CN110559681A - Device and method for preparing high-purity p-cresol - Google Patents
Device and method for preparing high-purity p-cresol Download PDFInfo
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- CN110559681A CN110559681A CN201910821184.0A CN201910821184A CN110559681A CN 110559681 A CN110559681 A CN 110559681A CN 201910821184 A CN201910821184 A CN 201910821184A CN 110559681 A CN110559681 A CN 110559681A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/004—Fractional crystallisation; Fractionating or rectifying columns
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/004—Fractional crystallisation; Fractionating or rectifying columns
- B01D9/0045—Washing of crystals, e.g. in wash columns
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
- C07C37/84—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment by crystallisation
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- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a device for preparing high-purity paracresol and a method for preparing the high-purity paracresol, wherein the device for preparing the high-purity paracresol comprises a shell with an accommodating space and a stirrer partially inserted into the accommodating space, the accommodating space is sequentially divided into a cooling crystallization area, a crystal bed growth area and a crystal melting area, a first feeding hole, a second feeding hole and a discharging hole are formed in the shell, the first feeding hole is communicated with the cooling crystallization area, and the second feeding hole and the discharging hole are respectively communicated with the crystal melting area. The method for preparing the high-purity p-cresol adopts the device for preparing the high-purity p-cresol. Compared with the prior art, the device for preparing high-purity p-cresol and the method for preparing high-purity p-cresol provided by the invention can be used for purifying the target object to be separated well, and the continuity and separation effect between solid and liquid phases are improved.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to the technical field of purification processes, in particular to a device and a method for preparing high-purity p-cresol.
[ background of the invention ]
p-methyl phenol is an important organic chemical raw material, and can be further processed to obtain a series of derivatives. The paracresol and the derivatives thereof are widely applied in the fields of medicines, pesticides, dyes, spices, cosmetics, foods, high polymer materials and the like. The components of the mixed phenol separated from the coal tar are isomers, and the basic physicochemical properties of p-cresol and m-cresol in the cresol isomers are shown in the following table:
| Para-cresol | M-cresol | |
| Melting Point C | 34.69 | 10.9 |
| Boiling point of | 202.27 | 202.8 |
The boiling points of the p-cresol and the m-cresol in the cresol isomers are very close, the separation and the purification by using a conventional rectification method are difficult, and the cresol monomers can be prepared by a melt crystallization method due to the large difference of the melting points of the p-cresol and the m-cresol. The melt crystallization method does not need extra solvent, has no pollution to the environment, can be said to be a green technology, and the melt crystallization method has good effect on extracting high-purity substances.
Therefore, it is necessary to provide a new apparatus for preparing high purity p-cresol and a method for preparing high purity p-cresol to solve the above problems.
[ summary of the invention ]
Aiming at the technical problems that in the related technology, the boiling points of p-cresol and m-cresol in cresol isomers are very close and the separation and purification are difficult to realize by using a conventional rectification method, the invention provides a device for preparing high-purity p-cresol by using a melt crystallization method.
The device for preparing the high-purity paracresol comprises a shell with an accommodating space and a stirrer partially inserted into the accommodating space, wherein the accommodating space is sequentially divided into a cooling crystallization area, a crystal bed growth area and a crystal melting area, a first feeding hole, a second feeding hole and a discharging hole are formed in the shell, the first feeding hole is communicated with the cooling crystallization area, and the second feeding hole and the discharging hole are respectively communicated with the crystal melting area.
preferably, the housing comprises a top, a bottom opposite to the top, and a sidewall connecting the top and the bottom, the cooling crystallization area is disposed near the top, the crystal melting area is disposed near the bottom, the first feed port and the second feed port are both opened on the sidewall, and the discharge port is opened at the bottom.
Preferably, the agitator is scraper formula agitator, the agitator include agitator motor, with agitator motor connects the (mixing) shaft and locate stir epaxial stirring helical blade, agitator motor is located the shell outside, the (mixing) shaft certainly the top penetrates in the accommodating space and run through in proper order the cooling crystallization district the crystal bed grows up the district and the crystal melting district.
Preferably, the apparatus for preparing high purity p-cresol further comprises a screen disposed in the receiving space, the screen being located between the crystal bed growth zone and the crystal melting zone.
