CN103848716B - Emulsion crystallization method of preparing crude anthracene from anthracene oil - Google Patents
Emulsion crystallization method of preparing crude anthracene from anthracene oil Download PDFInfo
- Publication number
- CN103848716B CN103848716B CN201410105078.XA CN201410105078A CN103848716B CN 103848716 B CN103848716 B CN 103848716B CN 201410105078 A CN201410105078 A CN 201410105078A CN 103848716 B CN103848716 B CN 103848716B
- Authority
- CN
- China
- Prior art keywords
- anthracene
- product
- emulsion
- carbolineum
- crude
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Nitrogen Condensed Heterocyclic Rings (AREA)
Abstract
The invention provides an emulsion crystallization method of preparing crude anthracene from anthracene oil, comprises the following steps: heating anthracene oil with anthracene content of 8-10%(wt) to 85-95 DEG C to completely melt, adding a surfactant and water, stirring and uniformly mixing to form emulsion, cooling to 35-40 DEG C, transferring crystal slurry into a centrifuge to centrifuge to obtain the crude anthracene product. The method only needs one crystallization operation, the process flow is simple, the anthracene content of the prepared crude anthracene product is 44-47%(wt), the average grading is 450-600 microns, the process mass yield is 8-11%. By adding less cheap surfactant and water, the anthracene oil with great viscosity can form the emulsion, the crystal substance system viscosity is reduced, the mixing effect is improved, the material is hard to adhere on the wall in the crystallization process, the mass transfer and heat transfer are enhanced, the operation time is shortened, and the purity and the yield of the crude anthracene product are beneficial to improvement.
Description
Technical field
The invention belongs to chemical engineering coal tar separation and purification field, particularly a kind of emulsion crystallization method being prepared crude anthracene by a carbolineum.
Technical background
One carbolineum is the cut in coal tar high temperature rectifying 300 ~ 360 DEG C of boiling ranges, and wherein anthracene content is between 7% ~ 10%.One carbolineum prepares crude anthracene by crystallization and purification, and containing 10 ~ 20 kinds of compounds in crude anthracene, mostly be the aromatic compounds of many rings, the main component of crude anthracene is: anthracene 35% ~ 45%, and luxuriant and rich with fragrance 15% ~ 25%, carbazole 10% ~ 20%.Crude anthracene is purified further and is obtained more highly purified anthracene, phenanthrene and carbazole, these three kinds of materials are important industrial chemicals, be widely used in the industries such as medicine, dyestuff, agricultural chemicals, the anthracene that purity is greater than 99.99% can be used for producing monocrystalline anthracene, and is applied in flicker survey meter as scintillator.
Prepare the method mainly crystallisation by cooling of crude anthracene, a carbolineum is warmed up to 85 ~ 95 DEG C and makes it fully melt, be then slow cooling to 35 ~ 45 DEG C and separate out solid, centrifugation obtains crude anthracene.Due to comparatively large containing a large amount of high-melting-point substances and viscosity in a carbolineum, there is following subject matter in producing in crude anthracene crystallization: (1) crude anthracene granularity is little, mean particle size about 200 μm, and product is mingled with seriously, and anthracene content is low, is difficult to reach more than 40%; (2) because system viscosity is high, in crystallisation by cooling process, crystal easily sticks on wall, increases heat transmission resistance, affects crystallization apparatus production capacity; (3) magma stickiness is large, centrifugation difficulty.
In two sections of crystallization processs disclosed in patent CN92104925.0, one carbolineum of anthracene content 4% ~ 7% is slow cooling to 30 ~ 35 DEG C by 90 DEG C and carries out one section of crystallization, centrifugal obtain anthracene content lower than 25% crude anthracene, add a carbolineum of anthracene content 4% ~ 7% again, high temperature melting obtains a carbolineum of anthracene content 7% ~ 10%, cool to 68 ~ 72 DEG C more gradually and carry out second segment crystallization, centrifugal obtain anthracene content higher than 40% crude anthracene; Filtrate continuation cools to 30 ~ 35 DEG C, obtains anthracene content lower than the crude anthracene of 25%, circulates for the next one.Patent CN96118957.6 discloses two sections of similar crystallization processs, and crude anthracene product content is 38% ~ 42%.Two sections of crystallization process technical process are complicated, and often criticizing a carbolineum needs to be separated with two times centrifugal through twice crystallization just can complete production, and the production cycle is long, and greatly, required equipment is many in power consumption, and pipeline complexity, easily causes line clogging.
