CN103173025A

CN103173025A - Method for preparing road asphalt by direct coal liquefaction residue

Info

Publication number: CN103173025A
Application number: CN2013100845893A
Authority: CN
Inventors: 赵鹏; 韩森; 雷达
Original assignee: Changan University
Current assignee: Changan University
Priority date: 2013-03-15
Filing date: 2013-03-15
Publication date: 2013-06-26
Anticipated expiration: 2033-03-15
Also published as: CN103173025B

Abstract

The invention discloses a method for preparing road asphalt by direct coal liquefaction residue; the method comprises the steps of: firstly, extracting low-softening point asphaltene in the direct coal liquefaction residue by utilizing coal tar; then separating the asphaltene from the coal tar by utilizing the low temperature split phase principle in the cooling process of the asphaltene and the coal tar; and preparing the road asphalt capable of meeting different pavement performance requirements from the extracted asphaltene, the direct coal liquefaction residue and petroleum asphalt according to different proportions. According to the method, an adopted asphalt matter extraction solvent is the coal tar, the solid-liquid separation is realized by utilizing the low temperature split phase principle in the cooling process of the asphaltene and the coal tar, and the method mainly adopts the coal liquefaction residue with lower cost as a raw material, so that the whole method has a good economic value.

Description

A kind of method of utilizing coal directly-liquefied residue to prepare road bitumen

Technical field

The invention belongs to the technical field that the Coal Chemical Industry solid waste is used in material of construction, be specifically related to prepare with coal directly-liquefied residue the method for road bitumen.

Background technology

In coal liquefaction technology, direct coal liquefaction technology begins heavy industrialization in China to be used, and coal directly-liquefied residue is that the softening temperature of discharging from vacuum distillation apparatus after DCL/Direct coal liquefaction is not no more than the coal directly-liquefied residue of 50% mass percent higher than 180 ℃, solids content.

In prior art about utilize method that coal directly-liquefied residue prepares bitumen as:

ZL200610012547.9 discloses a kind of road asphalt modifier and application method thereof, the method is that coal directly-liquefied residue is crushed to below 100 orders, with pitch 100-250 ℃ of scope, the mass ratio that accounts for modifying asphalt by coal directly-liquefied residue is that 5-10% mixes, the method is direct physical mixed, in matrix pitch, the coal liquefaction residue add-on is very low, if improve the add-on of coal liquefaction residue, because the softening temperature of coal liquefaction residue is higher, contain more inorganic component, cause the low-temperature performance of matrix pitch not meet the demands, limited the widespread use of coal liquefaction residue.

CN102399566 discloses a kind of method that extracts heavy liquefaction oil and bitumen from coal hydroliquefaction residue, the method adopts organic solvent to extract, the heavy liquefaction oil and the bitumen that obtain, its complex process, adopt the organic solvent price high, the extraction cost is high, the bitumen that obtains do not possess price advantage in the road engineering field.

To sum up, existingly there is following shortcoming about the method for utilizing coal directly-liquefied residue to prepare bitumen:

(1) prepared bitumen can not satisfy construction and will require.

(2) complex process, cost is high.

Summary of the invention

The object of the present invention is to provide a kind of method of utilizing coal directly-liquefied residue to prepare road bitumen, and the method technique is simple, road bitumen preparation can satisfy the road construction requirement.

For this reason, the method concrete steps of utilizing coal directly-liquefied residue to prepare road bitumen provided by the invention are as follows:

Step 1, under 100～150 ℃ of conditions, the coal directly-liquefied residue powder is dissolved soak in coal tar and obtain batch mixing after the bituminous matter make in coal directly-liquefied residue immerses coal tar, wherein the mass ratio of coal directly-liquefied residue powder and coal tar is 1:(1～3);

Step 2 is filtered the batch mixing of step 1 gained under 100～150 ℃ of conditions, obtain containing the filter residue of coal tar and contain bitum coal tar filtrate;

