CN102633585A - Method for preparing high-purity propane, iso-butane and n-butane - Google Patents
Method for preparing high-purity propane, iso-butane and n-butane Download PDFInfo
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Abstract
The invention discloses a method for preparing high-purity propane, iso-butane and n-butane. The method for preparing high-purity iso-butane and n-butane comprises the following steps of: hydrogenating mixed carbon 4 subjected to propylene extraction, etherification and aromatization, and separating the product, wherein olefins are respectively less than 0.5 percent, and the hydrogenating catalyst is a special catalyst comprising a common non-noble metal main catalyst and a noble metal cocatalyst. By adopting a process of hydrogenation and rectification in the method, the obtained alkane components have high purity; and compared with simple thermal processing, the method has the advantages that the method saves a large quantity of investment and is low in operation cost, high in flexibility, flexible and convenient and the products completely meet downstream chemical processes and have remarkable economic benefits.
Description
Technical field
The present invention relates to a kind of comprehensive degree of depth and utilize carbon 4 technology, to be raw material, the alkene in the tail gas is saturated through deep hydrogenation through the tail gas after the processing of unit such as propylene extracting, etherificate, aromizing; Obtain propane, Trimethylmethane and three kinds of paraffins mixtures of normal butane; Further this mixture is carried out high efficiency separation, obtain highly purified alkane monomer, monomer character satisfies industrial chemicals or pressurized gas specification requirement; Be the combination technique that a kind of high efficiency of energy is utilized, remarkable in economical benefits.
Background technology
Carbon 4 refers generally to a large amount of C of by-product in refining of petroleum and the petrochemical production process
4Hydrocarbon comprises normal butane, Trimethylmethane, n-butene, iso-butylene and divinyl etc.Before the eighties in 20th century, refining of petroleum is particularly from the C of CCU
4Cut is mainly as worker's domestic fuel; The C that steam cracking obtains
4Cut is also done fuel more except that divinyl is made synthetic rubber raw materials.Since the nineties in 20th century, since the progress of stripping technique, C
4Cut has obtained develop rapidly as the application of petrochemical materials.It is predicted C
4Cut is the petrochemical materials that after ethene and propylene, possibly be fully used.
The mixing carbon 4 of the common indication in market comprises from catalytic unit, cracking of ethylene unit; Even comprise the mixed gas of coking and normal decompressing unit; It is very many to mix carbon 4 components; Comprise ethene, propylene, propane, normal butane, Trimethylmethane, iso-butylene, n-butene and a spot of carbon 5 components, propylene component wherein is by extracting to greatest extent.
Along with development, the especially progress of fluid catalytic cracking of heavy oil device and ethylene cracker with the device level of the scale of China's petrochemical industry, the output of mixing carbon 4 presents output and increases the general trend that matter is fallen.Rough production and use-pattern that carbon 4 is directly acted as a fuel can not adapt to the needs that Chinese society develops.Mix carbon 4 through can be used as valuable industrial chemicals after the deep processing, also can be used as automobile-used cleaning liquor gasification.And China's motor liquified gas mainly depends on import with carbon 4 raw materials that are used for deep processing at present.The present situation in carbon 4 fields of China is: a large amount of on the one hand fossil resources are spent a large amount of foreign exchanges on the one hand and buy raw material by low value consumption, the motor liquified gas dependence on import that China is over half, and the iso-butylene import volume reaches more than 80% of domestic needs.The main root of this contradiction is that China's petrochemical industry deep processing level is lower, core technology lacking of market competition ability such as catalyzer.
