CN103805220A - Preparation method for high-softening point asphalt - Google Patents
Preparation method for high-softening point asphalt Download PDFInfo
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- CN103805220A CN103805220A CN201210439793.8A CN201210439793A CN103805220A CN 103805220 A CN103805220 A CN 103805220A CN 201210439793 A CN201210439793 A CN 201210439793A CN 103805220 A CN103805220 A CN 103805220A
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Abstract
The invention discloses a preparation method for high-softening point asphalt. The method includes: respectively spraying molten state asphalt and an oxidant into an oxidation reactor at the same time to undergo oxidation reaction, thus obtaining the high-softening point asphalt. Specifically, the oxidant is nanoscale potassium permanganate and/or nanoscale potassium dichromate. The asphalt and the oxidant are respectively sprayed into the oxidation reactor in the fog state at the same time by a high pressure pump and compressed air to undergo mixing. The method provided by the invention has the advantages of less oxidant consumption, low oxidation temperature, high reaction efficiency, convenient operation, environment-friendly reaction process, and low energy consumption.
Description
Technical field
The present invention relates to a kind of preparation method of high softening point bitumen, relate in particular to a kind of efficient oxidation method of utilizing oxygenant to prepare high softening point bitumen.
Background technology
High softening point bitumen refers to that softening temperature is more than 100 ℃, the especially pitch more than 120 ℃.High softening point bitumen is applied because its outstanding high-temperature resistance has more widely.As the use of the roof cover as building, even if also can not become during the broiling summer very soft even trickling.Can also be used for the drilling operation in deep-seated oil gas field, as the important component part of drilling fluid, can under hot conditions, play shutoff, anti-collapse, stabilizing borehole, reduces the effect of filter loss.In addition, can also be as property-modifying additive of macromolecular material etc.
High softening point bitumen production technique mainly adopts solvent de-asphalting process or oxidizing process.According to existing solvent de-asphalting process, produce high softening point bitumen, need to adopt heavier solvent.For removing the solvent of pitch in mutually, need to be heated to higher temperature, very easily cause the problems such as furnace coking, and energy consumption is very large.In addition, even the viscosity of high softening point bitumen is still very large at higher temperature, production equipment discharging is also more difficult, therefore not suitable for producing high softening point bitumen very of current solvent de-asphalting process.
Oxidized bitumen technique refers to softening temperature low, penetration degree is large and temperature sensitivity is high vacuum residuum, solution-off pitch or their mixture are raw material, in oxidizing tower, under certain temperature condition, passing into air (making oxygenant with oxygen) reacts, its composition is changed, softening temperature raises, penetration degree and temperature sensitivity decline, to reach the requirement of asphaltic products. specification and use properties.Compared with solvent de-asphalting process, the advantage such as oxidizing process has less investment, and technique is simple, easy to operate, can yet be regarded as and produce the comparatively ideal process means of high softening point bitumen.
But, in traditional oxidized bitumen technological operation, be that pressurized air is imported in raw material by an air distribution ring with very thin nozzle, utilize airborne oxygen to make oxygenant and carry out oxidized bitumen.But, be oxygen owing to only having small part in air, and the rare gas element of major part to be nitrogen and other can not carry out with pitch chemical reaction.The low oxidation efficiency that affects of oxygen level on the one hand, on the one hand a large amount of nitrogen has occupied again large quantity space with other rare gas element that can not carry out chemical reaction with pitch pitch can not fully be contacted with oxygen, partial oxidation is not fully utilized, and the oxidation efficiency of pitch is decreased again.Be that necessity passes into large quantity of air for pitch is fully oxidized, do not participate on the one hand in a large number the nitrogen of chemical reaction and other rare gas element and inevitably participate in the production process of pitch, greatly waste energy; The nitrogen that can not be utilized in a large number is on the one hand discharged in atmosphere together with carrying again the harmful light constituent of the part producing in pitch oxidation process with rare gas element, causes again topsoil.This has not only caused efficiency low, polluted air, and also reaction is also very inhomogeneous.In fact, reaction only occurs in oxidizing tower bottom.
