CN105585854B - A kind of high-viscosity modified asphalt and preparation method thereof for being easy to construct - Google Patents
A kind of high-viscosity modified asphalt and preparation method thereof for being easy to construct Download PDFInfo
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Abstract
The present invention relates to a kind of asphaltum with high viscosity for being easy to construct and preparation methods.The asphaltum with high viscosity includes 100 parts of high asphalt content matrix pitch, 0.2~1.2 part of polyphosphoric acids, increases and prolong 2 ~ 15 parts of agent mother liquor, higher aliphatic by weight: 0.1~0.8 part, 0.5~5 part of compound adjusting adhesive, and 0.1~0.5 part of silane coupling agent.Wherein compound adjusting adhesive is the mesopore molecular sieve for the polyethylene wax cladding being grafted by epoxy, and weight ratio is 60/40~50/50.Modified pitch of the present invention, 60 DEG C of dynamic viscosity height, low-temperature ductility is big, has both excellent high-temperature stability and low-temperature cracking-resistance, tired ageing properties and water resistant is resisted to encroach on energy, and more particularly its high temperature viscosity is relatively low, and construction mix temperature is lower, is easy to construct.
Description
Technical field
The invention belongs to asphalt fields, more particularly to a kind of high-viscosity modified asphalt for being easy to construct and its preparation
Method.
Background technique
The increasingly increase carried with the volume of traffic and axis and summer high temperature are prominent, and bituminous pavement is total to because what high temperature and wheel rolled
Mobility caused by same-action is destroyed and canalized traffic is on the rise, and harsher requirement is proposed to road asphalt material.Both
Guarantee that bituminous pavement under high temperature, acts on the plastic flow deformation being not likely to produce in wheel load or shearing becomes during the broiling summer
Shape guarantees that bituminous pavement has preferable crack resistance at low-temperature to enhance the ability of the permanent lesions such as its Rut resistance again.Cause
This, people have been devoted to the exploitation of the high-viscosity modified asphalt of function admirable for many years.
CN103819918A provides a kind of compound high-viscosity modified asphalt and preparation method, the high-viscosity modified asphalt with
Weight percent meter includes heavy traffic asphaltum 84~88, modified composite 12~16, and preparation method is first by SBS, desulfurization micelle
With the mixed and modified compound of compatilizer containing epoxy group, modified particle is made after mechanical pelleting, then the modified particle is added
Enter into 170~190 DEG C of pitch 30~60min of high speed shear in high-shear emulsion machine, becomes composite modified particle fusion
Carefully, it is then transferred to and is dispersed with stirring to obtain compound high-viscosity modified asphalt in high speed disperser, there is stable storing, high temperature performance
Excellent feature, the disadvantage is that the invention high-viscosity modified asphalt high temperature viscosity is larger, 135 DEG C of viscosity are greater than 3Pa.s, need compared with
High mix and compacting temperature, constructional difficulties, and it is unfavorable for environmental protection.
CN103073748A discloses a kind of warm-mixed asphalt and preparation method thereof, which includes base in mass ratio
Plinth pitch 85-97, polymer 1-10 and composite modifier 0.1-1.5.The composite modifier is by double-(γ-triethoxy silicon substrate
Propyl) tetrasulfide is formed with mesopore molecular sieve, wherein the mass parts ratio of the tetrasulfide and mesopore molecular sieve is 1:
0.1-5.The needle penetration of its provided warm-mixed asphalt has reached the requirement of No. 70 pitch, but its low-temperature ductility is unsatisfactory, no
High and low temperature performance can be combined.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of high-viscosity modified asphalt for being easy to construct and its preparation sides
Method.To improve 60 DEG C of dynamic viscosities of high-viscosity modified asphalt, increase low-temperature ductility, improves high and low temperature service performance, reduce simultaneously
The high temperature viscosity of high-viscosity modified asphalt, when to be applied to asphalt mixture mixing, mix temperature is lower, is easy to construct.
The asphaltum with high viscosity for being easy to construct of the invention, includes following components by weight:
Matrix pitch: 100 parts；
Polyphosphoric acids: 0.2~1.2 part, preferably 0.3~1.0 part；
Agent mother liquor: 2~15 parts, preferably 3~12 parts is prolonged in increasing；
Higher aliphatic: 0.1~0.8 part, preferably 0.2~0.6 part；
Compound adjusting adhesive: 0.5~5 part, preferably 1~3 part；
Silane coupling agent: 0.1~0.5 part；It is preferred that 0.2~0.4 part.
