CN107721803A - A kind of method that durol is extracted in the C10 aromatic solvent naphthas from lightweight - Google Patents
A kind of method that durol is extracted in the C10 aromatic solvent naphthas from lightweight Download PDFInfo
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- CN107721803A CN107721803A CN201711084043.2A CN201711084043A CN107721803A CN 107721803 A CN107721803 A CN 107721803A CN 201711084043 A CN201711084043 A CN 201711084043A CN 107721803 A CN107721803 A CN 107721803A
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- China
- Prior art keywords
- steel belt
- durol
- crystal
- steel
- lightweight
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/14—Purification; Separation; Use of additives by crystallisation; Purification or separation of the crystals
Abstract
The invention discloses from lightweight C10The method that durol is extracted in aromatic solvent naphtha, including continuous steel belt crystallization apparatus, the device includes the shell in a certain angle with horizontal direction, cooling medium pipe and steel belt inside the housing is set, and it is arranged on the charge door and crystal discharging opening of case surface, cooling medium pipe presses close to the lower surface of steel band on the upside of steel belt, and charge door is located at the top of steel band on the upside of steel belt；Upside steel strip surface including raw material to be added to steel belt by charge door, control charging rate, pass through cooling medium management and control steel belt temperature, control residence time of the raw material on steel band simultaneously, when crystal reaches upper end on steel belt, crystal is taken from crystal discharging opening, produces the durol；The inventive method can operate continuously, and equipment therefor is easy to control crystallization temperature and crystallization and the separation of mother liquor, after optimal conditions separation, can disposably obtain up to 99.18% or so durol crystal, yield can be up to 90.95%.
Description
Technical field
The invention discloses one kind from lightweight C10The method that durol is extracted in aromatic solvent naphtha, belongs to industrial chemicals and carries
Take technical field.
Background technology
Durol is the important source material of current production pyromellitic acid anhydride, and pyromellitic acid anhydride is the poly- phthalein of production
Imines insulation film is most economical, optimal raw material.
Being refined at present on durol mainly has absorption method and crystallisation, and absorption method is to exchange to inhale on X zeolite in file
Durol is received, removes other non-adsorbed aromatic hydrocarbons, adsorbate is then desorbed using low boiling hydrocarbon (>=5 DEG C), then using flash distillation
De- low boiling hydrocarbon obtains durol, and this method is in absorption and desorption process, and product purity is unstable, continuous operation is difficult；Knot
Brilliant typically to have kettle type crystallization, pillar and shell and tube crystallization and falling film type crystallization etc., kettle type crystallization is simple, but product purity and yield
Low, letter is had a rest operation；Pillar and shell and tube crystallization apparatus are simple in construction, and material is added inside crystallizer, is passed through in chuck cold
Thermal medium carries out temperature control, until wherein easy crystallographic component is fully crystallized, can typically reach the requirement of design, but crystallization time compared with
Long, cold and hot medium contact area is small, and the upper and lower part crystallization difference that inside has temperature difference, especially crystallization post is larger, knot
Brilliant process is uneven, and the purity and yield of crystalline product are relatively low；Shell and tube crystallization apparatus is to lead to cooling medium, shell side in tube side
A kind of crystallization mode of logical raw material, increase cold and hot medium contact area, the process needs to crystallize and melt two steps, and handles crystal grain
During larger material, crystal is easily sticked to outer wall, easily causes magma blocking, can not realize and operate continuously for a long time.
The content of the invention
Goal of the invention：Existing under production in order to make up, the invention provides a kind of continuous transmission crystallization extraction lightweight C10
The method of durol in aromatic solvent naphtha, this method, as crystalline carrier, control Steel Belt Transmission mistake using continuous steel belt
Temperature and velocity of rotation in journey, reach extraction lightweight C10The purpose of durol in aromatic solvent naphtha.The process is realized continuous
Crystallize to form one and equality of temperature operation with separating, after separation, can disposably obtain up to 99.18% or so durol crystalline substance
Body, yield can be up to 90.95%.
Technical scheme：The invention provides one kind from lightweight C10The method that durol is extracted in aromatic solvent naphtha, the party
Method includes a kind of continuous steel belt crystallization apparatus, and the device includes the shell in a certain angle with horizontal direction, is arranged on
The cooling medium pipe and steel belt of enclosure, and the charge door and crystal discharging opening of case surface are arranged on, cooling is situated between
Matter pipe presses close to the lower surface of steel band on the upside of steel belt, and charge door is located at the top of steel band on the upside of steel belt；
Methods described includes the upside steel strip surface that raw material is added to steel belt by charge door, control charging speed
Degree, by cooling medium management and control steel belt temperature, while controls residence time of the raw material on steel band, brilliant on steel belt
When body reaches upper end, crystal is taken from crystal discharging opening, produces the durol.