At present, the existing course of processing of mixing carbon 4 mainly contains dual mode: extracting propylene → etherificate → aromizing and extracting propylene → etherificate → alkylation.Adopt liquid acid all to eliminate as the alkylation route of catalyzer abroad, China minority enterprise is still in operation; Aromatization process is commonplace, has domesticly developed into nearly 50 covering devices.The subject matter of this dual mode is that product circuit is comprehensive inadequately, and the usability again of tail gas is not strong, and resource is not efficiently utilized, and the production process energy consumption is high, pollution is big.The tail gas of these two kinds of modes of production all is used as the cleaning civil liquefied gas and sells.Civil liquefied gas burns under normal pressure, and the alkene in the tail gas can not all utilize, and must have part to discharge into the atmosphere, and causes environmental pollution.If the impurity alkene in the tail gas is changed, be processed as motor liquified gas, on the one hand because the motor liquified gas low sulfur, low olefin is a kind of cleaning green fuel; The value of motor liquified gas is higher than civil liquefied gas on the other hand, the economy return that manufacturing enterprise will obtain.
No matter be to produce motor liquified gas, high-purity monomers such as Trimethylmethane and normal butane still are provided downstream, principal contradiction concentrates on impurity component alkene.At present, domestic most employing thermal processing method separates carbon 4 components, because it is more concentrated relatively to mix the boiling point of component in the carbon 4; Wherein, Trimethylmethane boiling point-11.8 ℃, normal butane boiling point-0.522 ℃, 1,3 divinyl boiling point-4.5 ℃, iso-butylene boiling point-6.9 ℃, n-butene boiling point-6.26 ℃; The separation accuracy of simple rectifying is not high; The complex equipments investment is higher, and it is limited that single covering device is handled load, fluctuation of service.
Separate to the processing that mixes carbon 4 both at home and abroad and developed a lot of Technologies.
CN101955405A discloses the purify technology of preparation normal butane of a kind of method that adopts rectifying, and equipment comprises that left reflux pump, left return tank, left condenser, feedstock pump, debutanizing tower, butane reboiler, intermediate reflux pump, intermediate reflux jar, intermediate condenser, left deisobutanizer, recycle pump, right deisobutanizer, Trimethylmethane reboiler, normal butane tower, right condenser, right return tank, right reflux pump, normal butane reboiler constitute through the connection line one that is linked in sequence.
CN101657396 discloses the method that 1-butylene is produced in a kind of absorption, absorption and distillation; Device comprises: an adsorption device that is made up of adsorption tower and two distillation towers (distillation tower is used to separate alkene/desorbent, and another distillation tower is used for separation of alkane/desorbent) of three sorbent materials that selective adsorption alkene is housed; And distillation tower, be used for the C for preparing from an adsorption device through distillation
4Alkene obtains 1-butylene.
CN101880549A discloses a kind of method of hydrotreating of liquefied gas fraction; This method is carried out hydrogenation to the liquefied gas raw material of olefin(e) centent 10-80%; Hydrogenation products can be directly as the raw material of ethylene cracker; Also can fractionation be cut into propane, normal butane and Trimethylmethane etc.,, increase the economic benefit of oil refining enterprise as the Elementary Chemical Industry raw material of high added value.The raw material olefin content that this method is selected is higher, and the hydrogenation process hydrogen-consuming volume is bigger.
CN101475429 discloses a kind of method that fully utilizes cracking c_4, through adopting combination techniques such as selecting hydrogenation, full hydrogenation, etherificate, rectifying, extracting, each component in the cracking c_4 is made full use of.
CN1116126 discloses a kind of novel process of producing high purity butene-1 by carbon four, and this method adopts the method acquisition of extracting rectifying and selective hydrogenation to need product.
CN1508103 discloses a kind of method and catalyzer thereof of hydrocarbon raw material hydrogenation preparing alkane and has formed and the preparation method.This method selects for use noble metal catalyst to C
4, C
5Behind the fraction hydrogenating, the total olefin content in the product is less than 1%, and total alkane content can satisfy the requirement of cracking stock and motor liquified gas greater than 99%.
The purpose of above technology and invention all is that the degree of depth is utilized the various valuable component in carbon four resources, and method is intended to overcome the approaching problem of mixing carbon 4 each component boiling points.
