CN102423542B - Melt crystallizer - Google Patents
Melt crystallizer Download PDFInfo
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- CN102423542B CN102423542B CN201110250841.4A CN201110250841A CN102423542B CN 102423542 B CN102423542 B CN 102423542B CN 201110250841 A CN201110250841 A CN 201110250841A CN 102423542 B CN102423542 B CN 102423542B
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- housing
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- rotation filler
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Abstract
Relates to a melt crystallization technology, the invention specifically provides a melt crystallizer, which solves the problems of large occupied area, complex operation and low separation efficiency in existing melt crystallizers. The melt crystallizer comprises a shell, a liquid distributor inserted into the shell from the shell top, and rotary filler that is disposed inside the shell and equipped with a driving device. A gap is left between the liquid distributor and the rotary filler. The top of the shell is provided with an air outlet, and the bottom of the shell is equipped with an air inlet and a liquid outlet. And the outside of the shell is sleeved with a constant temperature jacket. The product of the invention has simple structure, low cost, stable running, high separation efficiency as well as easy operation, and is widely suitable for separation of all isomers and homologue organic matters with obvious melting point difference.
Description
Technical field
The present invention relates to fusion-crystallization technology, be specially a kind of melting crystallizer.
Background technology
In the last few years, along with the develop rapidly of the industry such as chemical industry, food, medicine and material, these industry were more and more higher to the purity requirement of a lot of products, very strict and harsh to the purity requirement of the industries such as medicine, food especially in the world.Fusion-crystallization method has the feature of high efficiency, low energy consumption because of it, is used for widely preparing high purity product, because fusion-crystallization method is without introducing solvent, so application is a lot of in Chemical Manufacture, and will realize this method, must use melting crystallizer.US Patent No. 2659761 discloses a kind of fusion-crystallization method of purification, with the method supporting be a kind of tower crystallizer, tower body is divided into reflux section and crystallized region two parts; Reflux section is positioned at tower body top, and crystallized region is positioned at tower body bottom.Tower crystallizer is that material circulates in tower, crystallization and purification, and the feature of this technique is that crystallization rate is fast, purity is high; But device structure is complicated, fluctuation of service, easily fouling, floor space is large, separative efficiency is low.Application number is that 200510014193 patent discloses a kind of method of extracting 1-methyl naphthalene and 2-methyl naphthalene from tar, it utilizes isobutanol, methyl tertiary butyl ether, the tert-butyl alcohol etc. as alkylating agent, in solid or liquid acid or mixed acid, do under catalyst, make tar generation alkanisation polymerisation, then by three rectifying columns, isolate
-methyl naphthalene and
-methyl naphthalene product.Although the method less pollution, operation is very complicated, equipment operating is also very difficult.Publication number is the device that the patent of invention of CN1792406A discloses a kind of preparing high pure organic matter by fusion-crystallization method, and this device also exists the defects such as occupation area of equipment is large, technological parameter precision is high, complicated operation.
Summary of the invention
In order to solve, existing melting crystallizer floor space is large in the present invention, complicated operation and the low problem of separative efficiency, and a kind of melting crystallizer is provided.
The present invention adopts following technical scheme to realize: a kind of melting crystallizer, comprises housing, from case top, insert the liquid distribution trough in housing and be located in housing and with the rotation filler of drive unit; Between liquid distribution trough and rotation filler, leave gap; The top of housing has gas outlet; The bottom of housing has air inlet and liquid outlet; Housing overcoat has constant temperature jacket.During work, in advance mixture to be separated being put into heating furnace melts, the drive unit that starts rotation filler makes to rotate filler to start to rotate, by temperature in mixture to be separated gas between high-melting-point composition and the fusing point of low melting point composition in air inlet introducing housing, follow the mixture to be separated of melting on the rotation filler in liquid distribution trough is sent into housing, thereby being torn into superfine brin, drop, liquid film in rotation filler rotation process, mixture to be separated make the temperature of mixture to be separated cooling rapidly with the abundant contact heat-exchanging of gas in housing, in mixture to be separated like this, low melting point composition just flows out from the liquid outlet of housing bottom, and on the rotation filler that high-melting-point composition stays in housing, until low melting point composition from liquid outlet all flows out, temperature is introduced in housing from air inlet higher than the gas of high-melting-point congruent melting point in mixture to be separated, simultaneously in order to prevent that high-temperature gas and the external world from carrying out heat exchange and the temperature in housing is reduced, insulation jacket outside housing is passed into high-temperature heating medium, make housing inner chamber in stationary temperature, thereby by the high-melting-point composition melting remaining on rotation filler, by the drive unit of rotation filler, improve the rotating speed of rotation filler simultaneously, under the effect of rotary centrifugal force, the high-melting-point composition after melting is thrown in inner walls and is flowed out from liquid outlet, so just realized the separation of mixture.Described rotation filler is existing product; The drive unit of described rotation filler is the technology that those skilled in the art easily realize.
