CN101671221B - Preparation method of polymer solvent iso-butane - Google Patents
Preparation method of polymer solvent iso-butane Download PDFInfo
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- CN101671221B CN101671221B CN2009101925831A CN200910192583A CN101671221B CN 101671221 B CN101671221 B CN 101671221B CN 2009101925831 A CN2009101925831 A CN 2009101925831A CN 200910192583 A CN200910192583 A CN 200910192583A CN 101671221 B CN101671221 B CN 101671221B
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Abstract
The invention relates to a preparation method of polymer solvent iso-butane, comprising the following preparing steps: (1) hydrocracking liquefied petroleum gas and hydrogen are mixed according to 1:80-100 of volume ratio, and then are pre-heated to 220-280 DEG C; (2) the mixture is fed in a hydrogenation reactor, hydro-treatment is carried out under the condition that a hydrogenation catalyst exists, and the control conditions of the hydro-treatment are that: the reaction temperature is 200-250 DEG C, the reaction pressure is 2.0-2.8 MPa and reaction air speed is 1-2h<-1>; (3) the mixture is fed in a desulphurization reactor, desulfurization is carried out under the condition that the desulfurater exists, and the control conditions of the desulfurization are that: the reaction time is 200-400 DEG C, the reaction pressure is 2.0-2.8MPa and the reaction air speed is 0.4-1h<-1>; (4) the product obtained in the step 3 carries out gas-liquid separation, the separated butane gas carries out C3 and C4 constituent separation, and then iso-butane is separated out from the C4 constituent, and the separated iso-butane is dehydrated to obtain finished products. Compared with the traditional process, the invention can obtain iso-butane products with 99.5-99.9 percent of purity and causes content of total sulfur and total olefins of the iso-butane to meet requirements of polymer solvent.
Description
Technical field
The present invention relates to the Chemicals production technical field, particularly a kind of is the method that feedstock production high purity, sulfur-bearing are low, contain the low polymer solvent iso-butane of alkene with the hydrogen cracking LPG liquefied petroleum gas.
Background technology
Polymer solvent iso-butane is with in the oil hydrocracking process; The LPG liquefied petroleum gas fraction of by-product; Process through unifining, desulfurization and distillation technology; Have purity height, sulfur-bearing low, contain characteristics such as alkene is low, be mainly used in endless tube slurry method high density polyethylene(HDPE) and use as polymer solvent in producing, can be used for the replacement fluorine Leon again and make refrigeration agent.
At present, typical Trimethylmethane production technique mainly contains three kinds: its common ground is to be raw material with the hydrogen cracking LPG liquefied petroleum gas all, the one, and from LPG liquefied petroleum gas, adopt Y zeolite adsorbing and removing impurity to isolate the method for high-purity Trimethylmethane; The 2nd, produce Trimethylmethane through desulfurization and gas separation unit; The 3rd, alternating temperature absorption purification Trimethylmethane technology.Three kinds of production technique respectively have relative merits.Adopt Y zeolite absorbing process flow process simple, whole separating technology is normal-temperature operation, and is easy and simple to handle, and the process safety safety is high.Shortcoming product isobutane purity is not high.Adopting desulfurization and gas separation unit to produce the Trimethylmethane advantage is existing gas separation unit transformation capable of using, reduces investment outlay, and can't solve but shortcoming is the high problem of product olefin(e) centent.Alternating temperature absorption purifying technique advantage is that can to obtain purity be 99.5～99.9% Trimethylmethane product, but owing to lack desulfurization and deolefination technology, causes the total sulfur of Trimethylmethane and the requirement that total olefin content still can't satisfy the polymer solvent level.
In recent years, to the relative merits of above several kinds of production technique,, still there is not improvement at process aspect.
Summary of the invention
But the purpose of this invention is to provide a kind of high purity, sulfur-bearing low, contain the preparation method that the low and operational condition of alkene is easy to control the quantity-produced polymer solvent iso-butane.
The preparation method of polymer solvent iso-butane provided by the invention, its preparation process is:
(1) the hydrogen cracking LPG liquefied petroleum gas is mixed with hydrogen 1: 80 by volume～100, be preheated to 220～280 ℃ then;
(2) send into hydrogenator, under the condition that hydrogenation catalyst exists, carry out hydrotreatment, the control condition of hydrotreatment:
Temperature of reaction: 200～250 ℃, reaction pressure: 2.0～2.8MPa, reaction velocity: 1～2h-1;
(3) send into desulphurization reactor, under the condition that sweetening agent exists, carry out desulfurization and handle, the control condition that desulfurization is handled:
Temperature of reaction: 200～400 ℃, reaction pressure: 2.0～2.8MPa, reaction velocity: 0.4～1h
-1
(4) step (3) gained is carried out gas-liquid separation, isolated butagas carries out carbon three, carbon four components are separated, and again carbon four components is isolated Trimethylmethane, and isolated Trimethylmethane promptly gets after dehydration.
This hydrogenation catalyst is made up of the raw material of following parts by weight:
11～13 parts of molybdenum oxides
2～3 parts of powder blues
4～6 parts of nickel oxide
70～80 parts in aluminum oxide.