Wherein, the compound adjusting adhesive is the mesopore molecular sieve for the polyethylene wax cladding being grafted by epoxy.Epoxy grafting
Polyethylene wax and mesopore molecular sieve be by ratio of weight and the number of copies 60/40~50/50.The preparation process of the compound adjusting adhesive are as follows:
By ratio of weight and the number of copies it is 60/40~50/50 premix by the polyethylene wax of epoxy grafting and mesopore molecular sieve, is stirred in 90~110 DEG C
It mixes and is mixed 20~40min, be cooled to room temperature obtained.The wherein polyethylene wax of epoxy grafting, GMA grafting rate > 2%, fusing point 90 ± 2
DEG C, mesopore molecular sieve can be MCM-41, MCM-22, MCM-48, SBA-15 and/or SBA-16；The mesopore molecular sieve aperture 1~
20nm, specific surface area 300m2/ g~1200m2/g。
In asphaltum with high viscosity of the present invention, the matrix pitch is straight asphalt, the oxidized asphalt or molten of high bitumen content
One or more of agent depitching mixing, preferably asphalt content are 15wt%~25wt%, and 25 DEG C of needle penetrations are 40~80
The matrix pitch of 1/10mm.
In asphaltum with high viscosity of the present invention, the polyphosphoric acids can be P2O5Content >=80wt% technical grade or SILVER REAGENT
Compound, preferably P2O5Content >=83wt% polyphosphoric acid product, such as P2O5Content >=83wt% technical grade polyphosphoric acids and P2O5
Content >=84wt% food-grade polyphosphoric acids.
In high-viscosity modified asphalt of the present invention, it is the butadiene-styrene rubber (SBR) by 5wt%~15wt% that agent mother liquor is prolonged in the increasing
Or butadiene-styrene rubber particle and 85wt%~95wt% extraction oil form, and are prepared according to conventional method in that art, such as pass through high speed
Homogeneous mother liquor is made in shearing or stirring；Wherein SBR is this field conventional products, such as commercially available various products SBR-1502 and SBR-
1500 etc.；Extraction oil is the line that subtracts four of lubricating oil furfural (or phenol) purification and subtracts three line extracts or mixtures thereof oil, preferred fragrance out
The line that the subtracts four extraction oil of 50% or more hydrocarbon content.
In high-viscosity modified asphalt of the present invention, higher aliphatic C8~C22Fatty alcohol, preferably C12~C18Fat
Alcohol, such as one or both of lauryl alcohol, tetradecyl alchohol, hexadecanol and octadecyl alcolol mixture.
In high-viscosity modified asphalt of the present invention, the coupling agent is silane coupling agent, such as amino silane, methyl acetyl
At least one such as silane, epoxy radicals silicone hydride, sulfenyl silane and vinyl silanes.
The preparation method of the high-viscosity modified asphalt for being easy to construct of the invention, including following content:
(1) polyphosphoric acids is added in the matrix pitch of molten state, carries out chemical modification reaction；
(2) it is added to increase into step (1) material and prolongs agent mother liquor, the reaction was continued；
(3) higher aliphatic is added into step (2) material, the reaction was continued；
(4) compound adjusting adhesive and coupling agent is added into step (3) material, the reaction was continued a period of time, and easily construction is made
High-viscosity modified asphalt.Wherein compound adjusting adhesive is the mesopore molecular sieve for the polyethylene wax cladding being grafted by epoxy, and epoxy connects
The polyethylene wax and mesopore molecular sieve of branch are 60/40~50/50 by ratio of weight and the number of copies.The preparation process of compound adjusting adhesive is that will refer to
The polyethylene wax and mesopore molecular sieve for determining the epoxy grafting of parts by weight premix, and are stirred 20-40min in 90~110 DEG C, cooling
It is made to room temperature.
Wherein, the temperature of the matrix pitch of molten state described in step (1) is 140~160 DEG C；Reaction temperature be 145~
185 DEG C, preferably 150~170 DEG C, reaction time are 30~200 minutes.
Reaction temperature described in step (2) is 140~180 DEG C, and preferably 150~165 DEG C, the reaction time is 30~150 minutes.
