CN105601460A - Refining method of alkylation feedstock - Google Patents
Refining method of alkylation feedstock Download PDFInfo
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- CN105601460A CN105601460A CN201510961856.XA CN201510961856A CN105601460A CN 105601460 A CN105601460 A CN 105601460A CN 201510961856 A CN201510961856 A CN 201510961856A CN 105601460 A CN105601460 A CN 105601460A
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- adsorbent
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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
- 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
- C07C7/12—Purification; Separation; Use of additives by adsorption, i.e. purification or separation of hydrocarbons with the aid of solids, e.g. with ion-exchangers
- C07C7/13—Purification; Separation; Use of additives by adsorption, i.e. purification or separation of hydrocarbons with the aid of solids, e.g. with ion-exchangers by molecular-sieve technique
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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
- C07C7/163—Purification; Separation; Use of additives by treatment giving rise to a chemical modification of at least one compound by hydrogenation
Abstract
The present invention provides a refining method of an alkylation feedstock. The method is as below: treating an alkylation feedstock containing impurity by a washing tower (1), a dewatering tower (2), a desulfurization tower (3), a dechlorination column (4), a denitrogenation column (5), an oxygenated chemicals removal column (6), a preheater (7), and a selective hydrogenation reactor (8) to obtain a purified alkylation feedstock. The refining method of the alkylation feedstock can effectively remove impurities such as sulfide, nitride, chloride and oxygenated chemicals in the alkylation feedstock, so that the alkylation feedstock has significantly reduced content of impurities, and solid acid catalyst poisoning in a subsequent alkylation reaction can be avoided. The method improve the catalytic activity and usage cycle of the alkylation solid acid, greatly reduces production costs and improves production efficiency.
Description
Technical field
The present invention relates to a kind of process for purification of raw material for alkylation. Be particularly related to a kind of fourth two that removes from raw material for alkylationThe process for purification of one or more in alkene, sulfur-containing compound, oxygenatedchemicals, nitrogen-containing compound and chlorine-containing compound,Belong to petrochemical industry.
Background technology
Alkylation refer to by alkane (being generally isoparaffin) under strong acid exists with the reacting of alkene, for example produceThe alkane higher and that seethe with excitement in the scope of gasoline than raw material octane number. In petroleum refining, alkylated reactionGenerally C3To C5Alkene reacts with iso-butane.
In alkylation process, conventionally adopting hydrofluoric acid or sulfuric acid is catalyst. But sulfuric acid and hydrofluoric acid have environmentSerious pollution and harm, and high especially to the requirement of equipment. At present, adopt solid acid catalyst to replace liquid acidCatalytic alkylation reaction can be avoided equipment corrosion, is conducive to environmental protection simultaneously, has become the development of alkylation processDirection.
For example, CN102191081 discloses a kind of alkylation, and described method comprises and will contain C4-C6 isomeryAfter alkane mixes with circulation isoparaffin with the reaction raw material of C3-C6 singly-bound alkene, in alkylated reaction systemIn contact with solid acid catalyst and alkylated reaction occur. Reaction effluent, after supercooling and separating, obtains alkylCarburetion product.
As another embodiment, CN103421532A discloses a kind of alkylation, and described method comprises isomeryAlkane, if isobutane feed is to alkylation reactor, alkylated reaction adopts containing 50%H3PW12O14With 50% oxidationThe loaded catalyst of alumina supporter, is then separated into alkylate gasoline-range component and heavier alkylation is producedThing. Another example of prior art alkylation is disclosed in CN104857984.
Raw material for alkylation, such as oil plant catalytic pyrolysis (FCC) C4Cut can comprise many components, comprise normal butane,Iso-butane, n-butene. Unwanted component in raw material for alkylation can comprise oxygenatedchemicals (for example water and oxidationHydrocarbon, for example ether and alcohol), diene (for example butadiene), nitrogen-containing compound (for example nitrile and amine), sulfur-containing compound (exampleAs methyl mercaptan and ethyl mercaptan) and chlorine-containing compound (for example monochloro methane and monochlorethane). These do not need compoundExistence can cause the inactivation of solid acid catalyst.