In methods described, charging rate 40-80ml/h, preferably 60ml/h；Steel belt temperature is -10-0 DEG C, preferably -
5~-6 DEG C, residence time 3-5h, preferably 4 hours.
In the continuous steel belt crystallization apparatus, case surface is additionally provided with mother liquor discharging opening, steel belt clockwise direction
Upper rotation, crystal discharging opening are located near steel belt upper end, and are in contact provided with wing with the steel band of steel belt, energy
The solid material on steel band is enough set to fall into crystal discharging opening, mother liquor discharging opening is located at steel belt lower end.
Described and horizontal direction shell in a certain angle, wherein angle is 15-45 °.
The cooling medium pipe is spiral coil cooling tube, and one end that its horizontal position is set low is provided with refrigerant import, horizontal position
High one end is put to export provided with refrigerant.
The high one end of the steel belt horizontal level is provided with rotary shaft and buncher, and one end that horizontal position is set low is provided with
Power transmission shaft.
The charge door includes the first charge door, the second charge door and the 3rd charge door.
Crystal collecting tank is additionally provided with below the crystal discharging opening.
The case surface, the first temperature measuring point and the second temperature measuring point are additionally provided with close to the position of cooling medium pipe.
Technique effect：Compared with prior art, the inventive method can operate continuously, and equipment therefor is easy to control crystallization temperature
And crystallization and the separation of mother liquor, after optimal conditions separation, it can disposably obtain up to 99.18% or so durol crystalline substance
Body, yield can be up to 90.95%.
Brief description of the drawings
Fig. 1 is the inventive method process chart, including：Power transmission shaft 2, the first charge door 4, the second charge door 5,
Three charge doors 6, steel belt 7, rotary shaft 8, wing 10, crystal discharging opening 11, crystal collecting tank 12, shell 13, mother liquor go out
Material mouth 14, refrigerant import 15, refrigerant export the 16, first temperature measuring point 17, the second temperature measuring point 18 and low-temperature circulating freezing
Case 19.
Fig. 2 is continuous steel belt crystallization apparatus side view in the inventive method：Including：Cooling medium pipe 3, speed governing
Motor 9, remaining same Fig. 1；
Fig. 3 is continuous steel belt crystallizer birds-eye perspective in the inventive method, and wherein reference is the same as Fig. 1 and Fig. 2；
Fig. 4 is influence of the temperature to purity and yield in the inventive method；
Fig. 5 be in the inventive method the residence time purity and yield are influenceed；
Fig. 6 is that charging rate influences on purity and yield in the inventive method.
Embodiment
The present invention will be described in detail with reference to the accompanying drawings and detailed description, and described embodiment contributes to this
The understanding and implementation of invention, are not construed as limiting the invention, and implement the present invention, except material involved in specific embodiment
Outside distillation operation condition, those skilled in the art can also carry out equivalent or equivalent change according to different separation purposes to it
Change.Unless otherwise indicated, the percentage in the present invention is mass percent.
Embodiment 1
Continuous steel belt crystallization apparatus in the inventive method, as depicted in figs. 1 and 2, including with horizontal direction in certain
The shell 13 of angle, the cooling medium pipe 3 and steel belt 7 being arranged on inside shell 13, and it is arranged on the surface of shell 13
Charge door, crystal discharging opening 11 and mother liquor discharging opening 14；The cooling medium pipe 3 presses close to the following table of the upside steel band of steel belt 7
Face, charge door are located at the top of the upside steel band of steel belt 7, and steel belt 7 is rotated up clockwise, and crystal discharging opening 11 is located at
Near the upper end of steel belt 7, and it is in contact provided with wing 10 with the steel band of steel belt 7, the solid on steel band can be made
Material falls into crystal discharging opening 11, and mother liquor discharging opening 14 is located at the lower end of steel belt 7.
The shell 13 in a certain angle with horizontal direction, wherein angle are 15-45 °.
Cooling medium pipe 3 is spiral coil cooling tube, and one end that its horizontal position is set low is provided with refrigerant import 15, horizontal level
High one end is provided with refrigerant outlet 16.
The high one end of the horizontal level of steel belt 7 is provided with rotary shaft 8 and buncher 9, and one end that horizontal position is set low is provided with
Power transmission shaft 2.
Charge door includes the first charge door 4, the second charge door 5 and the 3rd charge door 6.
The lower section of crystal discharging opening 11 is additionally provided with crystal collecting tank 12.