Reaction temperature described in step (3) is 140~200 DEG C, and preferably 150~170 DEG C, the reaction time is 10~30 minutes
Reaction temperature described in step (4) is 120~150 DEG C, and the reaction time is 20~60 minutes.
In the method for the present invention, the mixing of material can be using technologies such as standard machinery stirring, high shear, colloid mill or ultrasounds
Means, mixed process are as far as possible uniformly mixed material, sufficiently react.
High-viscosity modified asphalt of the present invention, by polyphosphoric acids to the matrix pitch chemical modification of high asphalt content and increasing
Prolong the collective effect of agent mother liquor, 60 DEG C of dynamic viscosities of the high-viscosity modified asphalt product can be made to reach 20000Pa.s or more, together
When there is biggish low-temperature ductility again, have both excellent high and low temperature service performance；A small amount of advanced rouge is also introduced in the present invention
Fat alcohol, it occurs esterification with the complete polyphosphoric acids of a small amount of unreacted and generates alkyl phosphate, prevents polyphosphoric acids and drip
Green the reaction was continued, and the alkyl phosphate generated has certain peptization to asphalitine, keeps asphaltic products performance more stable；It is even
Connection agent can promote to form the good chemisorption of adhesion strength high-durability between pitch and building stones, significantly improve the anti-of bituminous pavement
Water Damages energy；In high-viscosity modified asphalt more particularly of the present invention, it is added to compound adjusting adhesive, it is grafted by epoxy
Polyethylene wax and mesopore molecular sieve composition, wherein the polyethylene wax of epoxy grafting has better suited fusing point (lower than 10 DEG C of water boiling point
Left and right), can be before the moisture in molecular sieve largely vaporize by its effective latching, and high temperature performance of asphalt is not influenced, it connects simultaneously
The wax and bitumen compatibility of branch are more preferable, influence on pitch cryogenic property small；Mesopore molecular sieve is because having biggish specific surface area and fitting
In aperture, have a stronger adsorptivity, a certain amount of hydrone of absorption in duct is located in advance by the polyethylene wax that epoxy is grafted
Reason, molecular sieve are coated by cere and lock moisture, and when temperature increases, the polyethylene wax of the low epoxy grafting of fusing point can dissolve into liquid completely
State is dissolved into pitch, and the high temperature viscosity of pitch is reduced；The moisture of mesopore molecular sieve association absorption at this time also can melting with wax
Change gradually discharges, and fine foam is generated in pitch, makes pitch volume expansion, reduces the viscosity of pitch, two kinds of substances it is compound
Using the high temperature viscosity for not only dripping high adhered modification significantly reduces, and improves the construction workability of high-viscosity modified asphalt；And it is right
The high-temperature behavior of asphalt has certain improvement result, while not influencing the low temperature service performance of asphalt again.
High-viscosity modified asphalt of the present invention covers the additives such as agent according to needing that age resister, antistripping agent, light can also be added.
60 DEG C of dynamic viscosity high and low temperature ductilities of high-viscosity modified asphalt of the present invention are big, storage is stablized, and high and low temperature uses
It has excellent performance, and can be easy to construct under relatively low temperature with building stones mix.Be particularly suitable for summer high temperature, humid area and
The big regional heavy traffic road making of day and night temperature, is effectively prevented pavement track, gathers around packet, fatigue cracking, cold cracking and water
The common pavement destruction such as infringement occurs, prolonging service life of pavement.Asphaltum with high viscosity production method of the present invention is simple, without special
Equipment, construction temperature is lower, and energy consumption is small, and the discharge of the pernicious gases such as smog is less, is conducive to environmental protection.
Specific embodiment
For a better understanding of the present invention, carry out the present invention is further explained content, these embodiments below with reference to embodiment
It does not provide constraints to the present invention.
It is as shown in table 1 to be directed to matrix pitch property；Polyphosphoric acids is the production of Shouguang City Hao Gang Chemical Co., Ltd.