Further, described rotation filler is annular corrugated plating rotation filler, and the mixture to be separated of melting is more easily flowed out; The height that described liquid distribution trough stretches in housing is the 1/5-1/4 of housing inner chamber height, the height of described rotation filler is the 1/2-2/3 of housing inner chamber height, thereby makes the mixture to be separated of melting can radially arrive rotation filler maximum radius place and arrive vertically the rotation filler bottom with axial flow simultaneously after liquid distribution trough.
Product structure of the present invention is simple, cost is low, stable and separative efficiency is high, easy to operate, solved that existing melting crystallizer floor space is large, complicated operation and the low problem of separative efficiency, can be widely used in the obvious isomer of all fusing point differences, the organic separation of homologue.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention.
Fig. 2 is the structural representation (top view) of annular corrugated plating rotation filler.
In figure: 1-housing; 2-liquid distribution trough; 3-rotates filler; 4-gas outlet; 5-air inlet; 6-liquid outlet; 7-constant temperature jacket; 8-buncher.
The specific embodiment
, comprise housing 1, from housing 1 top, insert the liquid distribution trough 2 in housing 1 and be located in housing 1 and with the rotation filler 3 of drive unit; Between liquid distribution trough 2 and rotation filler 3, leave gap; The top of housing 1 has gas outlet 4; The bottom of housing 1 has air inlet 5 and liquid outlet 6; Housing 1 overcoat has constant temperature jacket 7.Described rotation filler 3 is annular corrugated plating rotation filler.The height that described liquid distribution trough 2 stretches in housing 1 is the 1/5-1/4 of housing 1 inner chamber height; The height of described rotation filler 3 is the 1/2-2/3 of housing 1 inner chamber height.
During concrete enforcement, as shown in Figure 1, the drive unit of described rotation filler 3 comprises the buncher 8 of being located at housing 1 below; The bottom of described housing 1 has centre bore; The output shaft of buncher 8 is fixed together with the bottom of rotation filler 3 through the centre bore of housing 1 bottom.During work, the output shaft driven rotary filler 3 of buncher 8 rotates.
3 specific embodiments while being below melting crystallizer work:
Embodiment 1: the purification of mixed dichlorobenzene multicomponent system
In mixed dichlorobenzene coarse crystal, each component is isomer; Wherein the mass percent of paracide is 60%, and all the other are o-dichlorohenzene and m-dichlorobenzene.Paracide is a kind of fine chemical product, is also a kind of very important raw material in organic synthesis.The physical property of each component of mixed dichlorobenzene coarse crystal is as shown in table 1 below:
Table 1
| ? | Fusing point ℃ | Boiling point ℃ |
| Paracide | 53.09 | 174 |
| M-dichlorobenzene | -24.8 | 173 |
| O-dichlorohenzene | -17 | 180 |
The heating furnace of in advance mixture to be separated being put into Temperature Setting and be 60 ℃ melts, and starts buncher 8 driven rotary fillers 3 and starts rotate and rotating speed is adjusted to 150rpm, and the air of 10 ℃ is introduced in housings 1 from air inlet 5; Follow the mixture to be separated of melting on the rotation filler 3 in liquid distribution trough 2 is sent into housing 1, thereby being torn into superfine brin, drop, liquid film in rotation filler 3 rotation processes, mixture to be separated with the abundant contact heat-exchanging of air in housing 1, the temperature of mixture to be separated is cooled to rapidly below 50 ℃, in mixture to be separated like this, low melting point composition o-dichlorohenzene and m-dichlorobenzene just flow out from liquid outlet 6, and on the rotation filler 3 that high-melting-point composition paracide stays in housing 1; Until low melting point composition o-dichlorohenzene and m-dichlorobenzene from liquid outlet 6 all flows out, the air of 100 ℃ is introduced in housing 1 from air inlet 5,7 pairs of housing 1 inner chambers of insulation jacket that simultaneously start outside housing 1 are incubated, thereby by the high-melting-point composition melting remaining on rotation filler 3, improve the rotating speed of buncher 8 to 400rpm simultaneously, under the effect of rotary centrifugal force, the high-melting-point composition paracide after melting is thrown on housing 1 inwall and flows out from liquid outlet 6, so just realized the separation of mixture.By analysis, the paracide purity 99.95% obtaining.In this example, the height that liquid distribution trough 2 stretches in housing 1 is 1/5 of housing 1 inner chamber height, and the height of rotation filler 3 is 1/2 of housing 1 inner chamber height.
