CN1056704A

CN1056704A - Dead oil catalytic distillation technology

Info

Publication number: CN1056704A
Application number: CN 91106161
Authority: CN
Inventors: 尚崇礼
Original assignee: Individual
Current assignee: Individual
Priority date: 1991-06-25
Filing date: 1991-06-25
Publication date: 1991-12-04
Anticipated expiration: 2006-06-25
Also published as: CN1030504C

Abstract

The present invention is applicable to the dead oil catalytic distillation technology of processing heavy oil, characteristics be with crude distillation go out the gasoline solar oil through after mink cell focus, add a certain amount of natural catalyst---atlapulgite or coke powder, reaction at a certain temperature, its product is except a part of Jiao  (can be used as fuel), all become solar oil, gasoline or petrol gas, both can have the part characteristics of catalytic cracking process concurrently, can remedy the deficiency of delay coking process again.This technology is processing crude oil directly, waste lubricating oil and other unclean oil product etc.This technology also has simple, the flexible operation of equipment, easily characteristics such as realization.

Description

Dead oil catalytic distillation technology

The present invention relates to the improvement of petroleum refining process method, particularly a kind of with the processing method of mink cell focus through catalytic distillation processed finished products oil.

Mink cell focus after the general refinery time processing, adopt following two kinds of technologies: the one, do not popularize in an all-round way as yet at present, the just long residuum catalytic cracking of exploitation in recent years, used fluidized bed operating condition harshness, catalyzer is a Y molecular sieve, the cost height, and reaction and regeneration temperature are at 470-650 ℃ in addition, equipment material is used steel alloy more, so high price and complexity.The 2nd, delayed coking process, the former is heavier for employed raw material ratio, is vacuum residuum, and coking temperature for fear of coking in process furnace, must be sneaked into a large amount of moisture content up to 520 ℃, causes the stove inlet pressure at 25Kg/cm ²More than, its coke tower complexity of the discharging of the coke, operational condition is abominable, and must intermittent operation, and product stability is poor, and its wax oil is still the raw material of catalytic cracking.

The object of the present invention is to provide a kind of dead oil catalytic distillation technology that improves the light-end products output capacity, it is simple that this technology also has equipment, flexible operation, characteristics such as realization easily.

The object of the present invention is achieved like this: mink cell focus (or crude oil) is squeezed in the material-compound tank, the catalyzer (atlapulgite or coke powder) and the abundant mixing that under 100-200 ℃ of temperature, add its weight 1.5-10%, suspension behind the mixing squeezed into carry out reacting by heating in the reaction distillation still, temperature of reaction is 350-450 ℃ at the bottom of the still, recovered temperature is 150-280 ℃, reaction times is 3-24 hour, be cooled to 30-50 ℃ by still top distilled reaction product, make liquid, gas mixture enter in the middle separating tank; Above-mentioned condensed liquid squeezed into be heated to 250-350 ℃ in the process furnace, make the gas-liquid mixed of its generation enter the middle part of separation column mutually, this tower is with reflux ratio 1-5: 1 operation, pressure is 0.1-0.5Kg/cm ²(table), tower top temperature are 80-120 ℃, enter in the withdrawing oil jar after overhead product is cooled to 30-50 ℃, and then the boiling range that distillates gasoline from top of tower is 30-200 ℃, are 150-320 ℃ from the boiling range of tower middle part distillate diesel fuel.The weight percent of the above-mentioned contained composition of atlapulgite is: SiO ₂40-60%, Al ₂O ₃10-30%, Fe ₂O ₃0-5%, CaO0.5%, CuO0.5%, MgO0.5%, surplus is a water.The concrete structure of the reaction distillation still during above-mentioned process using operate continuously is: a rotary roller is arranged, bottom in cylinder is provided with an oil pipe that is evenly equipped with tap hole, this oil pipe links to each other with the material feeding tube that enters cylinder one end, at the middle part of cylinder one U type scraper plate is set upwards vertically, worm conveyor is housed in the scraper plate, and the other end and the separator of cylinder link.