Technical grade polyphosphoric acids, P2O5Content >=83%, viscosity are 35000 centipoises；To prolong agent be butadiene-styrene rubber (SBR) content is 10wt% for increasing
Mother liquor, wherein the butadiene-styrene rubber (SBR) used be China Petroleum Jilin Petrochemical company production SBR-1500；Extracting oil out is
The line furfural exquisiteness that the subtracts four extraction oil of Jingmen petrochemical iy produced, arene content 55%；Higher aliphatic is Malaysia Emery chemistry
The tetradecyl alchohol and hexadecanol of product company, content > 99.5%；Compound adjusting adhesive is the polyethylene wax and mesoporous molecular being grafted by epoxy
Screen banks is at weight ratio is 60/40~50/50, wherein the limited public affairs of the extra large high molecular material in polyethylene wax Hangzhou of epoxy grafting
Department's production, GMA grafting rate > 2%, 90 ± 2 DEG C of fusing point；Mesopore molecular sieve is Nanjing Xian Feng Nono-material Science & Technology Ltd.
3.5~4nm of the aperture MCM-41(, specific surface area > 800m2/ g) and 6~8nm of the aperture SBA-15(, specific surface area > 650m2/ g).
Coupling agent is the silane coupling agent KH-560 of the previous Chemical Co., Ltd.'s production in Nanjing.
Embodiment 1
It is respectively by ratio of weight and the number of copies 60/40,55/45 and 50/50 by the polyethylene wax of epoxy grafting and mesopore molecular sieve
Premix, is stirred 25min in 100 DEG C, is cooled to room temperature and compound adjusting adhesive is made.
Matrix pitch is heated to 150 DEG C, until melting trickling state, takes 100 parts of matrix pitches to be sent into reactor tank, and open
Dynamic blender, maintains 160 DEG C for reactor tank temperature, 0.3 part of polyphosphoric acids is added in reactor tank, low whipping speed 2000
It is reacted 80 minutes under the conditions of rev/min, agent mother liquor is prolonged in 3.0 parts of increasing, continues high-speed stirred and reacts 60 minutes, is then added 0.2
The hexadecanol of part is stirred to react 15 minutes, 1.0 parts of compound adjusting adhesives and 0.2 part of silane coupling agent is then added, is stirred to react 30
Minute, high-viscosity modified asphalt of the present invention is made；Wherein the group of compound adjusting adhesive becomes epoxidation grafted polyethylene wax 40%,
MCM-41 molecular sieve 60%.High adhered modification asphaltic products fundamental property and minimum mix temperature (referring to viscosity-temperature curve) are shown in Table 2.
Embodiment 2
High-viscosity modified asphalt is prepared according to 1 preparation method of embodiment, specific component proportion is as follows:
100 parts of matrix pitch
0.6 part of polyphosphoric acids
Increasing prolongs 6.0 parts of agent mother liquor
0.3 part of hexadecanol,
2.0 parts of compound adjusting adhesive,
0.3 part of silane coupling agent.
Wherein the group of compound adjusting adhesive becomes epoxidation grafted polyethylene wax 60%, and MCM-41 molecular sieve 40%, product is basic
Property is shown in Table 2.
Embodiment 3
High-viscosity modified asphalt is prepared according to 2 preparation method of embodiment, the difference is that the group of compound adjusting adhesive becomes epoxy
Change grafted polyethylene wax 50%, MCM-41 molecular sieve 50%, product property is shown in Table 2.
Embodiment 4
High-viscosity modified asphalt is prepared according to 2 preparation method of embodiment, the difference is that the group of compound adjusting adhesive becomes epoxy
Change grafted polyethylene wax 55%, SBA-15 molecular sieve 45%, product property is shown in Table 2.
Embodiment 5
High-viscosity modified asphalt is prepared according to 2 preparation method of embodiment, the difference is that the group of compound adjusting adhesive becomes epoxy
Change grafted polyethylene wax 50%, SBA-15 molecular sieve 50%.Its product property is shown in Table 2.
Embodiment 6
High-viscosity modified asphalt is prepared according to 1 preparation method of embodiment, specific component proportion is as follows:
100 parts of matrix pitch
0.8 part of polyphosphoric acids
Increasing prolongs 10 parts of agent mother liquor
0.4 part of hexadecanol,
3.0 parts of compound adjusting adhesive,
0.4 part of silane coupling agent.
Wherein the group of compound adjusting adhesive becomes epoxidation grafted polyethylene wax 50%, and MCM-41 molecular sieve 50%, product is basic
Property is shown in Table 2.