Article the innovative approach of quality " improve crude anthracene " (fuel and chemical industry, 2009, vol40,1) causes separating effect bad for the problem of filter and whizzer, crude anthracene oil-containing, greatly moisture, and quality product is defective improves centrifugal filter operation.Article " producing of crude anthracene " (scientific and technological information exploitation and economy, 2011, vol21,36) improves the stirring rake of carbolineum crystallizer, reinforcing mass transfer, heat transfer.Crude anthracene crystallization production process also exists that magma viscosity is large, the problem of the little centrifugal difficulty of crude anthracene product granularity, transforms, fundamentally do not solve the problem that crude anthracene granularity is little, centrifugation is difficult to crystallizer agitator or centrifugal separation equipment.
Summary of the invention
In order to overcome the deficiencies in the prior art, the invention provides a kind of emulsion crystallization process being prepared crude anthracene by a carbolineum.The method by adding tensio-active agent and water in a carbolineum, and make a carbolineum form emulsion, then crystallisation by cooling, centrifugation obtain crude anthracene product.Magma viscosity is low, and product granularity is large, and velocity of separation is fast.
A kind of emulsion crystallization method being prepared crude anthracene by a carbolineum provided by the invention, its technical scheme is as follows:
By anthracene content 8% ~ 10%(wt) carbolineum of (wt all in literary composition is expressed as quality) is heated to 85 ~ 95 DEG C makes it melt completely, and add tensio-active agent and water, be uniformly mixed formation emulsion; Then 35 ~ 40 DEG C are cooled to; Magma is proceeded to whizzer separation and obtain crude anthracene product.
Described tensio-active agent is selected from the one in tween 80, polysorbate60, sorbester p17 or span 20.
The add-on of described tensio-active agent is 0.1% ~ 0.5% of a carbolineum quality, and the add-on of water is 1 ~ 10 times of surfactant qualities.
Described cooling rate is 2 ~ 7 DEG C/h.
Described centrifuge speed is 2000 ~ 3000r/min, centrifugation time 10 ~ 30min.
The inventive method only needs primary crystallization to operate, and technical process is simple, and processing ease is not high to equipment requirements, reduces preparation cost.The anthracene content of the crude anthracene product using the inventive method to prepare reaches 44% ~ 47%(wt), mean particle size reaches 450 ~ 600 μm, and procedure quality yield reaches 8% ~ 11%.Magma viscosity is little, not easily sticky wall, and centrifuge speeds is fast.
The advantage being prepared the emulsion crystallization process of crude anthracene by a carbolineum provided by the invention is that (1) is by adding a small amount of cheap tensio-active agent and water, the carbolineum making viscosity larger forms emulsion, reduce crystallization system viscosity, improve stirring and mixing effect, make material not easily sticky wall in crystallisation process, thus enhance mass transfer and heat transfer, shorten the operating time, be beneficial to and improve crude anthracene product purity and yield; (2) in uniform emulsion system, crystallization is carried out in each drop, the existence of drop facilitates mass transfer and heat transfer, and water-oil interface provide the chance of Crystallisation, effectively can control nucleation rate, be conducive to that prepared sizes are large, the crude anthracene product of even particle size distribution, the crude anthracene product that granularity is large is easy to centrifugation, can effectively improve whizzer working efficiency; (3) gained crude anthracene product granularity is large, stickiness is low, is easy to storage and transport, also decreases to the dust pollution degree that environment causes.