Summary of the invention
The present invention is that a kind of comprehensive degree of depth is utilized carbon four technology; Mixed c 4 from devices such as cracking of ethylene, catalytic cracking, delayed cokings; Through the residue mixed c 4 after propylene extracting, etherificate, the aromizing course of processing; Still the alkene that contains few part, utilizability are not strong, generally use as the direct labor domestic fuel gas.
The present invention adopts the technology of deep hydrogenation saturation of olefins on the basis after propylene extracting, etherificate, the aromizing course of processing, and hydrogenation products is separated acquisition propane, Trimethylmethane and normal butane monomer.
Propylene extracting, etherificate, three kinds of courses of processing of aromizing have obtained sufficient industriallization.
Hydrogenation process of the present invention adopts two kinds of catalyzer, is respectively main hydrogenating catalyst and auxilliary hydrogenation catalyst, and main hydrogenating catalyst fills in the auxilliary hydrogenation catalyst upper reaches, adopts inert support to separate in the middle of two kinds of catalyzer.
The main hydrogenating catalyst carrier is the γ phase alumina; The raw material of preparation carrier is a water pseudo-boehmite; The carrier auxiliary agent is selected from least 5 kinds in Cu, Zn, Zr, K, F, P and the B element, and reactive metal is selected from 2 kinds in Pt, Pd, Mo, Co, the Ni element, and the specific surface area of catalyzer is 220-280m
2/ g, pore volume is 0.25-0.35mL/g, and mean pore size is distributed as 20-40nm, and crush strength is 180-350N/cm
2, this catalyzer accounts for the 75-90% of all loading catalyst total masses.
Auxilliary hydrogenation catalyst adopts anatase titanium dioxide TiO
2Be carrier, the carrier auxiliary agent is selected from least 5 kinds in Zr, P, K, La, Ce, Ag, Au, the Mn element, and reactive metal is selected from 2 kinds in Pt, Pd, Mo, the Co element, and the specific surface area of catalyzer is 150-250m
2/ g, pore volume is 0.30-0.45mL/g, and mean pore size is distributed as 15-35nm, and crush strength is 140-250N/cm
2, this catalyzer accounts for the 10-25% of all loading catalyst total masses.
Principle process of the present invention is: raw material, new hydrogen → unifining → degassing tower → depropanizing tower → Trimethylmethane and normal butane rectifying tower.
Hydrogenation process of the present invention is common processes, has no special requirements, and mainly comprises flow processs such as heat exchange, hydrogenation reaction, gas-liquid separation, recycle hydrogen.
The present invention mainly refers to the hydrogenation catalyst of hydrogenation process; This catalyzer has the saturated and hydrogenating desulfurization function of alkene simultaneously, through regulating the operating procedure parameter, changes the hydrogenation degree of depth; Obtain the hydrogenation products of different alkene and total sulfur content; After the hydroprocessing technique section, the total olefin mass content can satisfy the index less than 0.1% in the hydrogenation elute, and total sulfur content is smaller or equal to 10 μ g/g in the hydrogenation elute.
Hydrogenation process operating procedure parameter: volume space velocity 2.0-8.0h
-1, temperature 180-360 ℃, hydrogen-oil ratio 100-600v/v, carry out cold high score flow process, hydrogen recycle is used.
Successively through getting into degassing tower behind HP separator and the light pressure separator, degassing tower top tail gas is as process furnace fuel or get into the exhaust emissions system from the hydrogenator elute; The staple of top tail gas is carbon 1, carbon 2, hydrogen and a spot of hydrogen sulfide.