Preferably, a waste liquid outlet is further formed in the shell, the waste liquid outlet is communicated with the cooling crystallization area, the waste liquid outlet is formed in the side wall and is spaced from the second feed port, and the waste liquid outlet is closer to the top than the second feed port.
preferably, the device for preparing high-purity p-cresol further comprises a circulating pump, and the circulating pump is respectively communicated with the first feeding hole, the second feeding hole and the discharging hole through pipelines.
preferably, the apparatus for preparing high-purity p-cresol further comprises a temperature control jacket, wherein the temperature control jacket is arranged on the shell and is used for controlling the temperature in the cooling crystallization area, the crystal bed growth area and the crystal melting area through media.
A method for preparing high-purity p-cresol using the apparatus for preparing high-purity p-cresol according to any one of the above items, comprising the steps of:
S1, melting the target substance to be separated into a liquid phase and sending the liquid phase to the cooling crystallization area through the second feeding hole;
S2, continuously crystallizing and separating the target object to be separated in the cooling crystallization area to form crystals, and feeding the crystals into a crystal bed growth area for sweating and purification;
S3, the crystal is washed by the molten liquid injected from the first feed inlet in the crystal bed growing zone in a counter-current mode, and the washed crystal continues to move to the crystal melting zone;
s4, continuously performing exosmosis on impurities in the crystals along with the increase of the temperature, continuously performing sweating purification, and continuously performing countercurrent washing on the crystals by the molten liquid injected from the first feed inlet to ensure that the purity of the crystals is higher and higher;
S5, finally, melting the crystal in the crystal melting area into liquid, and flowing out of the discharge hole.
Preferably, the method for preparing high-purity p-cresol further comprises the following steps:
s6, discharging one part of the liquid as a finished product, and returning the other part of the liquid as reflux liquid into the accommodating space from the first feed port and the second feed port respectively, wherein the reflux liquid returned by the second feed port continues to enter the cooling crystallization area as the target object to be separated, and the reflux liquid returned by the first feed port continues to perform countercurrent washing on the crystal as the molten liquid.
Preferably, the crystals in the step S2 enter the crystal bed growth zone through gravity, a pushing force of a stirrer, and an auxiliary pushing force of a circulation pump externally connected to the second feed port, and the reflux liquid in the step S6 is refluxed to the first feed port and the second feed port through the circulation pump.
Compared with the prior art, the device for preparing high-purity p-cresol provided by the invention can well purify the target object to be separated by adopting a melt crystallization method, and the cooling crystallization area, the crystal bed growth area and the crystal melting area are respectively equivalent to a tower top condenser, a tower plate and a tower bottom reboiler of a rectifying tower, so that the continuity and the separation effect between solid and liquid phases are improved.
Correspondingly, the method for preparing high-purity p-cresol provided by the invention adopts the device for preparing high-purity p-cresol, so that the target object to be separated can be well purified, and the continuity and separation effect between solid and liquid phases are improved.
[ description of the drawings ]
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without inventive efforts, wherein:
FIG. 1 is a schematic structural view of an apparatus for preparing high-purity p-cresol according to the present invention;
FIG. 2 is a schematic flow chart of the process for preparing high-purity p-cresol according to the present invention.
[ detailed description ] embodiments
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Please refer to fig. 1. The invention provides a device 100 for preparing high-purity p-cresol, which is a tower structure, wherein the device 100 for preparing high-purity p-cresol comprises a shell 20 with a containing space 10, a stirrer 30 partially inserted into the containing space 10, a screen 40 arranged in the containing space 10, a circulating pump 50 externally connected with the shell 20 and a temperature control jacket (not shown) arranged on the shell 20.
the accommodating space 10 is divided into a cooling crystallization region 11, a crystal bed growth region 12 and a crystal melting region 13 in this order, and the temperatures of the cooling crystallization region 11, the crystal bed growth region 12 and the crystal melting region 13 are different from each other. Specifically, the temperatures of the cooled crystallization zone 11, the crystal bed growth zone 12, and the crystal melting zone 13 are sequentially increased.
The shell 20 is provided with a first feed inlet 21, a second feed inlet 22, a discharge outlet 23 and a waste liquid outlet 24. The first feed inlet 21 and the waste liquid outlet 24 are respectively communicated with the cooling crystallization area 11, and the second feed inlet 22 and the discharge outlet 23 are respectively communicated with the crystal melting area 13.