Embodiment
Embodiment 1:
By anthracene content 9.3%(wt) a carbolineum 500g be heated to 90 DEG C and make it melt completely, add 0.5g tensio-active agent sorbester p17 and 1.5g water, be uniformly mixed formation emulsion; Then 35 DEG C are cooled to the rate of temperature fall of 2 DEG C/h; Magma is proceeded to whizzer, centrifugal 20min under 3000r/min, obtain crude anthracene product 45.35g.Yield 9.1%, product granularity 506 μm, anthracene content 44.2% in product.Magma viscosity is little, not easily sticky wall, and centrifuge speeds is fast.
Embodiment 2:
By anthracene content 8.1%(wt) a carbolineum 500g be heated to 85 DEG C and make it melt completely, add 1.0g surface active agent tween 60 and 1.0g water, be uniformly mixed formation emulsion; Then 36 DEG C are cooled to the rate of temperature fall of 3.0 DEG C/h; Magma is proceeded to whizzer, centrifugal 30min under 2000r/min, obtain crude anthracene product 41.50g.Yield 8.3%, product granularity 456 μm, anthracene content 46.3% in product.Magma viscosity is little, not easily sticky wall, and centrifuge speeds is fast.
Embodiment 3:
By anthracene content 9.9%(wt) a carbolineum 500g be heated to 95 DEG C and make it melt completely, add 1.5g tensio-active agent span 20 and 15g water, be uniformly mixed formation emulsion; Then 35 DEG C are cooled to the rate of temperature fall of 4 DEG C/h; Magma is proceeded to whizzer, centrifugal 10min under 2500r/min, obtain crude anthracene product 53.90g, yield 10.8%, product granularity 601 μm, anthracene content 47.2% in product.Magma viscosity is little, not easily sticky wall, and centrifuge speeds is fast.
Embodiment 4:
By anthracene content 9.5%(wt) a carbolineum 500g be heated to 90 DEG C and make it melt completely, add 2.0g tensio-active agent sorbester p17 and 16g water, be uniformly mixed formation emulsion; Then 38 DEG C are cooled to the rate of temperature fall of 5.5 DEG C/h; Magma is proceeded to whizzer, centrifugal 25min under 3000r/min, obtain crude anthracene product 51.40g, yield 10.3%, product granularity 583 μm, anthracene content 47.0% in product.Magma viscosity is little, not easily sticky wall, and centrifuge speeds is fast.
Embodiment 5:
By anthracene content 8.3%(wt) a carbolineum 500g be heated to 85 DEG C and make it melt completely, add 2.5g surface active agent tween 80 and 10g water, be uniformly mixed formation emulsion; Then 40 DEG C are cooled to the rate of temperature fall of 7 DEG C/h; Magma is proceeded to whizzer, centrifugal 20min under 2800r/min, obtain crude anthracene product 40.25g, yield 8.1%, product granularity 548 μm, anthracene content 45.9% in product.Magma viscosity is little, not easily sticky wall, and centrifuge speeds is fast.
The emulsion crystallization method method being prepared crude anthracene by a carbolineum that the present invention discloses and proposes, those skilled in the art are by using for reference present disclosure, appropriate change raw material, and the links such as processing parameter are tested.Method of the present invention and product are described by preferred embodiments, person skilled obviously can be changed method as herein described and product or suitable change and combination not departing from content of the present invention, spirit and scope, realizes the technology of the present invention.Special needs to be pointed out is, all similar replacements and change are apparent concerning this technician, and they are deemed to be included in spirit of the present invention, scope and content.
Claims (4)
1. prepared an emulsion crystallization method for crude anthracene by a carbolineum, it is characterized in that: a carbolineum of anthracene mass content 8% ~ 10% is heated to 85 ~ 95 DEG C and makes it melt completely, add tensio-active agent and water, be uniformly mixed formation emulsion; Then 35 ~ 40 DEG C are cooled to; Magma is proceeded to whizzer separation and obtain crude anthracene product; Described cooling rate is 2 ~ 7 DEG C/h.
2. the method for claim 1, is characterized in that, described tensio-active agent is selected from the one in tween 80, polysorbate60, sorbester p17 or span 20.