The present invention contacts raw material in 350-450 ℃ of scope with solid catalyst, can promote macromolecular cracking, be not subjected to the restriction of air speed in liquid phase reaction, its reaction heat constantly is boiling state by supplying with at the bottom of the still, the lightweight oil of reaction is overflowed by the still top, until all becoming lightweight oil and coke.The present invention solves the deficiency of delay coking process because production technique is simple, and reaction conditions is loose, is particularly suitable for middle-size and small-size petroleum refining industry, can produce the light-end products of 80-93%.Above-mentioned reaction is to carry out in a reactor that can heat, and reactor can be the discontinuous operation, expects continuously preferably and the operation of the discharging of the coke that the latter realizes (as shown in Figure 2) by a rotatable reactor.

Below in conjunction with accompanying drawing specific embodiments of the present invention is further described.

Fig. 1 is a process flow sheet of the present invention.

Fig. 2 is a continous way operant response still kettle structural representation of the present invention.

Fig. 3 is the side-view of Fig. 2.

Referring to Fig. 1, concrete technology of the present invention is: with mink cell focus 16 is raw material, in material-compound tank 1, mix down 100-200 ℃ (reducing mink cell focus viscosity) with atlapulgite 17, the blended weight ratio classifies 100 as: 1.5-10, optimum proportion is 100: 4-8, make mixture be suspension, squeeze in the reaction distillation still 3 with pump 2 then, temperature of reaction is 350-450 ℃ at the bottom of the still, reaction times is 3-24 hour, the light-end products of reaction are distillated by separator 18 tops in 150-280 ℃ of scope, and residue is used for hot refuel at the bottom of the still, light-end products are condensed to 30-50 ℃ by water cooler 4, phlegma separates in separating tank 5 with incondensable gas 15, and phlegma is squeezed into by pump 6 and is heated to 250-350 ℃ in the process furnace 8, and then the gas-liquid mixed that is generated enters the middle part of separation column 7 mutually, this separation column is with reflux ratio 1-5: 1 operation, pressure is by 0.1-0.5Kg/cm ²(table), tower top temperature are 80-120 ℃, and overhead product enters return tank 10 after water cooler 9 is cooled to 30-50 ℃.The incondensable gas 11 and 15 of discharging can be used as fuel of this flow process or further processing respectively from backflow oil tank 10 and middle separating tank 5.Is 30-200 ℃ by the separation column top through the boiling range of the product gasoline 12 of backflow oil tank 10 outputs, can be used as motor spirit; Boiling range by the product diesel oil 13 of separation column middle part output is 150-320 ℃, can be used as solar oil and enters the finished product jar, and can directly squeeze into further reaction again in the material-compound tank 1 by the last mink cell focus 14 of tower bottom.The raw material that above-mentioned technology adopted can also adopt crude oil, waste lubricating oil and other unclean oil product except that heavy oil; Its optimum weight per-cent of the atlapulgite that is adopted is: SiO ₂50-55%, Al ₂O ₃10-20%, Fe ₂O ₃0-4%, CaO0.5%, CuO0.5%, MgO0.5%, surplus is a water.This technology can adopt discontinuous operation and continous way operation, and when intermittent operation, the reaction distillation still is a horizontal heating kettle, and the still top is a packing tower, and clear up once weekly by the phase for the residue at the bottom of the still; When operate continuously, the reaction distillation still is a continuously feeding and the equipment that discharges of the coke, the concrete structure of its equipment and preceding described and referring to Fig. 2 and Fig. 3, the specific operation process of this equipment is: squeezed into by pump in the oil pipe that is evenly equipped with discharge orifice 22 in the cylinder 19 that is rotating when stock oil becomes suspension with catalyst preparation, then suspension is on tap hole enters cylinder 19 inwalls as the reaction distillation still, when the coke on the swing roller inwall and catalyst solid are thickeied gradually, and rotate the arrival top with cylinder, scrape off by the U type scraper plate 21 that upwards is provided with in the tube, and the worm conveyor 20 that is set at simultaneously in the scraper plate is transported to cooling in the water sealed tank 23 that drops on the bottom in the separator 18 down, and the overhead product of cylinder internal heating reaction enters down processing step one through the top of separator.

To further describe the present invention by embodiment below.

Embodiment one

By testing apparatus of the present invention described crude oil of table 1 and coke powder were mixed with 100: 8, progressively heat temperature raising is to the 200-300 scope by low temperature in the reaction distillation still, and reactant progressively distillated in 8 hours, result that must table 2 after the condensation.