In order to solve the problems referred to above that exist in pitch oxidation process, Austrian Po Neng company discloses a kind of BITUROX technique, and it is in oxidizing tower, to have increased by three grades of whipping apptss.Rise in the process that becomes large at bubble, blended, again form small bubbles and be distributed in raw material, thereby improved oxidation efficiency.This method has not only increased the complicacy of mechanical means, has increased energy consumption, also brings certain difficulty to overhaul of the equipments.
CN1415699A discloses a kind of production method of oxidized bitumen, first adopts static mixer that air and pitch are mixed, and air is distributed in asphalt stock with small bubble, then enters oxidation unit and carries out oxidizing reaction.In the time of production ordinary road pitch and building asphalt, the method can improve oxidation efficiency to a certain extent.But for producing high softening point bitumen, this kind of technique exists obvious deficiency.Because the mixing temperature at static mixer Raw and air is oxidizing temperature, at higher temperature, carry out and produce high softening point bitumen.Under this temperature condition, mixing, can only have the bubble of little amount to be distributed in raw material, therefore will be very limited to the degree that improves oxidation efficiency, yet have air pollution problems inherent.
For within lower temperature of reaction and shorter reaction times, obtain the pitch that softening temperature is high, conventionally adopt the method for catalyzed oxidation, in reaction, add a certain amount of catalyzer, reduce temperature of reaction and improve speed of response.But for produce high softening point bitumen, catalyzed oxidation temperature still higher, need oxidization time still long.CN102464989A discloses a kind of premixed catalysed oxidation processes and has produced high softening point bitumen, and catalyzer used is zinc oxide, cupric sulfide, iron trichloride and polyphosphoric acid, has improved quality and the efficiency of oxidized bitumen product.But oxidising process is comparatively complicated, and oxidizing temperature is still higher.CN102363731A discloses a kind of method that improves pitch softening point, utilize gas blower from the bottom of reactor, oxygenant to be sent into reactor, the mode of pitch melting being carried out to high-speed and high-temperature oxidation, fast flash distillation and emulsify at a high speed, obtains the pitch with high softening-point.But the method complicated process of preparation, temperature of reaction are high, and do not write the softening point range of high softening point bitumen exactly.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of preparation method of high softening point bitumen, the method oxygenant consumption is still less, oxidizing temperature is low, reaction efficiency is high, easy to operate, and reaction process environmental friendliness, and energy consumption is low.
The preparation method of high soft spots pitch of the present invention, comprises following content: the pitch of molten state and oxygenant spray into respectively oxidation reactor simultaneously, carry out oxidizing reaction, obtain high softening point bitumen.
In the inventive method, pitch is petroleum pitch, the mixture of one or more that comprise de-oiled asphalt that vacuum residuum, straight-run pitch, solvent de-asphalting process obtain, are in harmonious proportion in pitch etc., 25 ℃ of penetration degrees of pitch are 20～200 1/10mm, softening temperature is 30～75 ℃.
In the inventive method, oxygenant is nano level potassium permanganate and/or nano level potassium bichromate, and its particle diameter is 10～100nm, and the add-on of oxygenant accounts for 0.5% ~ 10% of asphalt quality.
In the inventive method, by high-pressure pump and compress wind pitch and oxygenant respectively with mist state, spray into oxidation reactor simultaneously, make its full and uniform mixing.Wherein the working pressure of high-pressure pump is 0.2～2MPa, and compress wind working pressure is 0.2～1MPa.
In the inventive method, oxidizing temperature is 200 ~ 240 ℃, and oxidization time is 2 ~ 10 hours.Oxidizing reaction is carried out under shearing condition, and shears rotating speed is 3000～6000rpm.
The softening temperature of high softening point bitumen product prepared by the inventive method is at 120 ~ 200 ℃
The inventive method compared with prior art, has the following advantages:
(1) utilize high-pressure pump and compress wind that pitch is mixed with oxygenant, the dispersion effect of oxygenant particle in pitch medium is better, under the effect of high-shear, make oxidizing reaction more even, reduced oxygenant consumption, improved quality and the oxidation efficiency of oxidation products.
(2) utilize nano level high-efficient oxidant to be oxidized pitch, its great specific surface area and high surfactivity effect thereof have reduced oxidizing temperature in pitch oxidation process, make oxidizing reaction more abundant simultaneously, and reaction efficiency is high.
(3) do not need to pass into the required air of oxidizing reaction, reduced the pollution of waste gas to air, save the use of air compressor etc. and attached air feed equipment thereof simultaneously, make that technical process and equipment are simpler, more convenient operation.