The hydrogenation catalyst loadings is 66～70% of a hydrogenator useful volume.
Described sweetening agent is a zinc oxide.
The sweetening agent loadings is 54～60% of a desulphurization reactor useful volume.
The present invention compares with traditional technology, both can obtain purity and be 99.5～99.9% Trimethylmethane product, makes the total sulfur of Trimethylmethane and the requirement that total olefin content satisfies the polymer solvent level again.Product is superior to the standard of similar imported product, and alternative imported product is saved user's production cost greatly, improves economic benefit of enterprises.
Embodiment
, advances the hydrogen of feedstock pump supercharging (more than the 2.0MPa) and recycle compressor outlet heater heats to 200 after mixing laggard interchanger heat exchange again ℃ with enterprising hydrogenator from the Trimethylmethane of cat head; Come out laggard desulphurization reactor desulfurization then through heat exchange, cooling, separation from hydrogenator; Trimethylmethane removes storage tank; Separate back hydrogen and remove the recycle compressor inlet, because of the hydrogen that consumes is replenished by new hydrogen.
Embodiment one:
The hydrogen cracking raw liquefied petroleum gas is formed (v%): ethane 1.13%, propane 14.2%, Trimethylmethane 47.44%, normal butane 33.36%, total butylene (ppm) 71.0, carbon more than five 3.87%, total sulfur (ppm) 5.27～6.32.
Its preparation process is:
(1) hydrogen cracking LPG liquefied petroleum gas and hydrogen were mixed in 1: 80 by volume, be preheated to 280 ℃ then;
(2) send into hydrogenator, hydrogenation catalyst is arranged in the hydrogenator, loadings is 68% of a hydrogenator useful volume; This hydrogenation catalyst is made up of following raw materials by weight percent: 11 parts of molybdenum oxides, 3 parts of powder blues, 4 parts of nickel oxide; 80 parts in aluminum oxide, the control condition of hydrotreatment:
Temperature of reaction: 220 ℃, reaction pressure: 2.4MPa, reaction velocity: 1.5h
-1
(3) send into desulphurization reactor, sweetening agent zinc oxide is arranged in the desulphurization reactor, the sweetening agent loadings is 57% of a desulphurization reactor useful volume, the control condition that desulfurization is handled:
Temperature of reaction: 300 ℃, reaction pressure: 2.4MPa, reaction velocity: 0.7h
-1
(4) with step (3) to carrying out gas-liquid separation, isolated butagas carries out carbon three, carbon four components are separated, and again carbon four components is isolated Trimethylmethane, isolated Trimethylmethane promptly gets after dehydration.
The result sees table one:
Table one hydrogenation catalyst, sweetening agent are with the change of temperature test result
| Temperature of reaction/℃ | 320 | 300 | 280 | 250 | 200 |
| Product property: | |||||
| Analytical procedure | Chromatogram quantification | Chromatogram quantification | Chromatogram quantification | Chromatogram quantification | Chromatogram quantification |
| Trimethylmethane/v% | 47.78 | 49.08 | 44.68 | 41.58 | 44.01 |
| Normal butane/v% | 33.64 | 31.86 | 40.37 | 38.86 | 40.10 |
| Total olefin/ppm (wt) | 42.1 | 20.4 | 13.6 | 7.6 | 4.6 |
| Olefin conversion/% | 40.7 | 71.3 | 80.8 | 89.3 | 93.5 |
| Wherein: propylene/ppm (wt) | 11.3 | 2.8 | 0.9 | 1.1 | 0.0 |
| 1-butylene/ppm (wt) | |||||
| Iso-butylene/ppm (wt) | 22.3 | 9.9 | 3.9 | 0.0 | 4.6 |
| Anteiso-butene-2/ppm (wt) | 6.8 | 2.9 | 1.0 | 0.0 | 0.0 |
| Along iso-butylene-2/ppm (wt) | 1.7 | 4.8 | 7.8 | 6.5 | 0.0 |
| 2,2-dimethylpropane/ppm (wt) | 194.4 | 153.3 | 281.6 | 285.7 | |
| Total sulfur ppm (wt) | 0.95 | 0.94 | 0.92 | 0.5 | 0.39 |
Visible from table one, reaction pressure 2.8MPa, volume space velocity 1.0h
-1, under the hydrogen liquor ratio 150v/v condition, add split liquefied gas fall the alkene effect preferably temperature of reaction be 200 ℃, olefin conversion is 93.5%.In addition, the sweetening agent test-results sees that product can reach the requirement of sulfur-bearing≤1ppm (wt).
Embodiment two:
The hydrogen cracking raw liquefied petroleum gas is formed (v%): ethane 0.91～2.09%, propane 14.33～18.92%, propylene (ppm) 45.6～65.9, Trimethylmethane 46.12～48.39%, normal butane 28.95～33.22%, positive iso-butylene (ppm) 132.1～166.5, anti-butene-2 (ppm) 37.6～58, maleic-223.21～33.9%, dimethylpropane (ppm) 0.03～224.3, carbon more than five 3.87～4.42%, total sulfur (ppm) 5.27～6.32.