Step 3 is cooled to the coal tar filtrate of step 2 gained under 30～50 ℃ of conditions, and pitch is separated out from coal tar, obtains bituminous matter and coal tar;

Step 4, bituminous matter, coal directly-liquefied residue powder and the petroleum pitch mixing under 130～200 ℃ of conditions that step 3 is obtained namely gets road bitumen, wherein, the mass ratio of the bituminous matter that step 3 obtains and coal directly-liquefied residue powder is (0.2～1): 1, and the quality that adds of petroleum pitch is 20%～50% of the bituminous matter that obtains of step 3 and coal directly-liquefied residue total mass;

The particle diameter of the coal directly-liquefied residue powder described in above-mentioned steps one is less than 0.1mm.

Coal tar described in above-mentioned steps one is that density that in bituminous coal, low-temperature pyrolysis obtains is less than 1.0g/cm ³Middle coalite tar.

The filtering net that is 45～75 μ m with batch mixing with the filter opening size in above-mentioned steps two filters.

Utilize the method for air lift to reclaim the coal tar in the gained filter residue in above-mentioned steps two in aforesaid method, with the coal tar that the reclaims source as coal tar used in above-mentioned steps one, and the filter residue that will reclaim after coal tar is produced steam as boiler oil, and gained steam is used to that described in above-mentioned steps one, step 2 and step 4, condition provides thermal source.

The coal tar of gained in recycling step three in aforesaid method, and with the coal tar that the reclaims source as coal tar used in above-mentioned steps one.

At first method of the present invention utilizes the low softening point asphalt in coal tar extraction coal directly-liquefied residue; Then utilize the principle of bituminous matter and coal tar low temperature phase-splitting in temperature-fall period, realize pitch and coal tar oil separating; Then pitch, coal directly-liquefied residue and the petroleum pitch that extracts is mixed with road bitumen according to a certain percentage, the indices of this road bitumen all satisfies the related request in JTG F40-2004.The extraction solvent of the bitumen that the method adopts is coal tar, and utilize the principle of bituminous matter and coal tar low temperature phase-splitting in temperature-fall period to realize solid-liquid separation, the main raw material of while method is lower-cost coal directly-liquefied residue, and then guarantees that whole method has good economic worth.

To sum up, compared with prior art, method of the present invention has following characteristics:

(1) utilize coal tar to propose bitumen in coal directly-liquefied residue, compare chemical solvents and propose the cost decrease;

(2) take full advantage of solid matters such as catalyzer in waste residue and substitute breeze in road bitumen Concrete process, make other compositions in waste residue be fully used on the one hand, also needn't deliberately remove the solid matters such as catalyzer of bringing in pitch proposition process on the other hand, greatly reduce the proposition cost;

(3) take full advantage of the characteristic of the bitumen low softening point that proposes in the direct residue of coal, and the characteristic of coal directly-liquefied residue high softening-point, carry out composite, learn from other's strong points to offset one's weaknesses, can satisfy the requirement of different pavement performances, strengthened again the utilization ratio of coal directly-liquefied residue, and cost be low.

Description of drawings

Below in conjunction with accompanying drawing and embodiment, the present invention is described in further detail.

Fig. 1 is the method process flow sheet of embodiment 1.

Embodiment

In order to improve coal liquefaction residue usage quantity in road bitumen, and cut down finished cost, the present invention adopts the technology of bitumen proposition cheaply, to obtaining the road bitumen of different pavement performances.