Component gets into separation column at the bottom of the degassing Tata, and it is propane that cat head outflow owner wants component, and bottom stream is Trimethylmethane and normal butane; Cat head elute propane can be used as product and gets into the product tank field, and bottom stream Trimethylmethane and normal butane get into rectifying tower, and Trimethylmethane is separated with normal butane; The cat head elute is a Trimethylmethane, is normal butane at the bottom of the tower, and wherein the Trimethylmethane mass content is not less than 99.0%; Total olefin content is not more than 0.5%, and the normal butane mass content is not less than 98.0%, and total olefin content is not more than 0.3%; Monomer component total sulfur content is not more than 5 μ g/g respectively, gets into the tank field respectively as product.
Characteristics such as the present invention has the simple easy handling of flow process, technology is flexible, process cost is little, adaptability to raw material is strong, product technology content is high, steady quality and amount of finish are big are embodied in:
1. utilize the prior art means, and technology is extended, raw material is easy to get, and adaptability to raw material is strong.
2. olefin(e) centent hydrogenation technique engineering can satisfy the raw material of olefin(e) centent 2-30wt% in the hydrogenating materials, and alkene is formed does not have special demands, and invention has the strong characteristics of adaptability to raw material.
3. hydrotreating catalyst can be concentrated the same reactor drum of filling; Also can load the differential responses device respectively; Through the residual content that processing parameters such as red-tape operati temperature, working pressure and amount of finish are regulated alkene in the product, obtain the product of different size, have the technology flexible characteristic.
4. difference in functionality catalyzer can drop to side reactions such as catalyzer coking and methanation minimumly, and Primary Catalysts is taken into account and can be satisfied degree of depth saturation of olefins and deep desulfuration.
5. the hydrogenation after product is simple propane, Trimethylmethane and three kinds of alkane of normal butane, because enough big of three kinds of monomeric boiling-point differences can obtain highly purified detailed hydrocarbon through simple hot-work.
Advantage of the present invention demonstrates fully among the embodiment with concrete effect below.
Embodiment
Below in conjunction with the concrete elaboration of embodiment embodiment of the present invention
1, starting material are prepared
1. pass through residue mixed c 4 after propylene extracting, etherificate, the aromizing course of processing as the hydrogenation charging, certain aromizing tail gas is formed and is seen table 1, and wherein the total olefin mass content 6.255%, total alkane mass content 93.275%, carbon five mass content 0.415%;
Table 1
2. hydrogen, steel cylinder hydrogen, purity ≮ 99.0wt%
3. hydrogenation unit and flow process
4. hydroprocessing condition: hydrogenation catalyst total filling amount 2.0L, assistant agent 0.25L wherein, host 1.75L is in host volume space velocity 8.0h
-1, 185 ℃ of catalyst inlet temperature, hydrogen-oil ratio 500v/v, inlet pressure 1.6MPa
5. move 1500h result continuously
(1) table 2 is seen in the processing condition variation
(2) the product composition is seen table 3 with yield
Table 2
Table 3
Claims (4)
1. the preparation method of high purity Trimethylmethane and normal butane is characterized in that: the preparation raw material sources are in mixing carbon 4 through the residue of etherificate and aromizing, with this part raw material through the alkane product of hydrotreatment acquisition olefin(e) centent less than certain specification; Further this product is separated, obtain high-purity propane, Trimethylmethane and normal butane, wherein, the mass content of propane is greater than 99.0%, and the mass content of Trimethylmethane is greater than 99.0%, and the mass content of normal butane is greater than 98%.
2. according to claims 1 described method; It is characterized in that: the mixing carbon 4 that is used for etherificate and aromizing derives from the petrochemical industry courses of processing such as FCC, thermally splitting system ethene, delayed coking, mixes propylene in the carbon 4 and carries out etherification reaction and aromatization again after by extracting; Etherification reaction is meant that the iso-butylene in the mixed gas reacts acquisition MTBE (MTBE) with methyl alcohol under an acidic catalyst effect, and used an acidic catalyst is meant strongly-acid macropore cation resin class catalyzer; Aromatization is meant that alkene is converted into aromatic hydroxy compound under the modified molecular sieve catalyst effect, and modified molecular sieve catalyst is meant modified ZSM-5 5 or beta-molecular sieve.