Embodiment
Below will by embodiment, the present invention will be further described, but therefore do not limit the present invention.Percentage ratio is wherein massfraction.
Comparative example 1
Be 41 1/10mm by 25 ℃ of penetration degrees, softening temperature is the pitch of 54.6 ℃, accounts for 96.7% of total amount, be heated to 150 ℃ of molten states, add 3.3% polyphosphoric acid and pass into air, with high shearing mixing emulsor shearing 25 minutes, enter in oxidizing tower and carry out air blowing oxidation, obtain oxidized bitumen.Oxidation reaction condition and product property are in table 1.
Comparative example 2
Be 41 1/10mm by 25 ℃ of penetration degrees, softening temperature is the pitch of 54.6 ℃, is heated to 150 ℃ of molten states, and adding particle diameter is the common potassium permanganate (take asphalt quality as benchmark) of 1-2mm, carries out oxidizing reaction, obtains oxidized bitumen.Oxidation reaction condition and product property are in table 1.
Embodiment 1
Be 41 1/10mm by 25 ℃ of penetration degrees, softening temperature is that the potassium permanganate that the pitch of 54.6 ℃ and particle diameter are 50nm is used respectively high-pressure pump and compress wind, sprays into oxidation reactor with mist state simultaneously, makes its full and uniform mixing carry out oxidizing reaction, obtains oxidized bitumen.The working pressure of high-pressure pump is 0.8MPa, and compress wind working pressure is 0.5MPa.Oxidizing reaction is carried out under shearing condition, and shears rotating speed is 4000rpm.Oxidation reaction condition and product property are in table 1.
Embodiment 2
Be 41 1/10mm by 25 ℃ of penetration degrees, softening temperature is that the potassium permanganate that the pitch of 54.6 ℃ and particle diameter are 50nm is used respectively high-pressure pump and compress wind, sprays into oxidation reactor with mist state simultaneously, makes its full and uniform mixing carry out oxidizing reaction, obtains oxidized bitumen.The working pressure of high-pressure pump is 1.5MPa, and compress wind working pressure is 0.8MPa.Oxidizing reaction is carried out under shearing condition, and shears rotating speed is 3000rpm.Oxidation reaction condition and product property are in table 1.
Embodiment 3
Be 121 1/10mm by 25 ℃ of penetration degrees, softening temperature is that the potassium bichromate that the pitch of 41.8 ℃ and particle diameter are 75nm is used respectively high-pressure pump and compress wind, sprays into oxidation reactor with mist state simultaneously, makes its full and uniform mixing carry out oxidizing reaction, obtains oxidized bitumen.The working pressure of high-pressure pump is 2MPa, and compress wind working pressure is 1MPa.Oxidizing reaction is carried out under shearing condition, and shears rotating speed is 6000rpm.Oxidation reaction condition and product property are in table 1.
Embodiment 4
Be 121 1/10mm by 25 ℃ of penetration degrees, softening temperature is that the potassium permanganate that the pitch of 41.8 ℃ and particle diameter are 75nm is used respectively high-pressure pump and compress wind, sprays into oxidation reactor with mist state simultaneously, makes its full and uniform mixing carry out oxidizing reaction, obtains oxidized bitumen.The working pressure of high-pressure pump is 2MPa, and compress wind working pressure is 1MPa.Oxidizing reaction is carried out under shearing condition, and shears rotating speed is 6000rpm.Oxidation reaction condition and product property are in table 1.
Table 1 oxidation reaction condition and oxidation products character.
| Embodiment | Comparative example 1 | Comparative example 2 | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Oxidizing temperature, ℃ | 290 | 235 | 220 | 235 | 230 | 235 |
| Oxidization time, h | 8 | 8 | 3 | 8 | 9 | 10 |
| Air quantity, m 3×kg -1×h -1 | 0.18 | ? | ? | ? | ? | ? |
| Oxidant content (take asphalt quality as benchmark), % | ? | 10 | 10 | 1 | 8 | 10 |
| Softening temperature, ℃ | 120 | 121.5 | 120.1 | 135 | 165.8 | 195 |
Can find out from the data of table 1, the oxidation efficiency of high softening point bitumen prepared by the inventive method is high, and oxidation effectiveness is good, and oxygenant consumption is few.
