CN1270981A - Efficient asphalt soaker and its preparation - Google Patents

Abstract

A high-efficient asphalt soaker is prepared by using coal tar pitch or asphalt as base material sand sym-tetramethylbenzene in 5-15% as additive and through pressurized chemical copolymerization. It has a softening point of 100-150 deg.C, carbon carbon yield of 60-72% and viscosity at 300 deg.C lower than 0.12 Pa.s.

Description

A kind of efficient asphalt soaker and preparation method thereof

The invention belongs to the preparation method of efficient asphalt soaker, relate in particular to the preparation method of a kind of low viscosity, high carbon yield pitch soaker.

Asphalt impregnant is the density strengthening agent of raw material of wood-charcoal material and goods thereof, and its products obtained therefrom is widely used in fields such as electronics, metallurgy, machinery, space flight, aviation.In the production of carbon material, especially in the preparation process of c/c matrix material, the quality quality of asphalt impregnant directly has influence on the performance and the production cost of product.A kind of Perfected process that makes pitch have low viscosity and high charcoal yield is to optimize the bituminous molecular structure, makes its size to fit, is evenly distributed.Many for this reason scholars propose to prepare pitch to optimize its molecular structure from pure compound through catalyzed polymerization.But owing to adopt pure compound, production cost is increased substantially, simultaneously, this method also has operational path longer, severe reaction conditions, shortcomings such as catalyst separating difficulty.As Eur.Pat.Appl.EP381493, from naphthalene preparation bituminous process, with AlCl ₃Be catalyzer, after reaction, need to separate AlCl through four above steps ₃, and be difficult to separate clean.For another example, Jpn.KoKai Tokkyo Koho JP04154888 by the simple hydrocarbon polymer preparation pitch that sets out, adopts to have corrosive super acids HF/BF ₃Be catalyzer, bring inconvenience to equipment design and production operation.For avoiding these deficiencies, people have developed the molecular structure that the normal pressure chemical copolymerization method improves dipping agent bitumen.Thereby so-called normal pressure chemical copolymerization method promptly adds the purpose that the chemical substance warp with a fixed structure reaches adjustment with the copolymerization of asphaltene molecule normal pressure, optimizes the asphaltene molecule structure in tar or pitch.As Jpn.Kokai Tokkyo Koho JP03103490, in coal tar, add some simple organics and obtain 78.6 ℃ of softening temperatures, the dipping agent bitumen of fixed carbon content 32.7% through the normal pressure heat treated.But this type of dipping agent bitumen charcoal yield is lower, and purposes is limited.Especially in special dimensions such as aerospace, because the singularity (as High Temperature High Pressure) and the expensive characteristic of its material produce technological process, performance to dipping agent bitumen also has higher requirement (will get well as temperature flowing, preferably less than 0.15Pa.s, the charcoal yield is more preferably greater than 65% at 300 ℃ viscosity numbers).Add the requirement that pitch that some simple organism adopt normal pressure chemical copolymerization methods to make is difficult to satisfy special dimensions such as aerospace like this.

The purpose of this invention is to provide efficient asphalt soaker of a kind of low viscosity high yield charcoal and preparation method thereof.

The object of the present invention is achieved like this, adopts the pressurization chemical copolymerization to obtain good fluidity, asphalt impregnant that charcoal yield is high with coal-tar pitch or the petroleum pitch durol that is raw material through adding 5-15%.

Made efficient asphalt soaker, its softening temperature are 100-150 ℃, charcoal yield 60.0%-72.0%, and 300 ℃ viscosity number is less than 0.12Pa.s.

Preparation method of the present invention is as follows:

(1) durol of interpolation 5-15% in material asphalt mixes;

(2) blended is packed in the reactor, feed nitrogen protection, sealed reactor rises to 380-440 ℃ temperature with the heat-up rate of 3-5 ℃/min;

(3) stirring was reacted 6-28 hour under 380-440 ℃ of temperature and certain pressure down;

(4) go out still behind the naturally cooling, get high-quality dipping pitch.

Aforesaid pressure is 0.6-2.5Mp.

Aforesaid pitch is medium temperature coal pitch, petroleum pitch.

Aforesaid additive also can be other additive with the durol structural similitude.

Aforesaid pressure is provided by reaction system self or the external world provides.

The final performance of the made bituminous of the present invention can require to control by reaction times, temperature of reaction, reaction pressure according to difference.

The present invention has following advantage:

(1) raw material sources are extensive, low price.

(2) technological process is simple, and energy consumption is low, saves time, and is laborsaving.

(3) can artificially control the performance of product, to satisfy the needs of different levels.

(4) excellent product quality, stable performance.