The surface of shell 13, the first temperature measuring point 17 and the second temperature measuring point 18 are additionally provided with close to the position of cooling medium pipe 3.
The device basic functional principle and method are as follows
(1) cooling worm 3 controls coolant temperature, cooling medium enters from the lower end of spiral coil cooling tube 3, on bring out, then
Low-temperature circulating household freezer 19 is back to by transmission crystallizer upper end.
(2) 3 charging apertures of design above steel belt crystallization apparatus, including the first charge door 4, the second charge door 5 and the
Three charge doors 6, difference is formed according to raw material, selects different feed locations.Design steel belt specification be 150mm ×
1000mm, the temperature of steel belt 7 is controlled by serpentine condenser 3, reaches control crystallization temperature；Controlled by buncher 9
The transmission speed of steel band, reach control raw material residence time on steel band.
(3) after temperature and transmission speed are stable, the charging rate of raw material is controlled, crystal reaches upper end on steel belt
When, crystal is taken from crystal discharging opening 11, takes mother liquor to be analyzed from lower end mother liquor discharging opening 14.Inlet amount is advised with steel belt 7
Lattice are adjusted by equal proportion.
Embodiment 2
Using above-mentioned continuous steel belt crystallization apparatus from lightweight C10The method that durol is extracted in aromatic solvent naphtha：
By the operating method of said apparatus, by raw material C10(durol mass content 36% or so, is referred to aromatic solvent naphtha
Shown in table 1) the upside steel strip surface of steel belt is added to by charge door, charging rate is controlled, passes through cooling medium management and control
Steel belt temperature processed, while residence time of the raw material on steel band is controlled, when crystal reaches upper end on steel belt, from crystal
Discharging opening takes crystal, produces the durol.
In methods described, charging rate 40-80ml/h, steel belt temperature is -10-0 DEG C, residence time 3-5h.
It is specific as follows：
1st, with the lightweight C containing durol 36.87%10Aromatic hydrocarbons is raw material, C10Aromatic solvent naphtha is from steel belt crystallizer
Top adds, and controls inlet amount 60ml/h, keeps residence time 4h of the raw material on steel band, investigates control temperature to durol
The change of content and yield.Crystallization temperature and durol content and yield relation such as Fig. 4, as seen from Figure 4, crystallization temperature
At 0~-6 DEG C, the content and yield of durol are in rising trend for control, when crystallization temperature reaches -5~-6 DEG C, equal four
Toluene level and yield reach maximum, and continuing, which reduces crystallization temperature durol content, has declined, and yield change is little, therefore warm
It is optimal crystallization temperature to spend for -5~-6 DEG C.
2nd, under the conditions of crystallization temperature is -5~-6 DEG C, feeding quantity is 60ml/h, the investigation residence time contains to durol
The influence of amount and yield, change of the residence time for durol content and yield under the conditions of 3,3.5,4,4.5,5h is considered respectively
Change.As a result as shown in figure 5, residence time control was at 4 hours, the content and yield of durol reach maximum, during stop
Between extend after, durol content has declined, and yield change is little, thus the residence time be 4 hours preferably.
3rd, -5~-6 DEG C of steel belt temperature and residence time 4h are controlled, investigates charging rate to durol content and receipts
The change of rate.As a result as shown in fig. 6, when Fig. 6 shows that charging rate increases to 60ml/h, the content of durol reaches
99.18%, content is reduced when being further added by, but yield change is little.Therefore charging control for 60ml/h it is more suitable.
4th, for the crystallizer that steel belt specification is 150mm × 1000mm, control inlet amount 60ml/h, steel belt temperature
- 5~-6 DEG C and residence time 4h of degree is more suitable.With optimal conditions, separating resulting is shown in Table 1, durol purity and
Yield respectively reaches 99.18% and 90.95%.
A kind of continuous transmission crystallization extraction lightweight C of table 110The result of durol in aromatic solvent naphtha
Embodiment 3
The same Examples 1 and 2 of apparatus and method, the difference is that only as follows：
Charging rate is 40ml/h, and steel belt temperature is -10--9 DEG C, residence time 5h；
Final gained durol purity and yield respectively reach 98.67% and 89.34%.
Embodiment 4
The same Examples 1 and 2 of apparatus and method, the difference is that only as follows：
Charging rate is 80ml/h, and steel belt temperature is -1-0 DEG C, residence time 3h；
Final gained durol purity and yield respectively reach 98.72% and 89.45%.