Its preparation process is:
(1) hydrogen cracking LPG liquefied petroleum gas and hydrogen were mixed in 1: 100 by volume, be preheated to 220 ℃ then;
(2) send into hydrogenator, hydrogenation catalyst is arranged in the hydrogenator, loadings is 68% of a hydrogenator useful volume; This hydrogenation catalyst is made up of following raw materials by weight percent: 13 parts of molybdenum oxides, 2 parts of powder blues, 6 parts of nickel oxide; 70 parts in aluminum oxide, the control condition of hydrotreatment:
Temperature of reaction: 220 ℃, reaction pressure: 2.4MPa, reaction velocity: 1.5h
-1
(3) send into desulphurization reactor, sweetening agent zinc oxide is arranged in the desulphurization reactor, the sweetening agent loadings is 57% of a desulphurization reactor useful volume, the control condition that desulfurization is handled:
Temperature of reaction: 300 ℃, reaction pressure: 2.4MPa, reaction velocity: 0.7h
-1
(4) with step (3) to carrying out gas-liquid separation, isolated butagas carries out carbon three, carbon four components are separated, and again carbon four components is isolated Trimethylmethane, isolated Trimethylmethane promptly gets after dehydration.
The result sees table two, table three:
Table diisobutane product compositional analysis table
Table trimerization solvent iso-butane product quality indicator and assay
Claims (5)
1. the preparation method of a polymer solvent iso-butane is characterized in that its preparation process is:
(1) the hydrogen cracking LPG liquefied petroleum gas is mixed with hydrogen 1: 80 by volume～100, be preheated to 220～280 ℃ then;
(2) send into hydrogenator, under the condition that hydrogenation catalyst exists, carry out hydrotreatment, the control condition of hydrotreatment:
Temperature of reaction: 200～250 ℃, reaction pressure: 2.0～2.8MPa, reaction velocity: 1～2h
-1
(3) send into desulphurization reactor, under the condition that sweetening agent exists, carry out desulfurization and handle, the control condition that desulfurization is handled:
Temperature of reaction: 200～400 ℃, reaction pressure: 2.0～2.8MPa, reaction velocity: 0.4～1h
-1
(4) step (3) gained is carried out gas-liquid separation, isolated butagas carries out carbon three, carbon four components are separated, and again carbon four components is isolated Trimethylmethane, and isolated Trimethylmethane promptly gets after dehydration.
2. the preparation method of polymer solvent iso-butane according to claim 1 is characterized in that described hydrogenation catalyst is made up of the raw material of following weight part:
11～13 parts of molybdenum oxides
2～3 parts of powder blues
4～6 parts of nickel oxide
70～80 parts in aluminum oxide.
3. the preparation method of polymer solvent iso-butane according to claim 2 is characterized in that the hydrogenation catalyst loadings is 66～70% of a hydrogenator useful volume.
4. the preparation method of polymer solvent iso-butane according to claim 1 is characterized in that sweetening agent is a zinc oxide.
5. the preparation method of polymer solvent iso-butane according to claim 4 is characterized in that the sweetening agent loadings is 54～60% of a desulphurization reactor useful volume.
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| CN2009101925831A CN101671221B (en) | 2009-09-17 | 2009-09-17 | Preparation method of polymer solvent iso-butane |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102351627A (en) * | 2011-09-07 | 2012-02-15 | 洛阳金达石化有限责任公司 | Process method for extracting normal hexane and isohexane from crude hexane |
| CN102718617B (en) * | 2011-12-19 | 2014-05-28 | 天津联博化工股份有限公司 | System and method for refining isobutane |
| CN105949023B (en) * | 2016-05-16 | 2019-04-02 | 洛阳炼化奥油化工股份有限公司 | A kind of high-purity iso-butane production technology |
| CN115536487A (en) * | 2022-10-12 | 2022-12-30 | 宁波巨化化工科技有限公司 | High-purity low-carbon alkane production process and equipment |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6333442B1 (en) * | 1998-02-24 | 2001-12-25 | Institut Francais Du Petrole | Process for the preparation of an aliphatic alkylate with a high octane number from a C4 cracking fraction |
| CN101092321A (en) * | 2007-07-13 | 2007-12-26 | 沈阳泰富化工有限公司 | Method for separating out isobutene in high purity from liquefied petroleum gas |
| CN101519337A (en) * | 2009-03-25 | 2009-09-02 | 中国石油化工股份有限公司 | Method for fine desulfurization of high-sulfur C4 of refineries |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6333442B1 (en) * | 1998-02-24 | 2001-12-25 | Institut Francais Du Petrole | Process for the preparation of an aliphatic alkylate with a high octane number from a C4 cracking fraction |
| CN101092321A (en) * | 2007-07-13 | 2007-12-26 | 沈阳泰富化工有限公司 | Method for separating out isobutene in high purity from liquefied petroleum gas |
| CN101519337A (en) * | 2009-03-25 | 2009-09-02 | 中国石油化工股份有限公司 | Method for fine desulfurization of high-sulfur C4 of refineries |
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