Carrying out in alkylated reaction, the impurity in raw material for alkylation can cause alkylation catalyst poisoning at short noticeInactivation, and strengthened production cost, reduce production efficiency. Therefore, urgently seek a kind of refining alkyl raw materialMethod is carried out the impurity in deep purifying raw material for alkylation.
Summary of the invention
In order to solve the problems of the technologies described above, improve activity and the service life of solid catalyst in alkylated reaction, reduceCatalysqt deactivation, the object of the present invention is to provide a kind of carbon four that is directed to after oil plant ether as the essence of raw material for alkylationMethod processed.
Object of the present invention is realized by following technical scheme:
A process for purification for raw material for alkylation, comprises the steps:
(1) raw material for alkylation is sent into water scrubber, take off the processing of oxygenatedchemicals and/or nitrogen-containing compound, logicalCross this step process, can remove most of oxygenatedchemicals and/or most of nitrogen-containing compound;
(2) contact with dehydration molecular sieve sending into dehydrating tower by water scrubber material out, carry out processed;
(3) contact with sulfide removal adsorbent sending into desulfurizing tower by dehydrating tower material out, carry out sulfide removalProcessing;
(4) contact with dechloratation adsorbent sending into dechlorinator by desulfurizing tower material out, carry out dechloratationProcessing;
(5) contact with denitrogenation compound adsorbent sent into denitrification column by dechlorinator's material out, further take offExcept the processing of nitrogen-containing compound;
(6) contact with de-oxygenatedchemicals adsorbent sent into de-oxygenatedchemicals tower by denitrification column material out,Further remove the processing of oxygenatedchemicals;
(7) after allocating hydrogen into by de-oxygenatedchemicals tower material out, carry out preheating by preheater in the lump, soAfter send into and in selective hydrogenation reaction device, carry out alkadienes selective hydrogenation, the material flowing out through selective hydrogenation reaction deviceBe refining raw material for alkylation. In carrying out alkylate oil production, by its refining raw material for alkylation with reactThe remaining material of device is sent in the lump and in alkylation equipment, carries out alkylated reaction and generate alkylate oil.
In said method, described raw material for alkylation comprises positive alkene, normal butane, iso-butane and impurity, described impurity bagDraw together one or more the group in butadiene, sulfur-containing compound, oxygenatedchemicals, nitrogen-containing compound and chlorine-containing compoundClose.
In said method, preferably, dehydration molecular sieve described in step (2) can be 4A molecular sieve, more preferablyFor UOP4A molecular sieve.
In said method, preferably, sulfide removal adsorbent described in step (3) can be a kind of negative through copper metalThe NaY type molecular sieve carrying, is more preferably SQ108 adsorbent, and this adsorbent is that the special new material of Dongying Cole is limitedCompany produces.
In said method, preferably, dechloratation adsorbent described in step (4) can be that one changes through sodium carbonateProperty X-type molecular sieve, be more preferably QTL-05 adsorbent, this adsorbent is the limited public affairs of the special new material of Dongying ColeDepartment produces.
In said method, preferably, denitrogenation compound adsorbent described in step (5) can be a kind of through NaOHThe X-type molecular sieve of modification, is more preferably SQ103 adsorbent, and this adsorbent is that the special new material of Dongying Cole is limitedCompany produces.
In said method, preferably, de-oxygenatedchemicals adsorbent described in step (6) can be a kind of through alkaline earthThe X-type molecular sieve of magnesium metal load, is more preferably SQ112 adsorbent, and this adsorbent is the special green wood of Dongying ColeMaterial Co., Ltd produces.
In said method, preferably, the catalyst adopting in alkadienes selective hydrogenation process in step (7)Taking activated alumina as carrier, the catalyst taking palladium, silver as main active component, wherein, the mass percent of palladiumBe 0.4%, the mass percent of silver is 0.1%. The C4 choosing that can adopt Zibo Lv Xing Chemical Industry Science Co., Ltd to produceUrging of the well-known to those skilled in the art or disclosed patent literature of selecting property hydrogenation and removing alkadienes catalystAgent.