Embodiment 7
High-viscosity modified asphalt is prepared according to 1 preparation method of embodiment, specific component proportion is as follows:
100 parts of matrix pitch
1.0 parts of polyphosphoric acids
Increasing prolongs 12 parts of agent mother liquor
0.2 part of tetradecyl alchohol
0.4 part of hexadecanol,
3.0 parts of compound adjusting adhesive,
0.4 part of silane coupling agent.
Wherein the group of compound adjusting adhesive becomes epoxidation grafted polyethylene wax 50%, and MCM-41 molecular sieve 50%, product is basic
Property is shown in Table 2.
Comparative example 1
High-viscosity modified asphalt is prepared according to 6 preparation method of embodiment, the difference is that it is pure and mild compound not add higher aliphatic
Adjusting adhesive.Comparison asphaltic nature is shown in Table 2.
Comparative example 2
High-viscosity modified asphalt is prepared according to 6 preparation method of embodiment, the difference is that it is added without compound adjusting adhesive, comparison drip
Green product property is shown in Table 2.
Comparative example 3
High-viscosity modified asphalt is prepared according to 3 preparation method of embodiment, the difference is that it is added without higher aliphatic, comparison drip
Green product property is shown in Table 2.
1 matrix pitch property of table
| Number | Basic asphalt |
| Needle penetration (25 DEG C)/1/10mm | 60 |
| Softening point/DEG C | 57.1 |
| Ductility (10 DEG C)/cm | 5 |
| 60 DEG C of dynamic viscosity/Pa.s | 1026 |
| Asphalt content, % | 22.05 |
2 embodiment of table and comparative example asphaltic nature
| Project | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Example 7 | Than 1 | Than 2 | Than 3 |
| 25 DEG C of needle/1/10mm | 45 | 48 | 47 | 48 | 46 | 44 | 43 | 41 | 46 | 43 |
| Softening point/DEG C | 80.5 | 85.3 | 86.5 | 84.8 | 86.3 | 88.9 | 90.5 | 92.1 | 85.6 | 88.7 |
| 10 DEG C of ductility/cm | > 100 | > 100 | > 100 | > 100 | > 100 | > 100 | 97 | 91 | > 100 | 92 |
| 60 DEG C of viscous/Pa.s | 22286 | 39017 | 38798 | 39987 | 40008 | 53978 | 62918 | 52918 | 51806 | 41387 |
| 135 DEG C of viscous/mPa.s | 1026 | 1824 | 1801 | 1815 | 1835 | 1896 | 2789 | 4723 | 4273 | 1858 |
| Penetration ratio, % are remained after TFOT | 80 | 84 | 85 | 84 | 83 | 88 | 91 | 59 | 80 | 64 |
| Minimum mix temperature/DEG C | 156 | 161 | 160 | 161 | 162 | 163 | 170 | 220 | 195 | 164 |
The present invention is easy to the high adhered modification pitch constructed it can be seen from 2 data of table, and 60 DEG C of dynamic viscosities are big, softening point
High and low temperature ductility is big, and TFOT remains penetration ratio height, has excellent high-temperature stability, ageing resistance and low-temperature cracking-resistance
Can, and mix temperature is low, construction workability is good, is easy to construct.
Claims (16)
1. a kind of asphaltum with high viscosity for being easy to construct, it is characterised in that: by weight include following components:
Matrix pitch: 100 parts；
Polyphosphoric acids: 0.2~1.2 part；
Increase and prolong agent mother liquor: 2~15 parts；
Higher aliphatic: 0.1~0.8 part；
Compound adjusting adhesive: 0.5~5 part；
Silane coupling agent: 0.1~0.5 part；
The compound adjusting adhesive is the mesopore molecular sieve for the polyethylene wax cladding being grafted by epoxy, the poly- second of the epoxy grafting
Alkene wax and mesopore molecular sieve are 60/40~50/50 by ratio of weight and the number of copies；It is the fourth by 5wt%~15wt% that agent mother liquor is prolonged in the increasing
Benzene rubber or butadiene-styrene rubber particle and 85wt%~95wt% extraction oil composition；The higher aliphatic is selected from C8~C22Fat
Alcohol.
2. the asphaltum with high viscosity described in accordance with the claim 1 for being easy to construct, it is characterised in that: wherein:
Polyphosphoric acids: 0.3~1.0 part；
Increase and prolong agent mother liquor: 3~12 parts；
Higher aliphatic: 0.2~0.6 part；
Compound adjusting adhesive: 1~3 part；
Silane coupling agent: 0.2~0.4 part.
