Automatic separation apparatus for four fractions of heavy oil and separation method thereof

Patent metadata

Field	Value
Publication number	US-12544690-B2
Application number	US-202017772367-A
Country	US
Kind code	B2
Filing date	Oct 26, 2020
Priority date	Oct 28, 2019
Publication date	Feb 10, 2026
Grant date	Feb 10, 2026

Abstract

The present disclosure provides an automatic separation apparatus for four fractions of heavy oil and a separation method thereof, wherein the apparatus includes a solvent reservoir tank ( 1 ), a separation unit for four fractions of heavy oil ( 100 ) and a receiving apparatus ( 9 ). The separation unit for four fractions of heavy oil ( 100 ) includes: a filter disc ( 4 ) having one end in communication with the solvent reservoir tank ( 1 ), and the other end in communication with an inlet of a pre-column flow path switching valve ( 5 ); a chromatographic column ( 6 ) having an inlet in communication with an outlet of the pre-column flow path switching valve ( 5 ), and an outlet in communication with an inlet of a post-column flow path switching valve ( 8 ). The receiving apparatus is in communication with an outlet of the post-column flow path switching valve ( 8 ).

First claim

What is claimed is:

1 . An automatic separation apparatus for four fractions of heavy oil, comprising:
(a) a solvent reservoir tank; (b) a separation unit for the four fractions of heavy oil, comprising:
(i) a filter disc having one end in communication with the solvent reservoir tank, and an opposing end in communication with a first inlet of a pre-column flow path switching valve;
(ii) a chromatographic column having an inlet in communication with a first outlet of the pre-column flow path switching valve, and an outlet in communication with a first inlet of a post-column flow path switching valve; and
(iii) a bypass pipeline having one end in communication with a second outlet of the pre-column flow path switching valve, and an opposing end in communication with a second inlet of the post-column flow path switching valve;
(c) a receiving apparatus in communication with an outlet of the post-column flow path switching valve;
wherein a number of the separation unit for the four fractions of heavy oil is n, wherein n is an integer greater than or equal to 1, and the separation unit for the four fractions of heavy oil is used to perform automatic separation processes of the four fractions of heavy oil simultaneously in parallel;
wherein the automatic separation apparatus for the four fractions of heavy oil further comprises: a liquid splitting apparatus comprising a heating element and being arranged between the solvent reservoir tank and the separation unit for the four fractions of heavy oil; the liquid splitting apparatus comprising a splitter and n paths of metal pipes with equal back pressures, the number of the metal pipes being equal to the number of separation units for the four fractions of heavy oil, and liquid outlet ends of respective metal pipes being in communication with liquid inlet ends of respective separation units for the four fractions of heavy oil in a one-to-one correspondence;
wherein the receiving apparatus is an automatic receiving apparatus for eluent which is made of aluminum-plastic materials, comprising a box, a receiving container arranged in the box a transmission apparatus, and a liquid channel; and
wherein the receiving container is arranged at a bottom of the box, the transmission apparatus is arranged above the receiving container, the transmission apparatus is provided with the liquid channel, and an outlet of the liquid channel faces the receiving container.

2 . The automatic separation apparatus for the four fractions of heavy oil according to claim 1 , further comprising:
a sample loading apparatus arranged between the filter disc and the solvent reservoir tank; and a pump arranged between the solvent reservoir tank and the sample loading apparatus.

3 . The automatic separation apparatus for the four fractions of heavy oil according to claim 1 , wherein the splitter comprises one inlet and n outlets; and
wherein the one inlet of the splitter serves as a liquid inlet end, and respective outlets of the splitter are in communication with respective inlets of the metal pipes in a one-to-one correspondence.

4 . The automatic separation apparatus for the four fractions of heavy oil according to claim 3 , wherein the splitter comprises at least one multi-way pipe with three or more ways;
wherein the multi-way pipe has branch pipes with equal inner diameters and equal total lengths; and wherein the metal pipes have inner diameters of 0.05 mm to 0.5 mm and length-to-diameter ratios of 5000:1-50000:1.