Embodiment 2: the purification of acrylic acid-propionic acid bicomponent system
In acrylic acid-propionic acid mixture, acrylic acid mass percent is 75%.Acrylic acid is the raw material in a kind of important organic synthesis, and in synthetic acrylic acid, usually contains a small amount of accessory substance propionic acid, so want to prepare highly purified acrylic acid, needs propionic acid a small amount of in products of separated.In acrylic acid-propionic acid mixture, the physical property of the two is as shown in table 2 below:
Table 2
| ? | Fusing point ℃ | Boiling point ℃ |
| Propionic acid | -20.5 | 141.15 |
| Acrylic acid | 12.5 | 141 |
The heating furnace of in advance mixture to be separated being put into Temperature Setting and be 20 ℃ melts, and starts buncher 8 and makes to rotate filler 3 and starts rotate and rotating speed is adjusted to 120rpm, and the air of 0 ℃ is introduced in housings 1 from air inlet 5; Follow the mixture to be separated of melting on the rotation filler 3 in liquid distribution trough 2 is sent into housing 1, thereby being torn into superfine brin, drop, liquid film in rotation filler 3 rotation processes, mixture to be separated with the abundant contact heat-exchanging of air in housing 1, the temperature of mixture to be separated is cooled to rapidly below 5 ℃, in mixture to be separated like this, low melting point composition propionic acid just flows out from liquid outlet 6, and on the rotation filler 3 that high-melting-point composition acrylic acid stays in housing 1; Until low melting point composition propionic acid from liquid outlet 6 all flows out, the air of 25 ℃ is introduced in housing 1 from air inlet 5,7 pairs of housing 1 inner chambers of insulation jacket that simultaneously start outside housing 1 are incubated, thereby by the high-melting-point composition melting remaining on rotation filler 3, improve the rotating speed of buncher 8 to 350rpm simultaneously, under the effect of rotary centrifugal force, the high-melting-point composition acrylic acid after melting is thrown on housing 1 inwall and flows out from liquid outlet 6, so just realized the separation of mixture.By analysis, the acrylic acid purity 99.91% obtaining.In this example, the height that liquid distribution trough 2 stretches in housing 1 is 1/4 of housing 1 inner chamber height, and the height of rotation filler 3 is 2/3 of housing 1 inner chamber height.
Embodiment 3:
-methyl naphthalene and
the purification of-methyl naphthalene second-component system
-methyl naphthalene and
in-methyl naphthalene mixture
the mass fraction of-methyl naphthalene is 70%.Methyl naphthalene is a kind of very important Chemical Manufacture raw material, has two kinds of isomers:
-methyl naphthalene and
-methyl naphthalene, the physical property of the two is as shown in table 3 below.
Table 3
| ? | Fusing point | Boiling point |
| -methyl naphthalene | -30.46 | 244.69 |
 |
34.6 | 241.05 |
The heating furnace of in advance mixture to be separated being put into Temperature Setting and be 50 ℃ melts, and starts buncher 8 driven rotary fillers 3 and rotates also rotating speed is adjusted to 100rpm, and the nitrogen of 10 ℃ is introduced in housings 1 from air inlet 5; Follow the mixture to be separated of melting on the rotation filler 3 in liquid distribution trough 2 is sent into housing 1, thereby being torn into superfine brin, drop, liquid film in rotation filler 3 rotation processes, mixture to be separated with the abundant contact heat-exchanging of nitrogen in housing 1, the temperature of mixture to be separated is cooled to rapidly below 15 ℃, low melting point composition in mixture to be separated like this
-methyl naphthalene just flows out from liquid outlet 6, and high-melting-point composition
on the rotation filler 3 that-methyl naphthalene stays in housing 1; Treat low melting point composition
-methyl naphthalene is from liquid outlet 6 all flows out, the nitrogen of 60 ℃ is introduced in housing 1 from air inlet 5,7 pairs of housing 1 inner chambers of insulation jacket that simultaneously start outside housing 1 are incubated, thereby by the high-melting-point composition melting remaining on rotation filler 3, improve the rotating speed of buncher 8 to 300rpm simultaneously, under the effect of rotary centrifugal force by the high-melting-point composition after melting
-methyl naphthalene is thrown on housing 1 inwall and flows out from liquid outlet 6, has so just realized the separation of mixture.By analysis, obtain
-methyl naphthalene purity 99.97%.In this example, the height that liquid distribution trough 2 stretches in housing 1 is 1/5 of housing 1 inner chamber height, and the height of described rotation filler 3 is 2/3 of housing 1 inner chamber height.