The housing 20 includes a top portion 25, a bottom portion 26 disposed opposite the top portion 25, and a sidewall 27 connecting the top portion 25 and the bottom portion 26. The cooled crystallization zone 11 is disposed near the top 25 and the crystal melting zone 13 is disposed near the bottom 26. The first feed inlet 21, the second feed inlet 22 and the waste liquid outlet 24 are all arranged on the side wall 27, and the discharge outlet 23 is arranged at the bottom 26. Specifically, the waste liquid outlet 24 and the second feed inlet 22 are both opened on the side wall 27 and are arranged at intervals, and the waste liquid outlet 24 is closer to one side of the top 25 than the second feed inlet 22.
the stirrer 30 is a scraper stirrer, and specifically, the stirrer 30 comprises a stirring motor 31, a stirring shaft 32 connected with the stirring motor 31 and a stirring helical blade 33 arranged on the stirring shaft 32, the stirring motor 31 is positioned outside the shell 20, and the stirring shaft 32 penetrates from the top 25 into the accommodating space 10 and sequentially penetrates through the cooling crystallization area 11, the crystal bed growth area 12 and the crystal melting area 13.
the screen 40 is located between the crystal bed growth zone 12 and the crystal melting zone 13. Preferably, the screen 40 is a stainless steel screen, which can support the crystal bed growth zone 12 and prevent large crystal particles from falling into the crystal melting zone 13 and blocking the first feed port 21.
The circulating pump 50 is respectively communicated with the first feeding hole 21, the second feeding hole 22 and the discharging hole 23 through pipelines.
the temperature control jacket is installed around the housing 20, and is provided with a medium inlet and a medium outlet, and the temperature in the cooling crystallization zone 11, the crystal bed growth zone 12 and the crystal melting zone 13 is controlled by controlling the temperature of the medium.
The working principle of the device 100 for preparing high-purity p-cresol is as follows: during operation, the target substance to be separated is put into the pre-melting storage tank, nitrogen is introduced to prevent oxidation, the target substance to be separated is melted into a liquid phase in the pre-melting storage tank, the liquid phase is pumped to the second feeding hole 22 through the circulating pump 50 and enters the cooling crystallization area 11, the target substance with separation is continuously crystallized and separated in the cooling crystallization area 11, and the liquid phase enters the crystal bed growing area 12 by means of self gravity, the pushing force of the stirrer 30 and the auxiliary pushing force of the circulating pump 50. The crystals are deposited in said crystal bed growing zone 12 to form a dense crystal bed having a height at which they are subjected to sweat refining, while they are subjected to countercurrent washing with the melt from said crystal melting zone 13, which is injected into said crystal melting zone 13 through said first inlet 21. The washed crystal continuously moves towards the crystal melting zone 13, impurities in the crystal are continuously melted along with the rise of the temperature, sweating purification is continuously carried out, meanwhile, the melting liquid at the lower end continuously flows upwards to carry out countercurrent washing on the crystal, finally, the purity of the crystal is higher and higher, and finally, the crystal is completely melted into liquid in the crystal melting zone 13 and is discharged from the discharge hole 23. A part of the liquid discharged from the discharge port 23 is discharged as a finished product, and the other part of the liquid is pumped by the circulating pump 50 to flow as reflux to the first feed port 21 and the second feed port 22 respectively, so as to form an internal circulation located in the accommodating space 10 and an external circulation located outside the accommodating space 10 and powered by the circulating pump 50, and residual liquid generated in the purification process is discharged from the waste liquid outlet 24 at the upper end of the cooling crystallization zone 11.
In the purification operation, the target substance to be separated is pumped to the second feed port 22 through the circulation pump 50, the stirrer 30 is opened, the material is fed in a standing state after the liquid is filled, the temperature of the cooling crystallization zone 11 is controlled to generate a large amount of crystals, and the continuous feeding and discharging are started after the predetermined height of the crystals in the accommodating space 10 is reached.
