CN107266277A - A kind of removing of the low temperature from solvent naphtha isoparaffin purification normal heptane, the technique of n-hexane - Google Patents
A kind of removing of the low temperature from solvent naphtha isoparaffin purification normal heptane, the technique of n-hexane Download PDFInfo
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- CN107266277A CN107266277A CN201710538824.8A CN201710538824A CN107266277A CN 107266277 A CN107266277 A CN 107266277A CN 201710538824 A CN201710538824 A CN 201710538824A CN 107266277 A CN107266277 A CN 107266277A
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- hexane
- tower
- normal heptane
- adsorption
- desorption
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- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 title claims abstract description 87
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000002904 solvent Substances 0.000 title claims abstract description 24
- 238000000746 purification Methods 0.000 title claims abstract description 17
- 238000003795 desorption Methods 0.000 claims abstract description 24
- 238000001179 sorption measurement Methods 0.000 claims abstract description 22
- 238000010924 continuous production Methods 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 230000000274 adsorptive effect Effects 0.000 claims abstract description 4
- IJDNQMDRQITEOD-UHFFFAOYSA-N sec-butylidene Natural products CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000010521 absorption reaction Methods 0.000 claims description 14
- 238000002336 sorption--desorption measurement Methods 0.000 claims description 13
- 239000003463 adsorbent Substances 0.000 claims description 8
- 238000010992 reflux Methods 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 239000002808 molecular sieve Substances 0.000 claims description 6
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 4
- 238000010926 purge Methods 0.000 claims description 4
- 238000011017 operating method Methods 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000004088 simulation Methods 0.000 abstract description 3
- 230000006872 improvement Effects 0.000 abstract description 2
- IXSZQYVWNJNRAL-UHFFFAOYSA-N etoxazole Chemical compound CCOC1=CC(C(C)(C)C)=CC=C1C1N=C(C=2C(=CC=CC=2F)F)OC1 IXSZQYVWNJNRAL-UHFFFAOYSA-N 0.000 abstract 1
- 238000000926 separation method Methods 0.000 description 7
- 239000000203 mixture Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000000605 extraction Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 150000001924 cycloalkanes Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Water Supply & Treatment (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses the technique of a kind of low temperature from solvent naphtha removing isoparaffin purification normal heptane, n-hexane, the technique is using solvent naphtha as raw material, through ADSORPTION IN A FIXED BED → fixed bed desorption → separator denitrogenation → n-hexane it is refined → normal heptane refines, continuous production, n-hexane and normal butane are respectively obtained, in the ADSORPTION IN A FIXED BED stage, Materials Solvents oil is passed directly into ADSORPTION IN A FIXED BED tower and adsorbed, adsorption temp is no more than 55 DEG C, and adsorptive pressure is no more than 8atm；The present invention is by the improvement to original production technology and production equipment on the market, compared to baroque Simulation moving bed, while can obtain high-purity normal heptane, normal hexane product, also has the advantages that product operation is simple, energy consumption is relatively low.
Description
Technical field
Taken off the present invention relates to the separation of organic compound and purification technique field, more particularly to one kind low temperature from solvent naphtha
The technique for purifying normal heptane, n-hexane except isoparaffin.
Background technology
It is social now, with the separation and the increasingly raising of purification technique of organic compound, grasped with product under molecular scale
Based on vertical and control technology, it then follows molecule oil refining, the theory of atom chemical industry, implement petroleum resources efficiently using being Resources for construction
An urgent demand of conservation-minded society.
In typical naphtha process solvent oil composition, n-alkane accounts for 16%, and isoparaffin accounts for 71%, and cycloalkane is accounted for
12%, aromatic hydrocarbons accounts for 1%.Wherein just, isoparaffin has important application in terms of agricultural chemicals, medicine intermediate, equipment cleaning.But
Directly to process component in obtained oil product more for naphtha on the market, and there is the same carbon number that relative volatility is more or less the same
N-alkane and isoparaffin, therefore can not be purified by a kind of simple separation means.Accordingly, it would be desirable to design a set of many
The separating technology of separation method coupling is planted, the purification of normal heptane and normal octane is carried out from above-mentioned oil product.
At present, the separation both at home and abroad to n-alkane in oil product and isoparaffin focuses primarily upon grinding for adsorption separation technology
Study carefully.Playing representational has moving-bed adsorption separating technology（SMB）.But the technique relates generally to Simulation moving bed, knot
Structure is complicated, and cost is higher.It is not suitable for promoting in medium-sized and small enterprises at home.
The content of the invention
It is a kind of suitable for industrial continuous production present invention aims at providing for above-mentioned problem, it is produced into
This is small, and energy consumption is low, the high removing of the low temperature from the solvent naphtha isoparaffin purification normal heptane of comprehensive benefit, the technique of n-hexane.