3. the method for claim 1, is characterized in that, the add-on of described tensio-active agent is 0.1% ~ 0.5% of a carbolineum quality, and the add-on of water is 1 ~ 10 times of surfactant qualities.
4. the method for claim 1, is characterized in that, described centrifuge speed is 2000 ~ 3000r/min, centrifugation time 10 ~ 30min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410105078.XA CN103848716B (en) | 2014-03-20 | 2014-03-20 | Emulsion crystallization method of preparing crude anthracene from anthracene oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410105078.XA CN103848716B (en) | 2014-03-20 | 2014-03-20 | Emulsion crystallization method of preparing crude anthracene from anthracene oil |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103848716A CN103848716A (en) | 2014-06-11 |
| CN103848716B true CN103848716B (en) | 2015-07-22 |
Family
ID=50856883
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410105078.XA Active CN103848716B (en) | 2014-03-20 | 2014-03-20 | Emulsion crystallization method of preparing crude anthracene from anthracene oil |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103848716B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1161951A (en) * | 1996-02-09 | 1997-10-15 | 鞍山钢铁公司 | Two-stage crystallization method for extracting coarse anthracene from anthracene oil |
| CN102304013A (en) * | 2011-07-21 | 2012-01-04 | 辽宁科技学院 | Novel process for producing refined anthracene and refined carbazole by taking crude anthracene as raw material |
-
2014
- 2014-03-20 CN CN201410105078.XA patent/CN103848716B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1161951A (en) * | 1996-02-09 | 1997-10-15 | 鞍山钢铁公司 | Two-stage crystallization method for extracting coarse anthracene from anthracene oil |
| CN102304013A (en) * | 2011-07-21 | 2012-01-04 | 辽宁科技学院 | Novel process for producing refined anthracene and refined carbazole by taking crude anthracene as raw material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103848716A (en) | 2014-06-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102372591B (en) | Crystallization method for p-xylene production | |
| CN103420401B (en) | Method for preparing large-particle picromerite | |
| CN102070127A (en) | Method for producing insoluble sulfur | |
| CN104402023B (en) | A kind of production method improving carbonizatin method sodium bicarbonate product granularity | |
| CN102329212A (en) | Refining method for long-chain binary acid | |
| CN102371080B (en) | Crystallizing method utilizing external circulation of crystal slurry | |
| CN104844425A (en) | Synthetic method of 2,6 dihydroxy naphthlene | |
| CN105480994A (en) | Efficient method for enriching oxalate through washing of fine seeds | |
| CN103848716B (en) | Emulsion crystallization method of preparing crude anthracene from anthracene oil | |
| CN103013339B (en) | Dewaxing and degreasing method of shellac resin | |
| CN103058857A (en) | Preparation method of disproportionated rosin potassium soap | |
| CN104479707B (en) | A kind of method for preparing needle coke | |
| CN112745969B (en) | Method for preparing fatty acid type diesel oil antiwear agent by low-temperature freezing | |
| CN1417123A (en) | Production process of heavy soda ash | |
| CN102371081A (en) | Crystallization method with a fine crystal elimination | |
| CN103896814B (en) | Method for preparing sulfonated dehydroabietic acid | |
| CN103232402B (en) | A kind of method of Hydrolysis kinetics azophenlyene from 4-aminodiphenylamine waste material | |
| JPS61197688A (en) | Refining of coal-based pitch | |
| CN103709007A (en) | Cooling coupling solvent-out crystallization refinement method of erythritol | |
| CN105112090B (en) | Oil wax separating agent, preparation method thereof and oil wax separating method | |
| EP0004717A2 (en) | Improved method for separating solids from coal liquids | |
| CN112876331A (en) | Production method of durene | |
| CN105523878B (en) | A kind of method of rotary drum purifying industrial fluorenes | |
| CN115161071B (en) | Method for purifying decrystallized anthracene oil by ceramic membrane filtration and catalytic coupling | |
| CN209442915U (en) | A kind of integrated apparatus producing hot-fusible pressure-sensitive adhesive |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |