CN104888492B - A kind of closed crystal system and chemicals purified crystals method - Google Patents
A kind of closed crystal system and chemicals purified crystals method Download PDFInfo
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- CN104888492B CN104888492B CN201510338284.XA CN201510338284A CN104888492B CN 104888492 B CN104888492 B CN 104888492B CN 201510338284 A CN201510338284 A CN 201510338284A CN 104888492 B CN104888492 B CN 104888492B
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Abstract
Closed crystal system disclosed by the invention, comprising: with the crystallization kettle of chuck, its upper cover is provided with gas access after hot acid mist gas vent, cooling；Blower fan, the entrance of blower fan connects hot acid mist gas vent by the first pipeline；Condenser, condenser has a hot acid gas access and cooling gas-liquid two-phase outlet, hot acid gas access and the outlet of blower fan；Cooling gas-liquid two-phase outlet connects by the 3rd pipeline with gas access after cooling；One freezing liquid trap, freezing liquid trap entrance and the connection of the 3rd pipeline.The method that this closed crystal system that invention additionally discloses is purified crystallization to chemicals.The whole crystallization process of the present invention be the most airtight in the case of carry out, it is to avoid with atmosphere reduce pollute, cooling gas be circulation work, relative energy consumption is relatively low, significantly reducing labour intensity, product appearance quality improves further simultaneously, and crystallization temperature can accurately be controlled at technique tolerance band.
Description
Technical field
The present invention relates to chemicals technical field of purification, particularly to a kind of closed crystal system and use
This closed crystal system is purified the method for crystallization to chemicals.
Background technology
When the fine chemicals that chemical reagent produces or batch yield is little produces, the solid high for obtaining purity
Product, all uses means re-crystallization to purify.Crystallization process uses different types of crystallizer, has band to press from both sides
Set or not jacketed still, having unlimited has airtight container etc..Generally with cooling medium to needing cooling
Material directly cool down, during this, owing to cooling medium is the most indirect with the material that need to cool down
The temperature difference touched is relatively big, and crystal moment bears and is easy to stick on still (container) wall, has an effect on heat transfer simultaneously
Effect, some equipment adds scraper plate and removes, and some is with manually rooting out, and its result changes material crystal shape,
Also have the block phenomenon of part, produce line clogging phenomenon when blowing separates, owing to operating environment is more sudden and more violent
Dew, easily causes secondary pollution, and labour intensity is bigger.
Summary of the invention
For the problems referred to above, one of the technical problem to be solved is to provide one to utilize air-cooled
But the closed crystal system that solution is cooled down by hot acid fog body in solution surface.
The two of the technical problem to be solved are to provide the above-mentioned closed crystal system of use to change
Product are purified the method for crystallization.
As the closed crystal system of first aspect present invention, including:
One with the crystallization kettle of chuck, described with on the upper cover of the crystallization kettle of chuck at least provided with one
Gas access install an agitator after hot acid mist gas vent, a cooling, should be with the crystallization kettle of chuck
Bottom be configured with baiting valve；
One blower fan, the entrance of described blower fan connects described hot acid mist gas vent by the first pipeline；
One condenser, described condenser has a hot acid gas access and cooling gas-liquid two-phase outlet, described
Hot acid gas access is by the second pipeline and the first control valve being connected on described second pipeline and blower fan
Outlet；The outlet of described cooling gas-liquid two-phase by the 3rd pipeline and is connected on described 3rd pipeline
Second control valve connects with gas access after described cooling；
One freezing liquid trap, described freezing liquid trap entrance connects with described 3rd pipeline.
In a preferred embodiment of the invention, described condenser is graphite pores block condenser.
In a preferred embodiment of the invention, after described cooling, the inside of gas access is configured with wind
Amount distribution apparatus.