Claims (2)
1. a melting crystallizer, it is characterized in that: comprise housing (1), insert the liquid distribution trough (2) in housing (1) and be located in housing (1) and with the rotation filler (3) of drive unit from housing (1) top, described rotation filler (3) rotates filler for annular corrugated plating; Between liquid distribution trough (2) and rotation filler (3), leave gap; The height that described liquid distribution trough (2) stretches in housing (1) is the 1/5-1/4 of housing (1) inner chamber height; The height of described rotation filler (3) is the 1/2-2/3 of housing (1) inner chamber height; The top of housing (1) has gas outlet (4); The bottom of housing (1) has air inlet (5) and liquid outlet (6); Housing (1) overcoat has constant temperature jacket (7).
2. melting crystallizer according to claim 1, is characterized in that: the drive unit of described rotation filler (3) comprises the buncher (8) of being located at housing (1) below; The bottom of described housing (1) has centre bore; The output shaft of buncher (8) is fixed together with the bottom of rotation filler (3) through the centre bore of housing (1) bottom.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110250841.4A CN102423542B (en) | 2011-08-29 | 2011-08-29 | Melt crystallizer |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110250841.4A CN102423542B (en) | 2011-08-29 | 2011-08-29 | Melt crystallizer |
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| CN102423542A CN102423542A (en) | 2012-04-25 |
| CN102423542B true CN102423542B (en) | 2014-02-12 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104826356B (en) * | 2015-03-17 | 2016-05-18 | 张建臣 | Liquid laminar flow crystallizer |
| CN104801059A (en) * | 2015-03-31 | 2015-07-29 | 北京普利玛科技有限责任公司 | Melt crystallizer |
| CN112062176A (en) * | 2020-08-19 | 2020-12-11 | 大连理工大学 | Porous medium non-fixed type seawater desalination device grown by using gas hydrate |
| CA3225766A1 (en) | 2021-07-23 | 2023-01-26 | Jian Zhang | Supramolecular amino acid or salt thereof, and preparation method therefor and application thereof |
| CN114656325B (en) * | 2022-04-15 | 2024-03-01 | 煤炭科学技术研究院有限公司 | Purification refining system and method for 2-methylnaphthalene |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU965449A1 (en) * | 1981-03-13 | 1982-10-15 | Предприятие П/Я Р-6273 | Roller type crystallizer |
| JP2004050147A (en) * | 2002-07-24 | 2004-02-19 | Satake Chemical Equipment Mfg Ltd | Crystal grain size controlling unit for crystallizer |
| CN201551868U (en) * | 2009-09-18 | 2010-08-18 | 天津渤海化工有限责任公司天津碱厂 | Ammonium sulfate crystallizer |
| CN102125795A (en) * | 2011-01-28 | 2011-07-20 | 中北大学 | Method and device for removing CO2 from conversion gas of synthetic ammonia |
| CN202191722U (en) * | 2011-08-29 | 2012-04-18 | 中北大学 | Melting crystallizer |
-
2011
- 2011-08-29 CN CN201110250841.4A patent/CN102423542B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU965449A1 (en) * | 1981-03-13 | 1982-10-15 | Предприятие П/Я Р-6273 | Roller type crystallizer |
| JP2004050147A (en) * | 2002-07-24 | 2004-02-19 | Satake Chemical Equipment Mfg Ltd | Crystal grain size controlling unit for crystallizer |
| CN201551868U (en) * | 2009-09-18 | 2010-08-18 | 天津渤海化工有限责任公司天津碱厂 | Ammonium sulfate crystallizer |
| CN102125795A (en) * | 2011-01-28 | 2011-07-20 | 中北大学 | Method and device for removing CO2 from conversion gas of synthetic ammonia |
| CN202191722U (en) * | 2011-08-29 | 2012-04-18 | 中北大学 | Melting crystallizer |
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Inventor after: Jiao Weizhou Inventor after: Liu Youzhi Inventor after: Yuan Zhiguo Inventor after: Qi Guisheng Inventor after: Li Xiuping Inventor after: Shen Hongyan Inventor after: Wang Jianwei Inventor after: Li Zhenxing Inventor before: Liu Youzhi Inventor before: Jiao Weizhou Inventor before: Yuan Zhiguo Inventor before: Qi Guisheng Inventor before: Li Xiuping Inventor before: Shen Hongyan Inventor before: Wang Jianwei Inventor before: Li Zhenxing |
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Free format text: CORRECT: INVENTOR; FROM: LIU YOUZHI JIAO WEIZHOU YUAN ZHIGUO QI GUISHENG LI XIUPING SHEN HONGYAN WANG JIANWEI LI ZHENXING TO: JIAO WEIZHOU LIU YOUZHI YUAN ZHIGUO QI GUISHENG LI XIUPING SHEN HONGYAN WANG JIANWEI LI ZHENXING |
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