In said method, preferably, in described desulfurizing tower, the running temperature of reaction process is 20-50 DEG C, and pressure is0.6-2MPa, volume liquid air speed is 0.25-4h-1。
In said method, preferably, in described dechlorinator, the running temperature of reaction process is 20-50 DEG C, and pressure is0.6-2MPa, volume liquid air speed is 0.25-5h-1。
In said method, preferably, in described denitrification column, the running temperature of reaction process is 20-50 DEG C, and pressure is0.6-2MPa, volume liquid air speed is 0.25-5h-1。
In said method, preferably, in described de-oxygenatedchemicals tower, the running temperature of reaction process is 20-50 DEG C,Pressure is 0.6-2MPa, and volume liquid air speed is 0.25-5h-1。
In said method, preferably, in described selective hydrogenation tower, the running temperature of reaction process is 50-90 DEG C, pressesPower is 0.8-2MPa, and volume liquid air speed is 3-5h-1；
More preferably, in course of reaction, the volume ratio of hydrogen and alkadienes is 1-5:1.
In the present invention, if do not particularly not pointed out, the degree of catalyst is by weight, specific impuritiesContent ppm also by weight.
The content of the method for the invention trace impurity before and after raw material for alkylation is refining is as follows:
Before refining, after oil plant ether, the trace impurity of carbon tetraalkyl raw material consists of:
Mercaptan: 1-10ppm, dimethyl disulfide: 1-50ppm, total sulfur: 2-100ppm, dimethyl ether: 10-400ppm,Methyl alcohol: 5-200ppm, methyl tertiary butyl ether(MTBE) (MTBE): 1-50ppm, chlorine: 1-10ppm, methane acetonitrile: 1-30ppm,Alkadienes: 0.1-0.22wt% etc.
After refining, after oil plant ether, the trace impurity of carbon tetraalkyl raw material consists of:
Mercaptan: < 0.1ppm, dimethyl disulfide: < 0.5ppm, total sulfur: < 1ppm, dimethyl ether: < 50ppm,Methyl alcohol: < 5ppm, methyl tertiary butyl ether(MTBE) (MTBE): < 1ppm, chloromethanes: < 1ppm, acetonitrile: < 1ppm, twoAlkene < 100ppm etc.
Beneficial effect of the present invention:
Raw material for alkylation process for purification of the present invention can effectively remove sulfide, nitride, the chlorination in raw material for alkylationThe plurality of impurities such as thing, oxygenatedchemicals, obviously reduces the impurity content in raw material for alkylation, has avoided follow-up alkylIn change reaction, solid acid catalyst is poisoning, has improved alkylated solid surface acidity and life cycle, greatly reducesProduction cost, has improved production efficiency.
Brief description of the drawings
Fig. 1 is raw material for alkylation process for purification simplification of flowsheet figure.
Reference numeral explanation:
The de-oxygenatedchemicals tower of 1 water scrubber 2 dehydrating tower 3 desulfurizing tower 4 dechlorinator's 5 denitrification column 6
7 preheater 8 selective hydrogenation reaction device 9 alkylation equipment
Detailed description of the invention
Understand for technical characterictic of the present invention, object and beneficial effect being had more clearly, existing to skill of the present inventionArt scheme is carried out following detailed description, but can not be interpreted as restriction that can practical range of the present invention.
Embodiment
The present embodiment provides a kind of process for purification of raw material for alkylation, its flow process as shown in Figure 1, the method comprise withLower step:
Carbon tetraalkyl raw material after ether is added from the entrance of water scrubber 1, and the pressure of porch is 1.3MPa, entranceTemperature is 40 DEG C, and raw material input flow is 20000kg/h, and wherein impurity composition content is respectively: alkadienes 0.21wt%,Dimethyl ether 304ppmw, methyl alcohol 36ppmw, mercaptan 4ppmw, dimethyl disulfide 17ppmw, total sulfur 26ppmw,Methyl tertiary butyl ether(MTBE) (MTBE) 9ppmw, acetonitrile 4ppmw, monochloro methane 3ppmw.