Use above-mentioned closed crystal system as second aspect present invention is purified crystallization to chemicals
Method, it comprises the steps
(1) first the temperature of the crystallization kettle inwall with chuck is heated to and the chemicals needing purified crystals
Solution temperature is consistent；
(2) chemical solutions after concentration is placed in the crystallization kettle of chuck, stops crystallization, with
Exempt from crystal and be stained with wall；
(3) close the thermal source of the crystallization kettle with chuck, start agitator, the freezing liquid of open cold condenser
Turnover valve；Subsequent start-up blower fan, the chemical solutions upper end after concentrating in making the crystallization kettle with chuck
Hot acid fog body, under the effect of blower fan, is out sent to condenser by described hot acid mist gas vent cold
But, in the gas after cooling is again by after cooling, gas access enters the crystallization kettle with chuck, concentrating
After chemical solutions surface to solution cool down；
(4) when the chemical solutions after concentrating in the crystallization kettle with chuck is cooled to technological requirement, beat
Opening the baiting valve bottom the crystallization kettle with chuck, crystallization material is put into centrifuge and separates；During blowing, stirring turns
Speed answers full speed running, makes mother liquor stir with crystal, crystal can be avoided to be stained with wall in still by this kind of method.
In a preferred embodiment of the invention, in described step (4), if material crystal is had
In the case of requirement, agitator can be closed, until being as cold as when chilling temperature drops to and has crystallization
Technique assigned temperature, the crystalline solid so separated out is just basically identical with spontaneous nucleation.
Owing to have employed technical scheme as above, the whole crystallization process of the present invention be the most airtight in the case of
Carrying out, it is to avoid reduce with atmosphere and pollute, cooling gas is circulation work, and relative energy consumption is relatively low,
Significantly reducing labour intensity, product appearance quality improves further, and crystallization temperature can accurately be controlled simultaneously
At technique tolerance band.
Accompanying drawing explanation
Fig. 1 is the structural representation of closed crystal system of the present invention.
Detailed description of the invention
See Fig. 1, the closed crystal system be given in figure, including one with chuck crystallization kettle 100,
Blower fan 200, condenser 300 and freezing liquid trap 400.
With on the upper cover 110 of the crystallization kettle 100 of chuck at least provided with a hot acid mist gas vent
120, gas access 130 install an agitator 140 after a cooling, should be with the crystallization kettle 100 of chuck
Bottom be configured with baiting valve 150；Hot acid mist gas vent 120 is connected to blower fan 200 by pipeline 210
Entrance, the outlet of blower fan 200 is by pipeline 310 and the control valve 320 that is serially connected on pipeline 310 even
Receive the hot acid gas access 330 of condenser 300, the cooling gas-liquid two-phase outlet 340 of condenser 300
It is connected to the crystallization kettle 100 with chuck by pipeline 350 and the control valve 360 being connected on pipeline 350
Upper cover 110 on cooling after gas access 130.Freezing liquid trap 400 entrance is with pipeline 350 even
Logical.
Condenser 300 is additionally provided with freezing liquid import and export 370,380.
In order to improve cooling velocity, with chuck crystallization kettle 100 surface area condition permit under, be made
Larger, in gas access 130, configuration one air volume adjustment device (does not shows in figure the most after the cooling period
Go out) do air volume adjustment, make cooling surface contact surface increase and improve cooling effect.
If above-mentioned closed crystal system device crystallizes for stannous chloride, due to the production of stannous chloride
Material is acid medium, and the crystallization kettle 100 with chuck of the present invention uses glassed steel reaction vessels, condensation
Device 300 is graphite mould, and blower fan 200 and pipeline 210,310,350 are PP material.
