CN106365944A - Method for preparing polymerization-grade propylene through liquefied petroleum gas separation - Google Patents
Method for preparing polymerization-grade propylene through liquefied petroleum gas separation Download PDFInfo
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- CN106365944A CN106365944A CN201610778452.1A CN201610778452A CN106365944A CN 106365944 A CN106365944 A CN 106365944A CN 201610778452 A CN201610778452 A CN 201610778452A CN 106365944 A CN106365944 A CN 106365944A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/005—Processes comprising at least two steps in series
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/04—Purification; Separation; Use of additives by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/12—Purification; Separation; Use of additives by adsorption, i.e. purification or separation of hydrocarbons with the aid of solids, e.g. with ion-exchangers
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/144—Purification; Separation; Use of additives using membranes, e.g. selective permeation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/148—Purification; Separation; Use of additives by treatment giving rise to a chemical modification of at least one compound
- C07C7/14833—Purification; Separation; Use of additives by treatment giving rise to a chemical modification of at least one compound with metals or their inorganic compounds
- C07C7/1485—Purification; Separation; Use of additives by treatment giving rise to a chemical modification of at least one compound with metals or their inorganic compounds oxides; hydroxides; salts
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Abstract
The invention discloses a method for preparing polymerization-grade propylene through liquefied petroleum gas separation. According to the method, low-quality liquefied petroleum gas of heavy oil coking byproducts is used as raw materials; through the processes of liquefied petroleum gas hydrogen sulfide removal, liquefied petroleum gas thioalcohol removal, liquefied petroleum gas rectification, crude propylene dehydration and crude propylene carbonyl sulfide removal, a propylene product is prepared from the low-quality liquefied petroleum gas through separation; in the liquefied petroleum gas rectification process, carbonyl sulfide has the similar boiling point to propylene, and cannot be removed in an ordinary rectification mode. The method has the advantages that the carbonyl sulfide is removed through a carbonyl sulfide hydrolysis tank to obtain the polymerization-grade propylene product; the dehydration is performed in a mode of series connection of a coalescence dehydrater and a flake caustic soda dehydration tank; the moisture residue in the propylene product is strictly controlled; the application value of the liquefied petroleum gas is greatly improved.
Description
Technical field
The invention belongs to petrochemical industry, more particularly to a kind of coking liquefied gas separation polymerization-grade propylene processed
Method.
Background technology
China is the rare country of petroleum resources, and substantial amounts of oil needs import.In recent years, oil in world wide
Imbalance between supply and demand increasingly intensifies.China processes the quality of crude oil, increasingly heaviness and in poor quality.Coking is as processing poor oil
Important method, has obtained fairly common application in the refinery in coastal cities.
, because of its low quality, sulfur, nitrogen content are high, and actual application value is relatively low for carbonization produced liquefied gas, are mostly only used as firing
Material uses, and causes the waste of resource.In this partial liquefaction gas, propylene content there are about 15-18wt%, if can return this part propylene
Receive and utilize, and purification is polymerization-grade propylene, then be greatly improved the using value of coking liquefied gas.
Content of the invention
In view of the shortcomings of the prior art, it is an object of the invention to provide a kind of coking liquefied gas separates polymer grade processed
The method of propylene, solving coking liquefied gas in prior art could not make full use of, and cause the problem of the wasting of resources, by one be
Row technique, extracts polymer grade polypropylene from coking liquefied gas, improves the using value of coking liquefied gas.