Send into by tower top in the dehydrating tower 2 that is filled with UOP4A molecular sieve through water scrubber 1 material out, de-The dried material of water is sent in desulfurizing tower 3 and is contacted with sulfide removal adsorbent SQ108 adsorbent, in desulfurizing tower 3Reaction temperature be 40 DEG C, pressure is 1.2MPa, volume liquid air speed is 1h-1; Through desulfurizing tower 3 material outSend in dechlorinator 4 and contact with denitrogenation compound adsorbent QTL-05 adsorbent, the reaction temperature in dechlorinator 4 is 40DEG C, pressure is 1.15MPa, volume liquid air speed is 2h-1; Send in denitrification column 5 through dechlorinator 4 material outContact with denitrogenation compound adsorbent SQ103 adsorbent, the reaction temperature in denitrification column 5 is 40 DEG C, and pressure is1.1MPa, volume liquid air speed is 2h-1; Send into de-oxygenatedchemicals tower 6 and the de-oxygen that contains through denitrification column material outThe contact of compound adsorbent SQ112 adsorbent, the reaction temperature in de-oxygenatedchemicals tower 6 is 40 DEG C, pressure is1.05MPa, volume liquid air speed is 2h-1; It is logical in the lump after de-oxygenatedchemicals tower 6 material is out allocated hydrogen intoCross preheater 7 and heat, then send in selective hydrogenation reaction device 8 and carry out alkadienes selective hydrogenation, wherein,Reaction temperature is 73 DEG C, and pressure is 1.8MPa, and volume liquid air speed is 4h-1, catalyst selects C4 selective hydrogenation de-Except alkadienes catalyst, the volume ratio of hydrogen and alkadienes is 1, reacts saturated alkadienes, through selective hydrogenation reaction device8 materials that flow out are refining raw material for alkylation.
In carrying out alkylate oil production, by above-mentioned refining raw material for alkylation and the remaining material of reactor in the lumpBe sent to and in alkylation equipment 9, carry out alkylated reaction and generate alkylate oil.
In raw material for alkylation after above-mentioned refining, impurity content is respectively: alkadienes is 100ppmw, dimethyl ether1ppmw, methyl alcohol 1ppmw, mercaptan 0.1ppmw, dimethyl disulfide: 0.8ppmw, total sulfur: 0.9ppmw,Methyl tertiary butyl ether(MTBE) (MTBE): 1ppmw, acetonitrile 0.4ppmw, monochloro methane: 0.3ppmw.
From above-described embodiment, the content of refining rear various impurity obviously reduces, and impurity content is reduced to trace, canTo extend the life-span of subsequent alkylation reacting middle catalyst, avoid subsequent alkylation reacting middle catalyst poisoning, improveAlkylated solid surface acidity and life cycle, reduced greatly production cost, improved production efficiency.
Claims (10)
1. a process for purification for raw material for alkylation, is characterized in that, comprises the steps:
(1) raw material for alkylation is sent into water scrubber, take off the processing of oxygenatedchemicals and/or nitrogen-containing compound;
(2) contact with dehydration molecular sieve sending into dehydrating tower by water scrubber material out, carry out processed;
(3) contact with sulfide removal adsorbent sending into desulfurizing tower by dehydrating tower material out, carry out sulfide removalProcessing;
(4) contact with dechloratation adsorbent sending into dechlorinator by desulfurizing tower material out, carry out dechloratationProcessing;
(5) contact with denitrogenation compound adsorbent sent into denitrification column by dechlorinator's material out, further take offExcept the processing of nitrogen-containing compound;
(6) contact with de-oxygenatedchemicals adsorbent sent into de-oxygenatedchemicals tower by denitrification column material out,Further remove the processing of oxygenatedchemicals;
(7) after allocating hydrogen into by de-oxygenatedchemicals tower material out, carry out preheating by preheater in the lump, soAfter send into and in selective hydrogenation reaction device, carry out alkadienes selective hydrogenation, the material flowing out through selective hydrogenation reaction deviceBe refining raw material for alkylation.
2. method according to claim 1, is characterized in that: described in step (2), dehydration molecular sieve is4A molecular sieve, is preferably UOP4A molecular sieve.
3. method according to claim 1, is characterized in that: sulfide removal adsorbent described in step (3)Be a kind of through the NaY of copper Metal Supported type molecular sieve, be preferably SQ108 adsorbent.