The method of utilizing coal directly-liquefied residue to prepare road bitumen of the present invention is as follows:

At first adding quality in the coal directly-liquefied residue powder is coal directly-liquefied residue powder quality 1-3 coal tar doubly, dissolving is soaked during the bituminous matter made coal directly-liquefied residue in 20～60 minutes fully immerses coal tar at the temperature of 100-150 ℃, then filter at the temperature of 100-150 ℃, the filter residue that obtains containing bitum coal tar filtrate and contain coal tar, then will contain in the temperature range that bitum coal tar filtrate cools to 30-50 ℃, bituminous matter is separated out from coal tar naturally, pour out day-coal tar, the bottom precipitate is bituminous matter; At last with the bituminous matter separated out and coal directly-liquefied residue powder according to (0.2～1): 1 mass ratio carries out composite, and add again the petroleum pitch mixing namely to get road bitumen after melting mixing at 130-200 ℃ of temperature, wherein, the add-on of petroleum pitch is 20%～50% of bituminous matter and coal directly-liquefied residue powder total mass.

In order to guarantee that the pitch in coal directly-liquefied residue fully immerses coal tar in the short period of time, in method, the particle diameter of coal directly-liquefied residue powder used is less than 0.1mm.

For filtrate is effectively separated with filter residue, the filtering net that is 45～75 μ m with the filter opening size in method filters and obtains filter residue and filtrate.

For the production control cost, in using in method of the present invention, coal directly-liquefied residue is soaked in the coalite tar dissolving.

In order to reduce costs, utilize the coal tar in the gained filter residue in the method recovery method of air lift in method, with the coal tar recycle of reclaiming; And the filter residue that will reclaim after coal tar is produced steam as boiler oil, and gained steam is used to whole method that thermal source is provided.

In order further to reduce costs, reclaim the coal tar of separating out after pitch in method, and with this coal tar recycle.

What need to explain is: bituminous matter of the present invention is the bitumen in can dissolving in coal tar in coal directly-liquefied residue under 100-150 ℃ of condition, and its quality is 25%～35% of coal directly-liquefied residue quality; The bituminous matter of separating out from filtrate under the condition of 30-50 ℃ is the bituminous matter material that contains part heavy oil, and wherein the heavy oil quality is 5%～15% of coal directly-liquefied residue quality, and asphalt quality is 15%～25% of coal directly-liquefied residue quality.

Below the embodiment that the contriver provides, so that the present invention is described in further detail.

Embodiment 1:

With reference to figure 1, the method for this embodiment is as follows:

(1) coal directly-liquefied residue is adopted ball mill pulverizer pulverize, sieve, obtain particle diameter less than the coal directly-liquefied residue powder of 1mm;

(2) 3000 gram coal tar are added in reactor, add while stirring 1500 gram coal directly-liquefied residue powders, be incubated under the condition of 140 ℃, coal tar pitch volatiles between heating period returns to reactor by reflux condensation mode, be incubated that after 20 minutes, the bituminous matter in coal directly-liquefied residue incorporates in coal tar, be that the filter screen of 50 microns filters with filter opening at the temperature of 140 ℃ afterwards, obtain filtrate and filter residue, with after filtrate cooling down to 50 ℃, the bitumen that proportion is larger is separated out, be deposited to container bottom, obtain the bituminous matter of 280 grams, reclaim simultaneously day-coal tar, filter the filter residue that produces, adopt steam to carry out stripping, reclaim a small amount of coal tar that sticks in filter residue, all reclaim coal tar and recycle, and the filter residue after stripping is produced steam as boiler oil, and gained steam is used to whole method that thermal source is provided,

(3) with gained in 100 gram steps (2) separate out bituminous matter and 100 gram coal directly-liquefied residue powders add the petroleum pitch mixing of 40 grams namely to get road bitumen after melting mixing at the temperature of 130 ℃ again.

The performance that this embodiment makes road bitumen is as follows: penetration degree: 98(0.1mm); Ductility (15 ℃): 80cm; Softening temperature: 107 ° of C; Solid content (mass percent): 14%, meet the index of correlation of 90# pitch.