For achieving the above object, the technical scheme is that a kind of coking liquefied gas separates polymer grade third processed
The method of alkene it is characterised in that: comprise the following steps:
A, coking desulfuration of liquefied gas hydrogen: send into desulfuration of liquefied gas hydrogen tower after coking liquefied gas is pressurizeed, in liquefied gas
The bottom-up flowing of coking liquefied gas in de-hydrogen sulfide column, compounding desulfurizing agent from up to down flows, both counter current contacting, coking liquid
In activating QI, hydrogen sulfide is combined with compounding desulfurizing agent, discharges from tower bottom with compounding desulfurizing agent, not hydrogen sulfide containing coking liquefied gas
Discharge from top of tower；
B, coking liquid gas sweetening: the coking liquefied gas after depriving hydrogen sulphide enters alkali cleaning fibrous membrane removal of mercaptans tank, adopt
Traditional alkali cleaning fibrous membrane contact method removes the mercaptan in coking liquefied gas；
C, coking liquefied gas rectification: the coking liquefied gas after depriving hydrogen sulphide removal of mercaptans is successively through depropanizing tower, dethanizer
Isolate ethane in liquefied gas, propane and butane with propylene tower rectification, obtain crude propylene；
D, crude propylene dehydration: crude propylene first carries out preliminary hydro-extraction through coalescence drain sump, then takes off further through piece alkali dehydrating tower
Water, water content in crude propylene is down to below 10ppm；
E, crude propylene take off cos: the crude propylene after dehydration enters the de- cos tank of hydrolysis, under described hydrolyzing carbonyl sulfur tank
Layer is provided with carbonyl sulfide hydrolysis agent, and in order to remove cos in crude propylene, upper strata is provided with zinc oxide fine desulfurizer, in order to inhale
The hydrogen sulfide that attached water solution produces；
F, out enter exsiccator from the de- cos tank of hydrolysis afterwards and be dried.
The device that coking liquefied gas separates polymerization-grade propylene processed includes desulfuration of liquefied gas hydrogen tower, alkali cleaning fibrous membrane removal of mercaptans
Tank, depropanizing tower, dethanizer, propylene tower, coalescence drain sump, piece alkali drain sump, the de- cos tank of hydrolysis and exsiccator；Raw material
The feeding line of coking liquefied gas is connected with the first charging aperture of desulfuration of liquefied gas hydrogen tower, the feeding line of compounding desulfurizing agent and
The second charging aperture of desulfuration of liquefied gas hydrogen tower is connected, the first discharging opening of desulfuration of liquefied gas hydrogen tower and alkali cleaning fibrous membrane desulfurization
The first charging aperture of alcohol tank is connected, and the second discharging opening of desulfuration of liquefied gas hydrogen tower is used for discharging compounding desulfurizing agent, alkali cleaning fiber
The second charging aperture of film removal of mercaptans tank is connected with the feeding line of alkali liquor, the first discharging opening of alkali cleaning fibrous membrane removal of mercaptans tank with de-
The charging aperture of propane tower is connected, and the second discharging opening of alkali cleaning fibrous membrane removal of mercaptans tank is connected with the discharge pipe of alkali liquor；Depropanization
The tower top outlet of tower is connected with the charging of dethanizer, and the bottom of towe of depropanizing tower exports for discharging c4+ fraction；Dethanizer
Bottom of towe outlet is connected with the feeding line of propylene tower, and the tower top outlet of dethanizer is used for discharging c2 fraction, the tower top of propylene tower
Crude propylene discharging opening is connected with the import of coalescence drain sump, and the bottom of towe discharging of propylene tower is used for discharging propane；Coalescence drain sump
Outlet is connected with the bottom feed mouth of piece alkali drain sump, and the top exit of piece alkali drain sump is entered with the bottom of the de- cos tank of hydrolysis
Material mouth is connected, and the top exit of the de- cos tank of hydrolysis is connected with the bottom inlet of exsiccator, and the top exit of exsiccator is used for
Discharge polymerization-grade propylene product.
As a further improvement on the present invention, described desulfuration of liquefied gas hydrogen tower temperature degree 30-40 degree, pressure 0.2-
0.3mpa.
As a further improvement on the present invention, described compounding desulfurizing agent include the amorphous FeOOH of 10-20 weight portion,
10-20 weight portion chelating agent, 70-80 weight portion n- methyl diethanolamine, 15-30 weight portion NHD, 0.1-0.4
Weight portion antioxidant and 5-10 weight portion reinforcing agent.
As a further improvement on the present invention, described chelating agent be disodiumedetate, sodium tartrate or Jiao
One of sodium phosphate.