4. method according to claim 1, is characterized in that: dechloratation adsorbent described in step (4)Be a kind of X-type molecular sieve through modification of sodium carbonate, be preferably QTL-05 adsorbent.
5. method according to claim 1, is characterized in that: denitrogenation compound adsorbent described in step (5)Be a kind of X-type molecular sieve through NaOH modification, be preferably SQ103 adsorbent.
6. method according to claim 1, is characterized in that: described in step (6), de-oxygenatedchemicals is inhaledAttached dose is a kind of through the magnesium-supported X-type molecular sieve of alkaline-earth metal, is preferably SQ112 adsorbent.
7. method according to claim 1, is characterized in that: in step (7), alkadienes selective hydrogenation is anti-Answering the catalyst adopting in process is taking activated alumina as carrier, the catalyst taking palladium, silver as main active component,Wherein, the mass percent of palladium is 0.4%, and the mass percent of silver is 0.1%.
8. method according to claim 1, is characterized in that: the operation temperature of reaction process in described desulfurizing towerDegree is 20-50 DEG C, and pressure is 0.6-2MPa, and volume liquid air speed is 0.25-4h-1。
9. method according to claim 1, is characterized in that: described dechlorinator, denitrification column, de-containing oxidationIn compound tower, the running temperature of reaction process is 20-50 DEG C, and pressure is 0.6-2MPa, and volume liquid air speed is0.25-5h-1。
10. according to the method described in claim 1 or 7, it is characterized in that: in described selective hydrogenation tower, react workThe running temperature of skill is 50-90 DEG C, and pressure is 0.8-2MPa, and volume liquid air speed is 3-5h-1；
Preferably, in alkadienes selective hydrogenation process, the volume ratio of hydrogen and alkadienes is 1-5:1.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106279539A (en) * | 2016-06-03 | 2017-01-04 | 中国石油化工股份有限公司 | Hydrogenation of petroleum resin process desulfurization, the commercial run of dechlorination |
| CN108410501A (en) * | 2018-04-11 | 2018-08-17 | 宁波章甫能源科技有限公司 | A kind of light dydrocarbon fine de-sulfur device and the sulfur method based on the device |
| CN108636348A (en) * | 2018-04-25 | 2018-10-12 | 中国石油大学(北京) | The method for loading adsorbent of basic active component and preparation method thereof and depth dechlorination |
| CN110407660A (en) * | 2018-04-28 | 2019-11-05 | 东营市海科瑞林化工有限公司 | A kind of pretreating process and pretreatment system of the material carbon four for solid acid alkylation processes |
| CN112143518A (en) * | 2019-06-27 | 2020-12-29 | 中国石油化工股份有限公司 | Solid acid alkylation method for producing gasoline |
| CN112143523A (en) * | 2019-06-27 | 2020-12-29 | 中国石油化工股份有限公司 | Pretreatment method of alkylated gasoline raw material |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106279539A (en) * | 2016-06-03 | 2017-01-04 | 中国石油化工股份有限公司 | Hydrogenation of petroleum resin process desulfurization, the commercial run of dechlorination |
| CN108410501A (en) * | 2018-04-11 | 2018-08-17 | 宁波章甫能源科技有限公司 | A kind of light dydrocarbon fine de-sulfur device and the sulfur method based on the device |
| CN108636348A (en) * | 2018-04-25 | 2018-10-12 | 中国石油大学(北京) | The method for loading adsorbent of basic active component and preparation method thereof and depth dechlorination |
| CN110407660A (en) * | 2018-04-28 | 2019-11-05 | 东营市海科瑞林化工有限公司 | A kind of pretreating process and pretreatment system of the material carbon four for solid acid alkylation processes |
| CN110407660B (en) * | 2018-04-28 | 2022-06-14 | 东营市海科瑞林化工有限公司 | Pretreatment process and pretreatment system for raw material C4 for solid acid alkylation process |
| CN112143518A (en) * | 2019-06-27 | 2020-12-29 | 中国石油化工股份有限公司 | Solid acid alkylation method for producing gasoline |
| CN112143523A (en) * | 2019-06-27 | 2020-12-29 | 中国石油化工股份有限公司 | Pretreatment method of alkylated gasoline raw material |
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