Embodiment 2:

The method of this embodiment is as follows:

(2) 1000 gram coal tar are added in reactor, add 2000 gram coal directly-liquefied residue powders, stir on one side, heating on one side, be incubated under 120 ℃ of conditions, between heating period, coal tar pitch volatiles returns to reactor by reflux condensation mode, being incubated 35 minutes bituminous matters in coal directly-liquefied residue incorporates in coal tar, be that the filter screen of 45 microns filters with filter opening at the temperature of 110 ℃ afterwards, obtain filtrate and filter residue, the filtrate cooling down to 35 that filter to produce ℃, the pitch that proportion is larger is separated out and is obtained 390 gram bituminous matters;

(3) 390 gram coal directly-liquefied residue powders are joined in the bituminous matter that 200 grams propose, be heated to 150 ° of C, mechanical stirring makes road bitumen after adding 177 gram petroleum pitch mixings after evenly again.

The performance that this embodiment makes road bitumen is as follows: penetration degree: 72(0.1mm); Ductility (15 ℃): 58cm; Softening temperature: 128 ° of C; Solid content (mass percent): 18%, meet the index of correlation of 70# pitch.

Embodiment 3:

This embodiment is as different from Example 1: 1000 gram coal directly-liquefied residue powders are joined in 3000 grams in coalite tar, heated and stirred, temperature is controlled at 110 ° of C insulations 50 minutes, coal tar and residue are together poured under 135 ° of C in the filtering net of 65 microns and filtered, filtrate is carried out cooling, when reaching 50 ℃, pour out day-coal tar, obtain 440 gram bituminous matters.

440 gram coal directly-liquefied residue powders are joined in the bituminous matter that 300 grams propose, be heated to 155 ° of C, mechanical stirring makes road bitumen after adding 259 gram petroleum pitch mixings after evenly again.

The performance that this embodiment makes road bitumen is as follows: penetration degree: 81(0.1mm); Ductility (15 ℃): 65cm; Softening temperature: 118 ° of C; Solid content (mass percent): 17%, meet the index of correlation of 90# pitch.

Embodiment 4:

This embodiment is as different from Example 1: 1000 gram coal directly-liquefied residue powders are joined in 2700 grams in coalite tar, heated and stirred, temperature is controlled at 130 ° of C insulations 40 minutes, coal tar and residue are together poured under 120 ° of C in the filtering net of 55 microns, filtrate is carried out cooling, when reaching 45 ℃, pour out day-coal tar, obtain 450 gram bituminous matters.

1500 gram coal directly-liquefied residue powders are joined in the bituminous matter that 450 grams propose, be heated to 170 ° of C, mechanical stirring makes road bitumen after adding 780 gram petroleum pitch mixings after evenly again.

The performance that this embodiment makes road bitumen is as follows: penetration degree: 87(0.1mm); Ductility (15 ℃): 76cm; Softening temperature: 115 ℃; Solid content (mass percent): 22%, meet the index of correlation of 90# pitch.

Embodiment 5:

This embodiment is as different from Example 1: 1000 gram coal directly-liquefied residue powders are joined coalite tar in 1500 grams, heated and stirred, temperature is controlled at 100 ° of C insulations 60 minutes, coal tar and residue are together poured under 150 ° of C in the filtering net of 65 microns, filtrate is carried out cooling, when reaching 30 ℃, pour out day-coal tar, obtain 300 gram bituminous matters.

666 gram coal directly-liquefied residue powders are joined in the bituminous matter that 300 grams propose, be heated to and make road bitumen after adding again 193 gram petroleum pitch mixings after 185 ° of C stir.

The performance that this embodiment makes road bitumen is as follows: penetration degree: 64(0.1mm); Ductility (15 ℃): 50cm; Softening temperature: 134 ℃; Solid content (mass percent): 22.5%, meet the index of correlation of 70# pitch.

Embodiment 6:

This embodiment is as different from Example 1: 1000 gram coal directly-liquefied residue powders are joined coalite tar in 2800 grams, heated and stirred, temperature is controlled at 150 ° of C insulations 20 minutes, coal tar and residue are together poured under 140 ° of C in the filtering net of 75 microns, filtrate is carried out cooling, when reaching 35 ℃, pour out day-coal tar, obtain 420 gram bituminous matters.