As a further improvement on the present invention, described antioxidant is 2,6- DI-tert-butylphenol compounds, MEHQ or two
One of ethylhydroxyl amine.
As a further improvement on the present invention, described reinforcing agent is one or more of sodium bicarbonate or ammonium hydrogen carbonate.
As a further improvement on the present invention, described carbonyl sulfide hydrolysis agent includes 20-30 parts by weight sodium carbonate, 2-10 weight
Part zirconium oxide, 2-15 weight portion praseodymium oxide, 1-10 weight portion cobalt oxide, 70-80 weight portion aluminium sesquioxide.
The present invention with the low-quality coking liquefied gas of coking heavy oil institute by-product as raw material, by coking desulfuration of liquefied gas
Hydrogen, coking liquid gas sweetening, coking liquefied gas rectification, crude propylene dehydration and crude propylene take off the technique of cos, from low-quality
Coking liquefied gas in separate preparation propylene product, in coking liquefied gas distillation process, cos are close with propylene boiling point, no
Method is removed by the way of conventional distillation, and cos are removed by the present invention by hydrolyzing carbonyl sulfur tank, have obtained polymerization-grade propylene
Product, is dehydrated by the way of coalescence dehydrator and piece alkali drain sump serial operation, strictly controls moisture content in propylene product residual
Stay, greatly improve the using value of coking liquefied gas.
Brief description
Fig. 1 is the structural representation of the inventive method related device.
Specific embodiment
Below in conjunction with the embodiment given by accompanying drawing, the present invention is described in further detail.
As shown in figure 1, the adopted device of method of coking liquefied gas separation polymerization-grade propylene processed is as follows in the present invention: coking
Liquefied gas separate polymerization-grade propylene processed device include desulfuration of liquefied gas hydrogen tower, alkali cleaning fibrous membrane removal of mercaptans tank, depropanizing tower,
Dethanizer, propylene tower, coalescence drain sump, piece alkali drain sump, the de- cos tank of hydrolysis and exsiccator；Raw material coking liquefied gas
Feeding line is connected with the first charging aperture of desulfuration of liquefied gas hydrogen tower, the feeding line of compounding desulfurizing agent and desulfuration of liquefied gas
The second charging aperture of hydrogen tower is connected, and the first of the first discharging opening of desulfuration of liquefied gas hydrogen tower and alkali cleaning fibrous membrane removal of mercaptans tank enters
Material mouth is connected, and the second discharging opening of desulfuration of liquefied gas hydrogen tower is used for discharging compounding desulfurizing agent, alkali cleaning fibrous membrane removal of mercaptans tank
Second charging aperture is connected with the feeding line of alkali liquor, the first discharging opening of alkali cleaning fibrous membrane removal of mercaptans tank and the charging of depropanizing tower
Mouth is connected, and the second discharging opening of alkali cleaning fibrous membrane removal of mercaptans tank is connected with the discharge pipe of alkali liquor；The tower top outlet of depropanizing tower
It is connected with the charging of dethanizer, the bottom of towe of depropanizing tower exports for discharging c4+ fraction；The bottom of towe outlet and third of dethanizer
The feeding line of alkene tower is connected, and the tower top outlet of dethanizer is used for discharging c2 fraction, the tower top crude propylene discharging opening of propylene tower
Import with coalescence drain sump is connected, and the bottom of towe discharging of propylene tower is used for discharging propane；The outlet of coalescence drain sump and piece alkali take off
The bottom feed mouth of water pot is connected, and the top exit of piece alkali drain sump is connected with the bottom feed mouth of the de- cos tank of hydrolysis, water
The bottom inlet of the top exit and exsiccator of freeing cos tank is connected, and the top exit of exsiccator is used for discharging polymer grade third
Alkene product.
As follows using compounding desulfurizing agent preparation process in the present invention:
(1) the amorphous FeOOH of 10-20 weight portion, 10-20 weight portion chelating agent, the increasing of 5-10 weight portion are weighed successively
Strong agent and 50 parts by weight of deionized water, are added in mixing kettle, stir 30-60 minute, mix homogeneously under 800-1000r/min
Add 15-30 weight portion NHD afterwards.