In this embodiment, the target substance to be separated is the mixed phenol separated from the coal tar, in this embodiment, the p-cresol accounts for 80% and the m-cresol accounts for 20%, and after the purification by the apparatus 100 for preparing high-purity p-cresol, the purity of the p-cresol discharged from the discharge port 23 can reach more than 99.9%.
the apparatus 100 for preparing high-purity p-cresol simulates a rectifying tower, and the cooling crystallization zone 11, the crystal bed growth zone 12 and the crystal melting zone 13 are respectively equivalent to a tower top condenser, a tower plate and a tower bottom reboiler, so that the continuity and separation effect between solid and liquid phases are improved. The purification mechanism of the melt crystallization method, namely recrystallization, countercurrent washing and sweating, can be satisfied, and particularly the sweating and countercurrent washing mechanism can be fully utilized to improve the purity of the final product. The three sections of the cooling crystallization zone 11, the crystal growth zone 12 and the crystal melting zone 13 are precisely controlled in temperature and reasonably arranged, so that the reasonable operation of the device 100 for preparing high-purity p-cresol is ensured, and meanwhile, the energy consumption is greatly reduced. The external circulation pump 50 promotes the molten liquid to flow upwards by controlling the flow of the circulation pump 50, greatly improves the internal and external circulation effects of the molten liquid, can maintain higher crystal bed height, promotes countercurrent washing, and effectively improves the separation and purification effects. The stirrer 30 can mainly disperse solid-liquid two phases, and the solid-liquid continuity is greatly improved due to the existence of internal and external circulation, so that the rotating speed is not required to be too high, and the consumption of stirring kinetic energy is reduced. Meanwhile, the falling speed of the crystals can be promoted by the stirrer 30, so that the crystal bed layer is more compact. The temperature control jacket is used for carrying out heat preservation operation on the whole body, so that the temperature gradient in the accommodating space can be maintained, and the sweating effect can be controlled.
Meanwhile, the present invention also provides a method 200 for preparing high-purity p-cresol using the apparatus 100 for preparing high-purity p-cresol, wherein the method 200 for preparing high-purity p-cresol comprises the following steps:
S1, melting the target substance to be separated into a liquid phase and sending the liquid phase to the cooling crystallization area through the second feeding hole;
S2, continuously crystallizing and separating the target object to be separated in the cooling crystallization area to form crystals, and feeding the crystals into a crystal bed growth area for sweating and purification;
s3, the crystal is washed by the molten liquid injected from the first feed inlet in the crystal bed growing zone in a counter-current mode, and the washed crystal continues to move to the crystal melting zone;
s4, continuously performing exosmosis on impurities in the crystals along with the increase of the temperature, continuously performing sweating purification, and continuously performing countercurrent washing on the crystals by the molten liquid injected from the first feed inlet to ensure that the purity of the crystals is higher and higher;
S5, finally, melting the crystal in the crystal melting area into liquid, and flowing out of the discharge hole.
S6, discharging one part of the liquid as a finished product, and returning the other part of the liquid as reflux liquid into the accommodating space from the first feed port and the second feed port respectively, wherein the reflux liquid returned by the second feed port continues to enter the cooling crystallization area as the target object to be separated, and the reflux liquid returned by the first feed port continues to perform countercurrent washing on the crystal as the molten liquid.
Specifically, the crystals in the step S2 enter the crystal bed growth zone through gravity, a pushing force of a stirrer, and an auxiliary pushing force of a circulation pump externally connected to the second feed port, and the reflux liquid in the step S6 flows back to the first feed port and the second feed port through the circulation pump.
Compared with the prior art, the device for preparing high-purity p-cresol provided by the invention can well purify the target object to be separated by adopting a melt crystallization method, and the cooling crystallization area, the crystal bed growth area and the crystal melting area are respectively equivalent to a tower top condenser, a tower plate and a tower bottom reboiler of a rectifying tower, so that the continuity and the separation effect between solid and liquid phases are improved.
Correspondingly, the method for preparing high-purity p-cresol provided by the invention adopts the device for preparing high-purity p-cresol, so that the target object to be separated can be well purified, and the continuity and separation effect between solid and liquid phases are improved.
While the foregoing is directed to embodiments of the present invention, it will be understood by those skilled in the art that various changes may be made without departing from the spirit and scope of the invention.
Claims (10)
1. The device for preparing the high-purity p-cresol comprises a shell with an accommodating space and a stirrer partially inserted into the accommodating space, and is characterized in that the accommodating space is sequentially divided into a cooling crystallization area, a crystal bed growth area and a crystal melting area, a first feeding hole, a second feeding hole and a discharging hole are formed in the shell, the first feeding hole is communicated with the cooling crystallization area, and the second feeding hole and the discharging hole are respectively communicated with the crystal melting area.
