based terephthalic acid; under the conditions of 70-80 ℃ and argon protection, vinyl p-methyl phthalonitrile, n-hexane and cyclohexane are mixed according to the mass ratio of 1:4: 4-1: 6:6, uniformly mixing, cooling to 50-70 ℃, adding n-butyllithium with the mass of 0.6-0.8 times of that of vinyl-p-methylphthalonitrile, stirring for 2-4 hours at 800-1000 r/min, adding butadiene-based terephthalic acid with the mass of 0.5-0.7 times of that of vinyl-p-methylphthalonitrile, continuously stirring for 40-60 minutes, and performing rotary steaming at 1300-1500 r/min for 40-60 minutes at 10-30 Pa and 70-72 ℃ to obtain styrene-butadiene resin;
the semi-flexible asphalt is prepared by the following method: under the conditions of 75-85 ℃ and argon protection, the emulsified asphalt and the functionalized ceramsite are mixed according to the mass ratio of 1: 1-1: 3, uniformly mixing, and adding the components according to the mass ratio of 1: 0.4-1: 0.6 of mixed acetic acid solution with the mass fraction of 42-44% and concentrated sulfuric acid with the mass fraction of 98%, wherein the mass of the acetic acid solution is 0.4-0.6 times of the mass of emulsified asphalt, stirring for 1-2 h at 400-600 r/min after the temperature is raised to 110-130 ℃, adding sodium hydroxide with the mass of 0.1-0.3 times of the mass of the emulsified asphalt, continuously stirring for 1-3 h, then adding phosphorus trichloride with the mass of 0.8-1 time of the mass of the emulsified asphalt, continuously stirring for 11-13 h after the temperature is raised to 140-160 ℃, cooling to 100-115 ℃, and mixing the materials according to the mass ratio of 1: 0.1-1: 0.3, adding aluminum chloride and sodium chloride, wherein the mass of the aluminum chloride is 0.7-0.9 times of that of the emulsified asphalt, continuously stirring for 5-7 hours, adding a sodium hydroxide solution with the mass fraction of 20-30%, cooling to 35-40 ℃, continuously stirring for 8-9 hours, adding palladium carbon with the mass of 0.09-0.11 times of that of the emulsified asphalt, introducing hydrogen with the mass of 10-20 times of that of the emulsified asphalt at 90-100 ℃ and 2-3 MPa, continuously stirring for 7-8 hours, continuously stirring for 4-6 hours after the temperature is raised to 115-119 ℃, and then under the condition of 30-50 ℃, according to the mass ratio of 1:4:9~1:5:11 adding potassium tert-butoxide, methyl triphenyl iodized phosphorus and diethyl ether, wherein the mass of the potassium tert-butoxide is 0.4-0.6 times of that of emulsified asphalt, continuously stirring for 10-14 h, adding aluminum oxide 1-3 times of that of the emulsified asphalt, continuously stirring for 1-3 h, adding hydroxyl toluene sulfonyl iodibenzene 0.8-1 time of that of the emulsified asphalt, continuously stirring for 1-4 h at room temperature, and mixing according to the mass ratio of 1: 1.5-1: 3 adding lithium aluminum hydride and aluminum chloride, wherein the mass of the lithium aluminum hydride is 1-1.4 times of that of the emulsified asphalt, continuously stirring for 0.8-1.2 h, adding a 30% hydrogen peroxide solution with the mass fraction of 0.6-0.8 times of that of the emulsified asphalt at 0-4 ℃, continuously stirring for 10-18 h at room temperature, adding sodium sulfite with the mass of 3-5 times of that of the emulsified asphalt, continuously stirring for 30-50 min, and mixing according to the mass ratio of 1:0.8:3: 3-1: 1.2:5: and 5, adding triphenyl phosphite, calcium chloride, pyridine and dry N-methyl-2-pyrrolidone, wherein 0.5-0.7 times of the mass of the triphenyl phosphite emulsified asphalt is continuously stirred for 8-14 hours at 100-150 ℃ to prepare the semi-flexible asphalt.
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