Embodiment two

Crude oil by embodiment one, behind gasoline before steaming 300 ℃ earlier, the solar oil fraction, mink cell focus that it is last and atlapulgite are even with 100: 5 mixed, heat temperature raising in reactor 3, control distillates mouthful temperature in 200-280 ℃ of scope, first hurdle after the condensation in product yield such as the table 3.

Embodiment three

Gained result among the embodiment 2 is compared its reaction conditions and product yield such as table 3 with heavy oil fluid catalytic cracking and delayed coking.As seen from Table 3, yield of light oil of the present invention is because the latter has oily sauce not handle than catalytic cracking height, comprises liquefied gas in the gas, and identical with catalytic cracking, coke accounts for 6.5% of crude oil, and is lower than delayed coking, and lightweight oil and gas are than delayed coking height.

Claims

1, a kind of dead oil catalytic distillation technology that is applicable to processing heavy oil (or crude oil) is characterized in that:

(1), mink cell focus (or crude oil) is squeezed in the material-compound tank catalyzer (atlapulgite or coke powder) of its weight of adding 1.5-10% and abundant mixing under 100-200 ℃ of temperature;

(2), the suspension behind the mixing is squeezed into carried out reacting by heating in the reaction distillation still, temperature of reaction is 350-450 ℃ at the bottom of the still, recovered temperature is 150-280 ℃, reaction times is 3-24 hour, be cooled to 30-50 ℃ by still top distilled reaction product, make liquid, gas mixture enter in the middle separating tank;

(3), above-mentioned condensed liquid squeezed into be heated to 250-350 ℃ in the process furnace, make the gas-liquid mixed of its generation enter the middle part of separation column mutually, this tower is with reflux ratio 1-5: 1 operation, pressure is 0.1-0.5Kg/cm ²(table), tower top temperature are 80-120 ℃, enter in the withdrawing oil jar after overhead product is cooled to 30-50 ℃, and then the boiling range that distillates gasoline from top of tower is 30-200 ℃, are 150-320 ℃ from the boiling range of tower middle part distillate diesel fuel.

2, catalytic distillation technology according to claim 1 is characterized in that: residue can be used for heating raw at the bottom of the still of reaction distillation still.

3, catalytic distillation technology according to claim 1 is characterized in that: the weight percent of atlapulgite is: SiO ₂40-60%, Al ₂O ₃10-30%, Fe ₂O ₃0-5%, CaO0.5%, CuO0.5%, MgO0.5%, surplus is a water.

4, according to claim 1 or 3 described catalytic distillation technologies, it is characterized in that: the optimum range of the weight percent of atlapulgite is: SiO ₂50-55%, Al ₂O ₃10-20%, Fe ₂O ₃0-4%, CaO0.5%, CuO0.5%, MgO0.5%, surplus is a water.

5, catalytic distillation technology according to claim 1 is characterized in that: used stock oil is: crude oil or crude oil are told gasoline, last mink cell focus, waste lubricating oil and other the unclean oil product of solar oil after the normal pressure distillation.

6, catalytic distillation technology according to claim 1 is characterized in that: can be used as fuel of this technology or further processing from the insoluble gas of middle separating tank and the discharging of backflow oil tank.

7, catalytic distillation technology according to claim 1 is characterized in that: the mink cell focus that gives off from the separation column bottom is squeezed into head tank further reaction again.

8, catalytic distillation technology according to claim 1 is characterized in that:

(1), during intermittent operation, the reaction distillation still is a horizontal heating kettle, the still top is a packing tower, the phase cleaning is once weekly for the residue at the bottom of the still;

(2), during operate continuously, the reaction distillation still is a continuously feeding and the equipment that discharges of the coke.

9, catalytic distillation technology according to claim 8, it is characterized in that: the reaction distillation still of operate continuously is a rotary roller, bottom in cylinder is provided with an oil pipe that is evenly equipped with tap hole, this oil pipe links to each other with the material feeding tube that enters cylinder one end, the middle part of cylinder is vertically to being provided with a U type scraper plate, worm conveyor is housed in the scraper plate, and the other end and the separator of cylinder link.