In order to achieve the above object, the technical solution adopted by the present invention is as follows：One kind low temperature from solvent naphtha removes isomery
Alkane purification normal heptane, the technique of n-hexane, the technique using solvent naphtha as raw material, through ADSORPTION IN A FIXED BED → fixed bed desorption → point
→ normal heptane refined from device denitrogenation → n-hexane is refined, and continuous production respectively obtains n-hexane and normal butane, in ADSORPTION IN A FIXED BED
Stage, Materials Solvents oil is passed directly into ADSORPTION IN A FIXED BED tower and adsorbed, and adsorption temp is no more than 55 DEG C, and adsorptive pressure does not surpass
Cross 8atm.
The technique of the present invention includes adsorption desorption tower, separator, n-hexane rectifying tower and normal heptane rectifying column, institute using device
The adsorption desorption tower stated, separator, n-hexane rectifying tower and normal heptane rectifying column are sequentially connected；Pass through each equipment of series connection, side
Just the continuous production of integrated artistic；Production equipment quantity itself is more simplified simultaneously, compared to other purifications in the prior art
The technique of normal heptane, n-hexane, is more prone to produce and promotes in medium-sized and small enterprises at home.
The removing isoparaffin of the low temperature from solvent naphtha that the present invention is provided purifies normal heptane, the technique of n-hexane, the work
The operating procedure of skill is as follows：
1）Absorption phase：Materials Solvents oil is passed directly into the adsorption desorption tower equipped with adsorbent, in 35 ~ 55 DEG C, 5 ~ 8 atm
Down by the molecular sieve adsorbent bed layer in adsorption desorption tower, absorption air speed is 0.5 ~ 0.8 h-1, adsorption time is 20 ~ 30 min.
2）Desorption stage：Enter desorbing agent N in the adsorption desorption tower completed to absorption2Purging, 180 ~ 200 DEG C of desorption temperature takes off
The atm of enclosure pressure 5 ~ 8, desorption air speed 200 ~ 250 h-1, the min of desorption time 20 ~ 30.
3）Separator denitrogenation：Mixed gas after desorption is cooled to after 35 ~ 55 DEG C, in feeding separator, separator top
Reclaim N in portion2, separator bottom product feeding n-hexane rectifying tower.
4）N-hexane is refined：The atm of operating pressure 1 of n-hexane rectifying tower, 65 ~ 75 DEG C of tower top temperature, reboiler temperature
90 ~ 100 DEG C, tower top obtains n-hexane, tower reactor liquid feeding normal heptane rectifying column.
5）Normal heptane is exquisite：The atm of operating pressure 1 of normal heptane rectifying column, 95 ~ 105 DEG C of tower top temperature, reboiler temperature
110 ~ 120 DEG C, tower top obtains normal heptane；Tower reactor liquid is reclaimed.
The step 1 of the present invention）In used adsorbent be the one or more in 5A molecular sieves or ZSM-5 molecular sieve.
Step 4 of the present invention）The reflux ratio R of middle n-hexane rectifying tower is 7 ~ 9, shown step 5）Middle normal heptane rectifying column
Reflux ratio R be 5 ~ 7.
The step 1 of the present invention）In adsorption desorption tower be made up of two tower bodies in parallel；Pass through two adsorption desorptions in parallel
Tower, can meet quantity-produced needs, when a device fails, continue to produce by another equipment, the company of satisfaction
The need for continuous metaplasia production.
The advantage of the invention is that：The purity of n-hexane and normal heptane product produced by the invention can reach 97 (wt) %
More than, because the present invention uses two ADSORPTION IN A FIXED BED tower recyclings, continuous production can be achieved.It is multiple compared to structure
Miscellaneous Simulation moving bed, while can obtain high-purity normal heptane, normal hexane product, also with product operation is simple, energy consumption
Relatively low advantage.
Brief description of the drawings
Fig. 1 is device connection diagram of the invention.
Embodiment
The present invention is described in further detail with embodiment for explanation below in conjunction with the accompanying drawings.
Embodiment 1：As shown in figure 1, a kind of removing of the low temperature from solvent naphtha isoparaffin purification normal heptane, the work of n-hexane
Skill, comprises the following steps：
1）Raw material is passed through in the ADSORPTION IN A FIXED BED tower equipped with adsorbent, into absorption phase.By inhaling under 35 DEG C, 5 atm
Attached dose of bed, absorption air speed is 0.5 h-1.This stage carries out 30 min, and gained is inhaled extraction raffinate feeding postorder workshop section and collected.