(2) under 1000-3000r/min stirring, 70-80 weight portion n- methyl diethanolamine, 0.1-0.4 weight portion are resisted
Oxygen agent adds in mixing kettle, stirs 20-50 minute.
Adopt carbonyl sulfide hydrolysis agent preparation process as follows in the present invention:
Weigh 20-30 parts by weight sodium carbonate, 2-10 weight portion zirconium oxide, 2-15 weight portion praseodymium oxide, 1-10 weight respectively
Part cobalt oxide, 70-80 weight portion aluminium sesquioxide, add 80-90 parts by weight of deionized water, hydrothermal treatment consists 4 under the conditions of 80 DEG C
Hour, stand 5 hours；Then in 100 DEG C of dryings 10 hours, tabletting, broken, sieve take the sample of 10～20 mesh to obtain required catalysis
Agent.
Embodiment 1
A, coking desulfuration of liquefied gas hydrogen: raw material is low-quality Jiao of propylene content 15-18wt% coking heavy oil institute by-product
Change liquefied gas, after coking liquefied gas is pressurizeed, send into desulfuration of liquefied gas hydrogen tower, 30 degree of desulfuration of liquefied gas hydrogen tower temperature degree, pressure
0.2mpa, the bottom-up flowing of coking liquefied gas in desulfuration of liquefied gas hydrogen tower, compounding desulfurizing agent a from up to down flows, and two
Person's counter current contacting, in coking liquefied gas, hydrogen sulfide is combined with compounding desulfurizing agent a, discharges from tower bottom with compounding desulfurizing agent a, does not contain
The coking liquefied gas of hydrogen sulfide is discharged from top of tower；
B, coking liquid gas sweetening: the coking liquefied gas after depriving hydrogen sulphide enters alkali cleaning fibrous membrane removal of mercaptans tank, adopt
Traditional alkali cleaning fibrous membrane contact method removes the mercaptan in coking liquefied gas；
C, coking liquefied gas rectification: the coking liquefied gas after depriving hydrogen sulphide removal of mercaptans is successively through depropanizing tower, dethanizer
Isolate ethane in liquefied gas, propane and butane with propylene tower rectification, obtain crude propylene；
D, crude propylene dehydration: crude propylene first carries out preliminary hydro-extraction through coalescence drain sump, then takes off further through piece alkali dehydrating tower
Water, water content in crude propylene is down to below 10ppm；
E, crude propylene take off cos: the crude propylene after dehydration enters the de- cos tank of hydrolysis, under described hydrolyzing carbonyl sulfur tank
Layer is provided with carbonyl sulfide hydrolysis agent a, and in order to remove cos in crude propylene, upper strata is provided with zinc oxide fine desulfurizer, in order to
The hydrogen sulfide that adsorption of hydrolyzation produces；
F, out enter exsiccator from the de- cos tank of hydrolysis afterwards and be dried.
Embodiment 2
A, coking desulfuration of liquefied gas hydrogen: raw material is low-quality Jiao of propylene content 15-18wt% coking heavy oil institute by-product
Change liquefied gas, after coking liquefied gas is pressurizeed, send into desulfuration of liquefied gas hydrogen tower, 35 degree of desulfuration of liquefied gas hydrogen tower temperature degree, pressure
0.25mpa, the bottom-up flowing of coking liquefied gas in desulfuration of liquefied gas hydrogen tower, compounding desulfurizing agent b from up to down flows, and two
Person's counter current contacting, in coking liquefied gas, hydrogen sulfide is combined with compounding desulfurizing agent b, discharges from tower bottom with compounding desulfurizing agent b, does not contain
The coking liquefied gas of hydrogen sulfide is discharged from top of tower；
B, coking liquid gas sweetening: the coking liquefied gas after depriving hydrogen sulphide enters alkali cleaning fibrous membrane removal of mercaptans tank, adopt
Traditional alkali cleaning fibrous membrane contact method removes the mercaptan in coking liquefied gas；
C, coking liquefied gas rectification: the coking liquefied gas after depriving hydrogen sulphide removal of mercaptans is successively through depropanizing tower, dethanizer
Isolate ethane in liquefied gas, propane and butane with propylene tower rectification, obtain crude propylene；
D, crude propylene dehydration: crude propylene first carries out preliminary hydro-extraction through coalescence drain sump, then takes off further through piece alkali dehydrating tower
Water, water content in crude propylene is down to below 10ppm；
E, crude propylene take off cos: the crude propylene after dehydration enters the de- cos tank of hydrolysis, under described hydrolyzing carbonyl sulfur tank
Layer is provided with carbonyl sulfide hydrolysis agent b, and in order to remove cos in crude propylene, upper strata is provided with zinc oxide fine desulfurizer, in order to
The hydrogen sulfide that adsorption of hydrolyzation produces；
F, out enter exsiccator from the de- cos tank of hydrolysis afterwards and be dried.