Claims (9)
- It is 1. a kind of from lightweight C10The method that durol is extracted in aromatic solvent naphtha, it is characterised in that this method includes one kind Continuous steel belt crystallization apparatus, the device include the shell in a certain angle with horizontal direction, set inside the housing cold But medium tube and steel belt, and the charge door and crystal discharging opening of case surface are arranged on, cooling medium pipe presses close to transmission The lower surface of steel band on the upside of steel band, charge door are located at the top of steel band on the upside of steel belt；Methods described includes the upside steel strip surface that raw material is added to steel belt by charge door, controls charging rate, leads to Supercooling medium tube controls steel belt temperature, while controls residence time of the raw material on steel band, and crystal arrives on steel belt During up to upper end, crystal is taken from crystal discharging opening, produces the durol.
- It is 2. according to claim 1 from lightweight C10The method that durol is extracted in aromatic solvent naphtha, it is characterised in that institute State in method, charging rate 40-80ml/h, steel belt temperature is -10-0 DEG C, residence time 3-5h.
- It is 3. according to claim 1 from lightweight C10The method that durol is extracted in aromatic solvent naphtha, it is characterised in that institute State in continuous steel belt crystallization apparatus, case surface is additionally provided with mother liquor discharging opening, and steel belt is rotated up clockwise, crystal Discharging opening is located near steel belt upper end, and is in contact provided with wing with the steel band of steel belt, can make on steel band Solid material fall into crystal discharging opening, mother liquor discharging opening is located at steel belt lower end.
- It is 4. according to claim 1 from lightweight C10The method that durol is extracted in aromatic solvent naphtha, described and level side To shell in a certain angle, wherein angle is 15-45 °.
- It is 5. according to claim 1 from lightweight C10The method that durol is extracted in aromatic solvent naphtha, it is characterised in that institute It is spiral coil cooling tube to state cooling medium pipe, and one end that its horizontal position is set low is provided with refrigerant import, the high one end of horizontal level Exported provided with refrigerant.
- It is 6. according to claim 1 from lightweight C10The method that durol is extracted in aromatic solvent naphtha, it is characterised in that institute State the high one end of steel belt horizontal level and be provided with rotary shaft and buncher, one end that horizontal position is set low is provided with power transmission shaft.
- It is 7. according to claim 1 from lightweight C10The method that durol is extracted in aromatic solvent naphtha, it is characterised in that institute Stating charge door includes the first charge door, the second charge door and the 3rd charge door.
- It is 8. according to claim 1 from lightweight C10The method that durol is extracted in aromatic solvent naphtha, it is characterised in that institute State and be additionally provided with crystal collecting tank below crystal discharging opening.
- It is 9. according to claim 1 from lightweight C10The method that durol is extracted in aromatic solvent naphtha, it is characterised in that institute Case surface is stated, the first temperature measuring point and the second temperature measuring point are additionally provided with close to the position of cooling medium pipe.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711084043.2A CN107721803A (en) | 2017-11-07 | 2017-11-07 | A kind of method that durol is extracted in the C10 aromatic solvent naphthas from lightweight |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711084043.2A CN107721803A (en) | 2017-11-07 | 2017-11-07 | A kind of method that durol is extracted in the C10 aromatic solvent naphthas from lightweight |
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| CN107721803A true CN107721803A (en) | 2018-02-23 |
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| CN201711084043.2A Pending CN107721803A (en) | 2017-11-07 | 2017-11-07 | A kind of method that durol is extracted in the C10 aromatic solvent naphthas from lightweight |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110368712A (en) * | 2019-08-07 | 2019-10-25 | 南京师范大学 | A kind of device and method of continuous three sections of two-stages temperature gradient formula crystal refining durol |
| CN111377793A (en) * | 2020-04-09 | 2020-07-07 | 北方华锦化学工业股份有限公司 | Method for decoloring solvent oil and extracting durene |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1061728A (en) * | 1990-11-27 | 1992-06-10 | 苏舍兄弟有限公司 | Device by crystallization separate substance from liquid mixture |
-
2017
- 2017-11-07 CN CN201711084043.2A patent/CN107721803A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1061728A (en) * | 1990-11-27 | 1992-06-10 | 苏舍兄弟有限公司 | Device by crystallization separate substance from liquid mixture |
Non-Patent Citations (1)
| Title |
|---|
| 黄杰军: ""萃取精馏与连续结晶集成提取均四甲苯的研究"", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110368712A (en) * | 2019-08-07 | 2019-10-25 | 南京师范大学 | A kind of device and method of continuous three sections of two-stages temperature gradient formula crystal refining durol |
| CN111377793A (en) * | 2020-04-09 | 2020-07-07 | 北方华锦化学工业股份有限公司 | Method for decoloring solvent oil and extracting durene |
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Application publication date: 20180223 |