3. the asphaltum with high viscosity described in accordance with the claim 1 for being easy to construct, it is characterised in that: the preparation of the compound adjusting adhesive
Process are as follows: it by the polyethylene wax of epoxy grafting and mesopore molecular sieve is by ratio of weight and the number of copies 60/40~50/50 premix, in 90~
110 DEG C of stirrings are mixed 20~40min, are cooled to room temperature obtained.
4. the asphaltum with high viscosity described in accordance with the claim 1 for being easy to construct, it is characterised in that: the wherein polyethylene of epoxy grafting
Wax, GMA grafting rate > 2%, 90 ± 2 DEG C of fusing point.
5. the asphaltum with high viscosity described in accordance with the claim 1 for being easy to construct, it is characterised in that: the mesopore molecular sieve is MCM-
41, MCM-22, MCM-48, SBA-15 or SBA-16.
6. the asphaltum with high viscosity described in accordance with the claim 1 for being easy to construct, it is characterised in that: the mesopore molecular sieve aperture 1
~20nm, specific surface area 300m2/ g~1200m2/g。
7. the asphaltum with high viscosity described in accordance with the claim 1 for being easy to construct, it is characterised in that: the matrix pitch is asphalitine
Content is 15wt%~25wt%, straight asphalt, oxidized asphalt or the solvent deasphalting that 25 DEG C of needle penetrations are 40~80 1/10mm
One or more of mixing.
8. the asphaltum with high viscosity described in accordance with the claim 1 for being easy to construct, it is characterised in that: the polyphosphoric acids is P2O5Contain
The compound of amount >=80wt% technical grade or SILVER REAGENT.
9. being easy to the asphaltum with high viscosity constructed according to claim 8, it is characterised in that: the polyphosphoric acids is P2O5Contain
Amount >=83wt% polyphosphoric acid product.
10. the asphaltum with high viscosity described in accordance with the claim 1 for being easy to construct, it is characterised in that: the higher aliphatic is choosing
From C12~C18Fatty alcohol.
11. being easy to the asphaltum with high viscosity constructed according to claim 10, it is characterised in that: the higher aliphatic is ten
One or both of glycol, tetradecyl alchohol, hexadecanol and octadecyl alcolol mixture.
12. the asphaltum with high viscosity described in accordance with the claim 1 for being easy to construct, it is characterised in that: the silane coupling agent is ammonia
At least one of base silane, methyl vinyl base silane, epoxy radicals silicone hydride, sulfenyl silane and vinyl silanes.
13. the preparation method for the asphaltum with high viscosity for being easy to construct described in a kind of any one of claim 1-12, it is characterised in that:
Include the following steps:
(1) polyphosphoric acids is added in the matrix pitch of molten state, carries out chemical modification reaction；
(2) it is added to increase into step (1) material and prolongs agent mother liquor, the reaction was continued；
(3) higher aliphatic is added into step (2) material, the reaction was continued；
(4) compound adjusting adhesive and silane coupling agent is added into step (3) material, the reaction was continued, and easy working high viscosity is made
Pitch.
14. preparation method according to claim 13, it is characterised in that: the preparation of compound adjusting adhesive described in step (4)
Process is that the polyethylene wax for being grafted the epoxy of specified wt part and mesopore molecular sieve premix, and is stirred 20- in 90~110 DEG C
40min is cooled to room temperature obtained.
15. preparation method according to claim 13, it is characterised in that: the matrix pitch of molten state described in step (1)
Temperature be 140~160 DEG C；Reaction temperature is 145~185 DEG C, and the reaction time is 30~200 minutes；
Reaction temperature described in step (2) is 140~180 DEG C, and the reaction time is 30~150 minutes；
Reaction temperature described in step (3) is 140~200 DEG C, and the reaction time is 10~30 minutes；
Reaction temperature described in step (4) is 120~150 DEG C, and the reaction time is 20~60 minutes.
16. preparation method according to claim 15, it is characterised in that: reaction temperature described in step (1) be 150~
170℃；
Reaction temperature described in step (2) is 150~165 DEG C；
Reaction temperature described in step (3) is 150~170 DEG C.
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