3. according to claims 1 described method, it is characterized in that:
1. fixed-bed process is adopted in hydrotreatment, and two kinds of hydrotreating catalysts of filling are respectively main hydrogenating catalyst and auxilliary hydrogenation catalyst in the reactor drum, and main hydrogenating catalyst fills in the auxilliary hydrogenation catalyst upper reaches, adopts inert support to separate in the middle of two catalyzer.
2. main hydrogenating catalyst adopts gama-alumina to prepare carrier, and the carrier auxiliary agent is selected from least 5 kinds in Cu, Zn, Zr, K, F, P and the B element, and reactive metal is selected from 2 kinds in Pt, Pd, Mo, Co, the Ni element, and the specific surface area of catalyzer is 220-280m
2/ g, pore volume is 0.25-0.35mL/g, and mean pore size is distributed as 20-40nm, and crush strength is 180-350N/cm
2, this catalyzer accounts for the 75-90% of all loading catalyst total masses.
3. auxilliary hydrogenation catalyst adopts anatase titanium dioxide T
iO
2Be carrier, the carrier auxiliary agent is selected from least 5 kinds in Zr, P, K, La, Ce, Pd, Ag, Au, the Mn element, and reactive metal is selected from 2 kinds in Pt, Pd, Mo, the Co element, and the specific surface area of catalyzer is 150-250m
2/ g, pore volume is 0.30-0.45mL/g, and mean pore size is distributed as 15-35nm, and crush strength is 140-250N/cm
2, this catalyzer accounts for the 10-25% of all loading catalyst total masses.
4. hydrotreatment process operation processing parameter is interval, volume space velocity 2.0-8.0v/v, temperature 180-360 ℃, hydrogen-oil ratio 100-600h
-1, carry out cold high score flow process, hydrogen recycle is used.
5. after passing through the hydroprocessing technique section, the total olefin mass content is smaller or equal to 0.5% in the product, and total sulfur content can obtain the hydrogenation products of different alkene and total sulfur content through regulating the hydrogenation degree of depth smaller or equal to 10 μ g/g in the product.
4. according to claim 2, it is characterized in that:
1. the elute at the bottom of the hydrogenator tower, through getting into separation column behind the high-low pressure separator, fractionation cat head elute is a propane, bottom stream is Trimethylmethane and normal butane.
2. the elute at the bottom of the separation column gets into rectifying tower, and rectifying tower is common float valve tray column, and Trimethylmethane is separated with normal butane; The cat head elute is a Trimethylmethane; Be normal butane at the bottom of the tower, wherein the Trimethylmethane mass content is not less than 99.0%, and olefin(e) centent is not more than 0.5%; The normal butane mass content is not less than 98.0%, and olefin(e) centent is not more than 0.3%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104892339A (en) * | 2015-06-05 | 2015-09-09 | 常州瑞华化工工程技术有限公司 | Method for preparing n-butane by using iso-butane |
| CN105481627A (en) * | 2015-11-23 | 2016-04-13 | 山东粤安化工有限公司 | Production method of high-purity propane used as environment-friendly refrigerant R290 |
| CN106669798A (en) * | 2015-11-09 | 2017-05-17 | 中国石油化工股份有限公司 | Non-hydrogen modified catalyst and preparation method and application thereof |
| CN109952151A (en) * | 2016-11-17 | 2019-06-28 | 利安德巴塞尔乙酰有限责任公司 | For being used to generate the crushing strength and porosity of the alumina support of the catalyst of the enhancing of vinyl acetate monomer |
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| CN109952151B (en) * | 2016-11-17 | 2022-06-03 | 利安德巴塞尔乙酰有限责任公司 | Crush strength and porosity of alumina supports for enhanced catalysts used to produce vinyl acetate monomer |
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Application publication date: 20120815 |