Embodiment 3
A, coking desulfuration of liquefied gas hydrogen: raw material is low-quality Jiao of propylene content 15-18wt% coking heavy oil institute by-product
Change liquefied gas, after coking liquefied gas is pressurizeed, send into desulfuration of liquefied gas hydrogen tower, 40 degree of desulfuration of liquefied gas hydrogen tower temperature degree, pressure
0.3mpa, the bottom-up flowing of coking liquefied gas in desulfuration of liquefied gas hydrogen tower, compounding desulfurizing agent c from up to down flows, and two
Person's counter current contacting, in coking liquefied gas, hydrogen sulfide is combined with compounding desulfurizing agent c, discharges from tower bottom with compounding desulfurizing agent c, does not contain
The coking liquefied gas of hydrogen sulfide is discharged from top of tower；
B, coking liquid gas sweetening: the coking liquefied gas after depriving hydrogen sulphide enters alkali cleaning fibrous membrane removal of mercaptans tank, adopt
Traditional alkali cleaning fibrous membrane contact method removes the mercaptan in coking liquefied gas；
C, coking liquefied gas rectification: the coking liquefied gas after depriving hydrogen sulphide removal of mercaptans is successively through depropanizing tower, dethanizer
Isolate ethane in liquefied gas, propane and butane with propylene tower rectification, obtain crude propylene；
D, crude propylene dehydration: crude propylene first carries out preliminary hydro-extraction through coalescence drain sump, then takes off further through piece alkali dehydrating tower
Water, water content in crude propylene is down to below 10ppm；
E, crude propylene take off cos: the crude propylene after dehydration enters the de- cos tank of hydrolysis, under described hydrolyzing carbonyl sulfur tank
Layer is provided with carbonyl sulfide hydrolysis agent c, and in order to remove cos in crude propylene, upper strata is provided with zinc oxide fine desulfurizer, in order to
The hydrogen sulfide that adsorption of hydrolyzation produces；
F, out enter exsiccator from the de- cos tank of hydrolysis afterwards and be dried.
The propylene situation that different embodiments obtain is as in the table below:
The above is only the preferred embodiment of the present invention, and protection scope of the present invention is not limited merely to above-mentioned enforcement
Example, all technical schemes belonging under thinking of the present invention belong to protection scope of the present invention.It should be pointed out that for the art
Those of ordinary skill for, some improvements and modifications without departing from the principles of the present invention, these improvements and modifications
Should be regarded as protection scope of the present invention.