5 . The automatic separation apparatus for the four fractions of heavy oil according to claim 3 , wherein the liquid splitting apparatus further comprises:
a fixing element that is a metal sheet with a plurality of grooves; wherein the metal sheet is arranged on the heating element; and wherein each of the metal pipes is wound on the fixing element in sections.

6 . The automatic separation apparatus for the four fractions of heavy oil according to claim 1 , further comprising:
a column oven; wherein the separation unit for the four fractions of heavy oil is provided inside the column oven; and wherein a heater and a fan are further provided inside the column oven with the fan being placed behind the heater.

7 . The automatic separation apparatus for the four fractions of heavy oil according to claim 1 , wherein the filter disc is provided with a layer of filter membrane or multi layers of filter membranes; and
wherein the filter membrane or the filter membranes has a pore size of 0.1 μm-100 μm.

8 . The automatic separation apparatus for the four fractions of heavy oil according to claim 1 , wherein a packing material of the chromatographic column is alumina having a specific surface area of 150 m 2 /g to 200 m 2 /g and a pore volume of 0.25 mL/g to 0.35 mL/g;
wherein a mass of the alumina having a particle size of 60 microns-200 microns accounts for 60%-80% of a total mass of the packing material; wherein an amount of the alumina is not less than 20 g/g of a sample of the heavy oil; and wherein a column layer after packing of the alumina has a height-to-diameter ratio of not less than 5:1, and a density of not less than 0.8 g/m 3 .

9 . The automatic separation apparatus for the four fractions of heavy oil according to claim 1 ,
wherein the receiving apparatus comprises a heating component arranged on an outer surface of the receiving container;
wherein the receiving apparatus comprises a vent hole opened on top of the box; and
wherein the receiving container has a thickness of 0.1 mm-1 mm and a capacity of 10 mL-50 mL.

10 . A separation method for the four fractions of heavy oil, applied in the automatic separation apparatus for four fractions of heavy oil according to claim 1 , comprising the following steps of:
S1: adding the heavy oil dispersed with a first solvent into the separation unit for four fractions of heavy oil, the heavy oil flowing through the filter disc and the chromatographic column sequentially, and using the first solvent to flush the separation unit for the four fractions of heavy oil, to obtain a saturates eluent; S2: switching the pre-column flow path switching valve and the post-column flow path switching valve, adding a second solvent into the separation unit for the four fractions of heavy oil for flushing, and the second solvent flowing through the filter disc and the bypass pipeline sequentially, to obtain an asphaltenes eluent; S3: switching the pre-column flow path switching valve and the post-column flow path switching valve, adding the second solvent into the separation unit for the four fractions of heavy oil for flushing, and the second solvent flowing through the filter disc and the chromatographic column sequentially, to obtain an aromatics eluent; and S4: adding a third solvent, the second solvent, and a fourth solvent sequentially into the separation unit for the four fractions of heavy oil for flushing, to obtain a resins eluent, and using the receiving apparatus to collect eluents respectively obtained in S1-S4.

11 . The separation method for the four fractions of heavy oil according to claim 10 , further comprising a step of S5: removing a solvent from the collected eluent for each fraction, to obtain separated four fractions of heavy oil.

12 . The separation method for the four fractions of heavy oil according to claim 10 , wherein boiling points of the first solvent, the second solvent, the third solvent, and the fourth solvent are lower than 150° C.

13 . The separation method for the four fractions of heavy oil according to claim 12 , wherein:
the first solvent is an organic solvent capable of dissolving saturates, a

Assignees

• Petrochina Co Ltd
• Beijing Orienda Instr Co Ltd

Inventors

• Cao Qing
• Wen Dawei
• He Shengbao
• Xiu Yuan
• Tian Lin
• Yang Dingzhong
• He Jing
• Dou Minna
• Chen Fei
• Liu Kunhong
• Li Chenchen
• Xue Huifeng
• Wang Jianming

Classifications

• G01N2030/027

  Liquid chromatography · CPC title

• G01N30/38

  Flow patterns · CPC title

• G01N30/06

  Preparation · CPC title

• C10G25/003

  Specific sorbent material, not covered by C10G25/02 or C10G25/03 · CPC title

• B01J2220/52

  Sorbents specially adapted for preparative chromatography · CPC title