Most preferred embodiment of the present invention is as follows:

Embodiment 1

Take by weighing 90.0g medium temperature coal pitch (S.P.:68 ℃ C.Y.:43.01%) is mixed in the reactor of packing into nitrogen protection with the 10.0g durol; sealed reactor rises to 430 ℃ of constant temperature, stirring reaction 6h with the temperature rise rate of 4 ℃/min; system pressure 1.0Mp; reaction finishes the back naturally cooling, goes out still, gets high-quality dipping pitch 80.0g; S.P.:100 ℃; C.Y.:59.54%, and viscosity (300 ℃, 20r/min): 0.035Pa.s.

Embodiment 2

Take by weighing 90.0g medium temperature coal pitch (S.P.:68 ℃ C.Y.:43.01%) is mixed in the reactor of packing into nitrogen protection with the 10.0g durol; sealed reactor rises to 420 ℃ of constant temperature, stirring reaction 12h with the temperature rise rate of 4 ℃/min; system pressure 0.6Mp; reaction finishes the back naturally cooling, goes out still, gets high-quality dipping pitch 65.0g; S.P.:130 ℃; C.Y.:68.02%, and viscosity (300 ℃, 20r/min): 0.074Pa.s.

Embodiment 3

Take by weighing 95.0g medium temperature coal pitch (S.P.:68 ℃ C.Y.:43.01%) is mixed in the reactor of packing into nitrogen protection with the 5.0g durol; sealed reactor rises to 420 ℃ of constant temperature, stirring reaction 12h with the temperature rise rate of 4 ℃/min; system pressure 0.8Mp; reaction finishes the back naturally cooling, goes out still, gets high-quality dipping pitch 60.0g; S.P.:146 ℃; C.Y.:72.15%, and viscosity (300 ℃, 20r/min): 0.120Pa.s.

Embodiment 4

Take by weighing 85.0g medium temperature coal pitch (S.P.:68 ℃ C.Y.:43.01%) is mixed in the reactor of packing into nitrogen protection with the 15.0g durol; sealed reactor rises to 420 ℃ of constant temperature, stirring reaction 12h with the temperature rise rate of 4 ℃/min; system pressure 0.8Mp; reaction finishes the back naturally cooling, goes out still, gets high-quality dipping pitch 75.0g; S.P.:118 ℃; C.Y.:62.07%, and viscosity (300 ℃, 20r/min): 0.042Pa.s.

Embodiment 5

Take by weighing 90.0g medium temperature coal pitch (S.P.:68 ℃ C.Y.:43.01%) is mixed in the reactor of packing into nitrogen protection with the 10.0g durol; sealed reactor rises to 410 ℃ of constant temperature, stirring reaction 28h with the temperature rise rate of 3 ℃/min; system pressure 2.5Mp; reaction finishes the back naturally cooling, goes out still, gets high-quality dipping pitch 70.0g; S.P.:106 ℃; C.Y.:66.67%, and viscosity (300 ℃, 20r/min): 0.070Pa.s.

Embodiment 6

Take by weighing 90.0g medium temperature coal pitch (S.P.:68 ℃ C.Y.:43.01%) is mixed in the reactor of packing into nitrogen protection with the 10.0g durol; sealed reactor rises to 440 ℃ of constant temperature, stirring reaction 6h with the temperature rise rate of 5 ℃/min; system pressure 1.2Mp; reaction finishes the back naturally cooling, goes out still, gets high-quality dipping pitch 70.0g; S.P.:120 ℃; C.Y.:63.12%, and viscosity (300 ℃, 20r/min): 0.045Pa.s.

Embodiment 7

Take by weighing 90.0g petroleum pitch (S.P.:65 ℃ C.Y.:40.12%) is mixed in the reactor of packing into nitrogen protection with the 10.0g durol; sealed reactor rises to 380 ℃ of constant temperature, stirring reaction 20h with the temperature rise rate of 3 ℃/min; system pressure 0.8Mp; reaction finishes the back naturally cooling, goes out still, gets high-quality dipping pitch 70.0g; S.P.:121 ℃; C.Y.:64.58%, and viscosity (300 ℃, 20r/min): 0.052Pa.s.

Claims (2)

1. an efficient asphalt soaker adopts the pressurization chemical copolymerization method to make, and it is characterized in that with coal-tar pitch or petroleum pitch be raw material, add the durol of 5-15%, the softening temperature of product soaker is 100-150 ℃, and the charcoal yield is 60-72%, and 300 ℃ viscosity number is less than 0.12Pa.s.

2. the preparation method of asphalt impregnant as claimed in claim 1 is characterized in that:

(1) durol of interpolation 5-15% in material asphalt mixes;

(2) compound is packed in the reactor, feed nitrogen protection, sealed reactor rises to 380-440 ℃ temperature with the heat-up rate of 3-5 ℃/min;

(3) stirring was reacted 6-28 hour under 380-440 ℃ of temperature and certain pressure down;

(4) go out still behind the naturally cooling, get high-quality dipping pitch.