2. The apparatus according to claim 1, wherein the casing comprises a top portion, a bottom portion disposed opposite to the top portion, and a side wall connecting the top portion and the bottom portion, the cooled crystallization zone is disposed near the top portion, the crystal melting zone is disposed near the bottom portion, the first and second feed openings are opened in the side wall, and the discharge opening is opened in the bottom portion.
3. the apparatus for preparing high purity p-cresol according to claim 2, wherein the stirrer is a scraper stirrer, the stirrer comprises a stirring motor, a stirring shaft connected to the stirring motor, and a stirring helical blade provided on the stirring shaft, the stirring motor is located outside the housing, and the stirring shaft penetrates into the accommodating space from the top and sequentially penetrates through the cooling crystallization zone, the crystal bed growth zone and the crystal melting zone.
4. the apparatus for preparing high purity p-cresol according to claim 2, further comprising a screen disposed in the accommodating space, wherein the screen is located between the crystal bed growth zone and the crystal melting zone.
5. The apparatus for preparing high purity p-cresol according to claim 2, wherein a waste liquid outlet is further formed in the casing, the waste liquid outlet is communicated with the cooling crystallization zone, the waste liquid outlet is formed in the side wall and spaced apart from the second feed opening, and the waste liquid outlet is closer to the top than the second feed opening.
6. The apparatus for preparing high-purity p-cresol according to claim 1, further comprising a circulation pump, wherein the circulation pump is respectively communicated with the first inlet, the second inlet and the outlet through pipelines.
7. The apparatus for preparing high-purity p-cresol according to claim 1, further comprising a temperature control jacket installed in the housing for controlling the temperature in the cooling crystallization zone, the crystal bed growth zone and the crystal melting zone by a medium.
8. a method for preparing high-purity p-cresol using the apparatus for preparing high-purity p-cresol according to any one of claims 1 to 7, comprising the steps of:
S1, melting the target substance to be separated into a liquid phase and sending the liquid phase to the cooling crystallization area through the second feeding hole;
s2, continuously crystallizing and separating the target object to be separated in the cooling crystallization area to form crystals, and feeding the crystals into a crystal bed growth area for sweating and purification;
s3, the crystal is washed by the molten liquid injected from the first feed inlet in the crystal bed growing zone in a counter-current mode, and the washed crystal continues to move to the crystal melting zone;
S4, continuously performing exosmosis on impurities in the crystals along with the increase of the temperature, continuously performing sweating purification, and continuously performing countercurrent washing on the crystals by the molten liquid injected from the first feed inlet to ensure that the purity of the crystals is higher and higher;
S5, finally, melting the crystal in the crystal melting area into liquid, and flowing out of the discharge hole.
9. The method of producing high-purity p-cresol according to claim 8, further comprising the steps of:
S6, discharging one part of the liquid as a finished product, and returning the other part of the liquid as reflux liquid into the accommodating space from the first feed port and the second feed port respectively, wherein the reflux liquid returned by the second feed port continues to enter the cooling crystallization area as the target object to be separated, and the reflux liquid returned by the first feed port continues to perform countercurrent washing on the crystal as the molten liquid.
10. The method of claim 9, wherein the crystals in step S2 are introduced into the crystal bed growth zone by gravity, the pushing force of the stirrer and the auxiliary pushing force of a circulation pump externally connected to the second inlet, and the reflux liquid is refluxed to the first inlet and the second inlet by the circulation pump in step S6.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113501748A (en) * | 2021-07-05 | 2021-10-15 | 湘潭大学 | Method for separating m-cresol and p-cresol |
| CN115337662A (en) * | 2022-08-29 | 2022-11-15 | 烟台裕祥精细化工有限公司 | Equipment and method for purifying isophthaloyl dichloride through layered melt crystallization |
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| 王化淳等: "我国对甲酚化工新进展", 《专论与综述》 * |
| 郑旭煦，李然 主编: "《化工原理 下》", 30 April 2009, 华中科技大学出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113501748A (en) * | 2021-07-05 | 2021-10-15 | 湘潭大学 | Method for separating m-cresol and p-cresol |
| CN115337662A (en) * | 2022-08-29 | 2022-11-15 | 烟台裕祥精细化工有限公司 | Equipment and method for purifying isophthaloyl dichloride through layered melt crystallization |
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| CN110559681B (en) | 2022-05-13 |
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