Claims (9)
1. a preparation method for high soft spots pitch, is characterized in that comprising following content: the pitch of molten state and oxygenant spray into respectively oxidation reactor simultaneously, carry out oxidizing reaction, obtain high softening point bitumen.
2. in accordance with the method for claim 1, it is characterized in that: pitch is petroleum pitch, comprise de-oiled asphalt that vacuum residuum, straight-run pitch, solvent de-asphalting process obtain and one or more the mixture being in harmonious proportion in pitch.
3. in accordance with the method for claim 1, it is characterized in that: 25 ℃ of penetration degrees of pitch are 20～200 1/10mm, and softening temperature is 30～75 ℃.
4. in accordance with the method for claim 1, it is characterized in that: oxygenant is nano level potassium permanganate and/or nano level potassium bichromate, and its particle diameter is 10～100nm, and the add-on of oxygenant accounts for 0.5% ~ 10% of asphalt quality.
5. in accordance with the method for claim 1, it is characterized in that: by high-pressure pump and compress wind pitch and oxygenant respectively with mist state, spray into oxidation reactor simultaneously, make its full and uniform mixing.
6. in accordance with the method for claim 5, it is characterized in that: the working pressure of high-pressure pump is 0.2～2MPa, compress wind working pressure is 0.2～1MPa.
7. in accordance with the method for claim 1, it is characterized in that: oxidizing temperature is 200 ~ 240 ℃, oxidization time is 2 ~ 10 hours.
8. in accordance with the method for claim 1, it is characterized in that: oxidizing reaction is carried out under shearing condition, shears rotating speed is 3000～6000rpm.
9. it is characterized in that in accordance with the method for claim 1: the softening temperature of high softening point bitumen product is between 120 ~ 200 ℃.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105586063A (en) * | 2014-10-22 | 2016-05-18 | 中国石油化工股份有限公司 | Preparation method of high softening point asphalt for drilling fluid |
| CN106318424A (en) * | 2015-07-03 | 2017-01-11 | 上海宝钢化工有限公司 | Novel environment-friendly method for improving asphalt softening point |
| CN110272764A (en) * | 2019-06-04 | 2019-09-24 | 新奥科技发展有限公司 | A kind of preparation method of semicoke flying dust modifying agent and the utilization method of semicoke flying dust |
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| GB229690A (en) * | 1924-02-22 | 1925-12-03 | Knud Waldemar Nielsen | Method of treating asphalt oil or pitch with a view to producing rubber-like masses therefrom |
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| CN1415699A (en) * | 2001-10-30 | 2003-05-07 | 中国石油化工股份有限公司 | Method for oxidizing asphaltum |
| CN101688122A (en) * | 2006-06-08 | 2010-03-31 | 马拉松石油加拿大有限公司 | Bitum oxidation |
| CN101838542A (en) * | 2010-05-19 | 2010-09-22 | 镇江新光冶金辅材厂 | Manufacturing method of ultra-temperature pitch |
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| SU925981A1 (en) * | 1980-06-18 | 1982-05-07 | Украинский научно-исследовательский углехимический институт | Process for producing electrode pitch |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105586063A (en) * | 2014-10-22 | 2016-05-18 | 中国石油化工股份有限公司 | Preparation method of high softening point asphalt for drilling fluid |
| CN105586063B (en) * | 2014-10-22 | 2018-03-16 | 中国石油化工股份有限公司 | A kind of preparation method of drilling fluid high softening point bitumen |
| CN106318424A (en) * | 2015-07-03 | 2017-01-11 | 上海宝钢化工有限公司 | Novel environment-friendly method for improving asphalt softening point |
| CN106318424B (en) * | 2015-07-03 | 2019-04-12 | 宝武炭材料科技有限公司 | Novel environment-friendly method for improving asphalt softening point |
| CN110272764A (en) * | 2019-06-04 | 2019-09-24 | 新奥科技发展有限公司 | A kind of preparation method of semicoke flying dust modifying agent and the utilization method of semicoke flying dust |
| CN110272764B (en) * | 2019-06-04 | 2020-12-29 | 新奥科技发展有限公司 | Preparation method of semicoke fly ash modifier and utilization method of semicoke fly ash |
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| CN103805220B (en) | 2015-09-30 |
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