Claims (7)
1. a kind of coking liquefied gas separate polymerization-grade propylene processed method it is characterised in that: comprise the following steps:
A, coking desulfuration of liquefied gas hydrogen: send into desulfuration of liquefied gas hydrogen tower after coking liquefied gas is pressurizeed, in desulfuration of liquefied gas
Change the bottom-up flowing of coking liquefied gas in hydrogen tower, compounding desulfurizing agent from up to down flows, both counter current contacting, coking liquefied gas
Middle hydrogen sulfide is combined with compounding desulfurizing agent, discharges from tower bottom with compounding desulfurizing agent, not hydrogen sulfide containing coking liquefied gas is from tower
Top is discharged；
B, coking liquid gas sweetening: the coking liquefied gas after depriving hydrogen sulphide enters alkali cleaning fibrous membrane removal of mercaptans tank, using alkali cleaning
Fibrous membrane contact method removes the mercaptan in coking liquefied gas；
C, coking liquefied gas rectification: the coking liquefied gas after depriving hydrogen sulphide removal of mercaptans is successively through depropanizing tower, dethanizer and third
Ethane in liquefied gas, propane and butane are isolated in alkene tower rectification, obtain crude propylene；
D, crude propylene dehydration: crude propylene first carries out preliminary hydro-extraction through coalescence drain sump, then is dehydrated further through piece alkali dehydrating tower, will
In crude propylene, water content is down to below 10ppm；
E, crude propylene take off cos: the crude propylene after dehydration enters the de- cos tank of hydrolysis, and described hydrolyzing carbonyl sulfur tank lower floor sets
It is equipped with carbonyl sulfide hydrolysis agent, in order to remove cos in crude propylene, upper strata is provided with zinc oxide fine desulfurizer, in order to adsorb water
The hydrogen sulfide that solution produces；
F, out enter exsiccator from the de- cos tank of hydrolysis afterwards and be dried.
2. coking liquefied gas according to claim 1 separate polymerization-grade propylene processed method it is characterised in that: described liquefaction
QI prostration hydrogen sulfide tower temperature degree 30-40 degree, pressure 0.2-0.3mpa.
3. coking liquefied gas according to claim 2 separate polymerization-grade propylene processed method it is characterised in that: described compound
Desulfurizing agent includes the amorphous FeOOH of 10-20 weight portion, 10-20 weight portion chelating agent, 70-80 weight portion n- methyl diethyl
Hydramine, 15-30 weight portion NHD, 0.1-0.4 weight portion antioxidant and 5-10 weight portion reinforcing agent.
4. coking liquefied gas according to claim 3 separate polymerization-grade propylene processed method it is characterised in that: described network
Mixture is disodiumedetate, one of sodium tartrate or sodium pyrophosphate.
5. coking liquefied gas according to claim 4 separate polymerization-grade propylene processed method it is characterised in that: described antioxygen
Agent is one of 2,6- DI-tert-butylphenol compounds, MEHQ or diethyl hydroxylamine.
6. coking liquefied gas according to claim 5 separate polymerization-grade propylene processed method it is characterised in that: described enhancing
Agent is one or more of sodium bicarbonate or ammonium hydrogen carbonate.
7. coking liquefied gas according to any one of claim 1-6 separate polymerization-grade propylene processed method it is characterised in that:
Described carbonyl sulfide hydrolysis agent includes 20-30 parts by weight sodium carbonate, 2-10 weight portion zirconium oxide, 2-15 weight portion praseodymium oxide, 1-10
Weight portion cobalt oxide, 70-80 weight portion aluminium sesquioxide.
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| CN107188776A (en) * | 2017-06-09 | 2017-09-22 | 中石化上海工程有限公司 | The removal methods of acid impurities in ethylene cracking gas |
| CN113088331A (en) * | 2021-04-09 | 2021-07-09 | 南京金炼科技有限公司 | Process and system for sweetening alcohol and decarbonylation sulfur |
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| CN107188776A (en) * | 2017-06-09 | 2017-09-22 | 中石化上海工程有限公司 | The removal methods of acid impurities in ethylene cracking gas |
| CN113088331A (en) * | 2021-04-09 | 2021-07-09 | 南京金炼科技有限公司 | Process and system for sweetening alcohol and decarbonylation sulfur |
| CN116903431A (en) * | 2023-09-07 | 2023-10-20 | 山东寿光鲁清石化有限公司 | Method for preparing propylene by purifying coked liquefied gas |
| CN116903431B (en) * | 2023-09-07 | 2023-12-26 | 山东寿光鲁清石化有限公司 | Method for preparing propylene by purifying coked liquefied gas |
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