2）After above-mentioned absorption phase terminates, desorbing agent N is passed through2Purging, into desorption stage.Desorption stage carries out the time 30
Min, 180 DEG C of desorption temperature, the atm of desorption pressure 5, desorption air speed 200 h-1.Gained puffs away as absorption phase and N2Mixing
Gas.
2）The mixture temperature obtained in upper step is down to after 35 DEG C, in feeding separator.Separator tower top obtains N2
Can be as step 1）In desorbing agent recycle.
4）Separator bottom product sends into n-hexane rectifying tower, reflux ratio R=9, the atm of operating pressure 1, tower top temperature 69
DEG C, 93 DEG C of reboiler temperature.N-hexane rectifying tower tower top can obtain normal hexane product, n-hexane purity 97 ~ 99 (wt) %.
5）In tower reactor logistics feeding normal heptane rectifying column.Normal heptane rectifying column parameter is：Reflux ratio R=7, operating pressure 1
Atm, 99 DEG C of tower top temperature, 115 DEG C of reboiler temperature.Normal heptane rectifying column tower top can obtain normal heptane product, normal heptane product
Purity 97 ~ 99 (wt) %.
Embodiment 2：As shown in figure 1, a kind of removing of the low temperature from solvent naphtha isoparaffin purification normal heptane, the work of n-hexane
Skill, comprises the following steps：
1）Raw material is passed through in the ADSORPTION IN A FIXED BED tower equipped with adsorbent, into absorption phase.By inhaling under 40 DEG C, 8 atm
Attached dose of bed, absorption air speed is 0.5 h-1.This stage carries out 20 min, and gained is inhaled extraction raffinate feeding postorder workshop section and collected.
2）After above-mentioned absorption phase terminates, desorbing agent N is passed through2Purging, into desorption stage.Desorption stage carries out the time 20
Min, 200 DEG C of desorption temperature, the atm of desorption pressure 8, desorption air speed 250 h-1.Gained puffs away as absorption phase and N2Mixing
Gas.
3）The mixture temperature obtained in upper step is down to after 50 DEG C, in feeding separator.Separator tower top obtains N2
Can be as step 1）In desorbing agent recycle.
4) separator bottom product feeding n-hexane rectifying tower, reflux ratio R=7, the atm of operating pressure 1, tower top temperature 70
DEG C, 95 DEG C of reboiler temperature.N-hexane rectifying tower tower top can obtain normal hexane product, n-hexane purity 97 ~ 98 (wt) %.
5) in tower reactor logistics feeding normal heptane rectifying column.Normal heptane rectifying column parameter is：Reflux ratio R=7, operating pressure 1
Atm, 100 DEG C of tower top temperature, 117 DEG C of reboiler temperature.Normal heptane rectifying column tower top can obtain normal heptane product, normal heptane product
Purity 97 ~ 98 (wt) %.
Embodiment 3：Embodiment 1 ~ 2 is purified into entering with technical scheme of the prior art for normal heptane n-hexane implementing process
Row contrast, obtained result is as shown in the table：（Wherein comparative example 1 is in the prior art using moving-bed adsorption separation work
The result that skill is produced）
As seen from the above table：For being produced in the prior art using moving-bed adsorption separating technology, the present invention is most prominent
Improvement be to be the reduction to overall energy consumption, its adsorption temp for being primarily due to Solid Bed in production process does not surpass
Cross 55 DEG C, adsorptive pressure no more than caused by 8atm, and in-house facility compared with prior art in technique carry out it is big
The reduction of amount, installation area is small, installs more flexible, is more applicable for purchasing and producing for small business, production cost
Substantially reduce.
It should be noted that it is above-mentioned be only presently preferred embodiments of the present invention, not for limit the present invention protection model
Enclose, any combination or equivalents made on the basis of above-described embodiment belong to protection scope of the present invention.
Claims (6)
1. a kind of removing of the low temperature from solvent naphtha isoparaffin purification normal heptane, the technique of n-hexane, it is characterised in that the technique
Using solvent naphtha as raw material, through ADSORPTION IN A FIXED BED → fixed bed desorption → separator denitrogenation → n-hexane it is refined → normal heptane refines,
Continuous production, respectively obtains n-hexane and normal butane, in the ADSORPTION IN A FIXED BED stage, Materials Solvents oil is passed directly into ADSORPTION IN A FIXED BED
Adsorbed in tower, adsorption temp is no more than 55 DEG C, and adsorptive pressure is no more than 8atm.
2. the removing of the low temperature from solvent naphtha isoparaffin purification normal heptane according to claim 1, the technique of n-hexane, its
It is characterised by, described technique includes adsorption desorption tower, separator, n-hexane rectifying tower and normal heptane rectifying column, institute using device
The adsorption desorption tower stated, separator, n-hexane rectifying tower and normal heptane rectifying column are sequentially connected.
3. the removing of the low temperature from solvent naphtha isoparaffin purification normal heptane according to claim 1 or 2, the work of n-hexane
Skill, it is characterised in that the operating procedure of the technique is as follows：
1）Absorption phase：Materials Solvents oil is passed directly into the adsorption desorption tower equipped with adsorbent, in 35 ~ 55 DEG C, 5 ~ 8 atm
Down by the molecular sieve adsorbent bed layer in adsorption desorption tower, absorption air speed is 0.5 ~ 0.8 h-1, adsorption time is 20 ~ 30 min；
2）Desorption stage：Enter desorbing agent N in the adsorption desorption tower completed to absorption2Purging, 180 ~ 200 DEG C of desorption temperature, desorption pressure
The atm of power 5 ~ 8, desorption air speed 200 ~ 250 h-1, the min of desorption time 20 ~ 30；
3）Separator denitrogenation：Mixed gas after desorption is cooled to after 35 ~ 55 DEG C, in feeding separator, returned at the top of separator
Receive N2, separator bottom product feeding n-hexane rectifying tower；
4）N-hexane is refined：The atm of operating pressure 1 of n-hexane rectifying tower, 65 ~ 75 DEG C of tower top temperature, reboiler temperature 90 ~
100 DEG C, tower top obtains n-hexane, tower reactor liquid feeding normal heptane rectifying column；
5）Normal heptane is exquisite：The atm of operating pressure 1 of normal heptane rectifying column, 95 ~ 105 DEG C of tower top temperature, reboiler temperature 110 ~
120 DEG C, tower top obtains normal heptane；Tower reactor liquid is reclaimed.
4. the removing of the low temperature from solvent naphtha isoparaffin purification normal heptane according to claim 1, the technique of n-hexane, its
It is characterised by, described adsorbent is the one or more in 5A molecular sieves or ZSM-5 molecular sieve.
5. the removing of the low temperature from solvent naphtha isoparaffin purification normal heptane according to claim 1, the technique of n-hexane, its
It is characterised by, the step 4）The reflux ratio R of middle n-hexane rectifying tower is 7 ~ 9, shown step 5）Time of middle normal heptane rectifying column
Stream is 5 ~ 7 than R.
6. the removing of the low temperature from solvent naphtha isoparaffin purification normal heptane according to claim 1, the technique of n-hexane, its
It is characterised by, described step 1）In adsorption desorption tower be made up of two tower bodies in parallel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710538824.8A CN107266277B (en) | 2017-07-04 | 2017-07-04 | Process for purifying n-heptane and n-hexane by removing isoparaffin from solvent oil at low temperature |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710538824.8A CN107266277B (en) | 2017-07-04 | 2017-07-04 | Process for purifying n-heptane and n-hexane by removing isoparaffin from solvent oil at low temperature |
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| Publication Number | Publication Date |
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| CN107266277A true CN107266277A (en) | 2017-10-20 |
| CN107266277B CN107266277B (en) | 2021-07-16 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710538824.8A Active CN107266277B (en) | 2017-07-04 | 2017-07-04 | Process for purifying n-heptane and n-hexane by removing isoparaffin from solvent oil at low temperature |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101134703A (en) * | 2007-10-12 | 2008-03-05 | 南京工业大学 | Process for skellysolve C abstraction with combined production of octane product by pressure swing adsorption |
| CN101148390A (en) * | 2007-10-12 | 2008-03-26 | 中国石化扬子石油化工有限公司 | Technique for extracting high-pure normal hexane product by pressure swing adsorption |
-
2017
- 2017-07-04 CN CN201710538824.8A patent/CN107266277B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101134703A (en) * | 2007-10-12 | 2008-03-05 | 南京工业大学 | Process for skellysolve C abstraction with combined production of octane product by pressure swing adsorption |
| CN101148390A (en) * | 2007-10-12 | 2008-03-26 | 中国石化扬子石油化工有限公司 | Technique for extracting high-pure normal hexane product by pressure swing adsorption |
Non-Patent Citations (2)
| Title |
|---|
| SILVA J A ET AL.: "Sorption and diffusion of n-pentane in pellets of 5A zeolite", 《IND ENG CHEM RES》 * |
| 黄恒文等: "用吸附-精馏法分离重整抽余油中的正构烷烃", 《精细石油化工》 * |
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Denomination of invention: A Process for Low Temperature Removal of Isoalkanes and Purification of n-Heptane and n-Hexane from Solvent Oil Effective date of registration: 20240103 Granted publication date: 20210716 Pledgee: China Postal Savings Bank Co.,Ltd. Lai'an County Branch Pledgor: CHUZHOU RUNDA SOLVENTS Co.,Ltd. Registration number: Y2024980000220 |