525 gram coal directly-liquefied residue powders are joined in the bituminous matter that 420 grams propose, be heated to and make road bitumen after adding again 444 gram petroleum pitch mixings after 190 ° of C stir.

The performance that this embodiment makes road bitumen is as follows: penetration degree: 94(0.1mm); Ductility (15 ℃): 77cm; Softening temperature: 114 ℃; Solid content (mass percent): 16%, meet the index of correlation of 90# pitch.

Embodiment 7:

This embodiment is as different from Example 1: 1000 gram coal directly-liquefied residue powders are joined coalite tar in 1000 grams, heated and stirred, temperature is controlled at 115 ° of C insulations 55 minutes, coal tar and residue are together poured under 145 ° of C in the filtering net of 60 microns, filtrate is carried out cooling, when reaching 45 ℃, pour out day-coal tar, obtain 300 gram bituminous matters.

333 gram coal directly-liquefied residue powders are joined in the bituminous matter that 300 grams propose, be heated to 200 ° of C, mechanical stirring makes road bitumen after adding 317 gram petroleum pitch mixings after evenly again.

The performance that this embodiment makes road bitumen is as follows: penetration degree: 80(0.1mm); Ductility (15 ℃): 62cm; Softening temperature: 120 ℃; Solid content (mass percent): 18%, meet the index of correlation of 90# pitch.

Claims

1. a method utilizing coal direct liquefaction residue to prepare road asphalt, is characterized in that, method is carried out according to the following steps:

Step 1, under the condition of 100-150°C, dissolving and soaking the coal direct liquefaction residue powder in coal tar so that the asphaltene in the coal direct liquefaction residue is immersed in the coal tar to obtain a mixture, wherein the coal direct liquefaction residue powder and coal The mass ratio of tar is 1: (1~3);

Step 2, filtering the mixture obtained in Step 1 at 100-150° C. to obtain a filter residue containing coal tar and a coal tar filtrate containing asphaltenes;

Step 3, cooling the coal tar filtrate obtained in step 2 to 30-50° C. to precipitate asphaltene from the coal tar to obtain asphaltenes and coal tar;

Step 4, mixing the asphaltenes obtained in step 3, the direct coal liquefaction residue powder and petroleum asphalt at 130-200°C to obtain road asphalt, wherein the mixture of the asphaltene obtained in step 3 and the coal direct liquefaction residue powder The mass ratio is (0.2-1): 1, and the added mass of petroleum asphalt is 20%-50% of the total mass of asphaltene and coal direct liquefaction residue;

The particle diameter of the coal direct liquefaction residue powder is less than 1mm.

2. the method for preparing road asphalt by utilizing coal direct liquefaction residue as claimed in claim 1, is characterized in that, the coal tar described in step 1 is the medium-low temperature coal tar that the density that obtains is less than 1.0g/cm3 in the low-temperature dry distillation of bituminous coal .

3. The method for preparing road asphalt using coal direct liquefaction residue as claimed in claim 1, characterized in that in step 2, the mixture is filtered through a filter screen with a filter hole size of 45-75 μm.

4. the method for utilizing coal direct liquefaction residue to prepare road asphalt as claimed in claim 1, is characterized in that, utilizes the method for gas stripping to reclaim the coal tar in the gained filter residue in step 2 in the method, the coal tar that reclaims is used as step The source of coal tar used in one, and the filter residue after recovering coal tar is used as boiler fuel to produce steam, and the steam obtained is used to provide a heat source for the conditions described in step 1, step 2 and step 4 of the method.

5. the method for preparing road asphalt by utilizing coal direct liquefaction residue as claimed in claim 1, is characterized in that, reclaims the coal tar gained in step 3 in the method, and the coal tar that reclaims is used as the coal tar used in step 1 source.