The use above-mentioned closed crystal system of the present invention is described below in detail as a example by stannous chloride crystallizes
The method that stannous chloride is purified crystallization, the method comprises the steps
(1) first the temperature of crystallization kettle 100 inwall with chuck is heated to and the chlorine needing purified crystals
Change stannous solution temperature consistent；
(2) stannous chloride solution after concentration is placed in the crystallization kettle 100 of chuck, stops protochloride
Tin crystals separates out, in order to avoid stannous chloride crystal is stained with wall；
(3) close the thermal source of the crystallization kettle 100 with chuck, start agitator 140, open cold condenser
The freezing liquid turnover valve of 300；Subsequent start-up blower fan 200, after concentrating in making the crystallization kettle 100 with chuck
The hot acid fog body of stannous chloride solution upper end, under the effect of blower fan 200, hot acid fog body go out
Mouth 120 is out sent to condenser 300 and cools down, and the gas after cooling is again by gas access 130 after cooling
Entering in the crystallization kettle 100 with chuck, solution is cooled down by stannous chloride solution surface after concentration；
(4) stannous chloride solution after concentrating in the crystallization kettle 100 with chuck is cooled to technological requirement
Time, open the baiting valve 150 bottom the crystallization kettle 100 with chuck, stannous chloride crystallization material is put into centrifugal
Machine separates；During blowing, speed of agitator answers full speed running, makes mother liquor stir with stannous chloride crystal, with this kind
Method can avoid stannous chloride crystal to be stained with wall in still.
If in the case of stannous chloride crystal is required, can drop at chilling temperature and have stannous chloride
During crystallization, close agitator 140, until being as cold as technique assigned temperature, the stannous chloride so separated out
Crystalline solid is just basically identical with spontaneous nucleation.
Claims (4)
1. use the method that closed crystal system is purified crystallization to chemicals, described closed
Crystal system, including:
One with the crystallization kettle of chuck, described with on the upper cover of the crystallization kettle of chuck at least provided with one
Gas access install an agitator after hot acid mist gas vent, a cooling, should be with the crystallization kettle of chuck
Bottom be configured with baiting valve；
One blower fan, the entrance of described blower fan connects described hot acid mist gas vent by the first pipeline；
One condenser, described condenser has a hot acid gas access and cooling gas-liquid two-phase outlet, described
Hot acid gas access is by the second pipeline and the first control valve being connected on described second pipeline and blower fan
Outlet；The outlet of described cooling gas-liquid two-phase by the 3rd pipeline and is connected on described 3rd pipeline
Second control valve connects with gas access after described cooling；
One freezing liquid trap, described freezing liquid trap entrance connects with described 3rd pipeline；
It is characterized in that, described use closed crystal system is purified the method bag of crystallization to chemicals
Include following steps:
(1) first the temperature of the crystallization kettle inwall with chuck is heated to and the chemicals needing purified crystals
Solution temperature is consistent；
(2) chemical solutions after concentration is placed in the crystallization kettle of chuck, stops crystallization, with
Exempt from crystal and be stained with wall；
(3) close the thermal source of the crystallization kettle with chuck, start agitator, the freezing liquid of open cold condenser
Turnover valve；Subsequent start-up blower fan, the chemical solutions upper end after concentrating in making the crystallization kettle with chuck
Hot acid fog body, under the effect of blower fan, is out sent to condenser by described hot acid mist gas vent cold
But, in the gas after cooling is again by after cooling, gas access enters the crystallization kettle with chuck, concentrating
After chemical solutions surface to solution cool down；
(4) when the chemical solutions after concentrating in the crystallization kettle with chuck is cooled to technological requirement, beat
Opening the baiting valve bottom the crystallization kettle with chuck, crystallization material is put into centrifuge and separates；During blowing, stirring turns
Speed answers full speed running, makes mother liquor stir with crystal, crystal can be avoided to be stained with wall in still by this kind of method.
2. the method for claim 1, it is characterised in that in described step (4), if right
In the case of material crystal requires, agitator can be closed when chilling temperature drops to and has crystallization,
Until being as cold as technique assigned temperature, the crystalline solid so separated out is just basically identical with spontaneous nucleation.
3. the method for claim 1, it is characterised in that described condenser is the condensation of graphite pores block
Device.
4. the method for claim 1, it is characterised in that after described cooling in gas access
Portion is configured with air volume adjustment device.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510338284.XA CN104888492B (en) | 2015-06-17 | 2015-06-17 | A kind of closed crystal system and chemicals purified crystals method |
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| CN201510338284.XA CN104888492B (en) | 2015-06-17 | 2015-06-17 | A kind of closed crystal system and chemicals purified crystals method |
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| CN104888492B true CN104888492B (en) | 2016-09-07 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202822846U (en) * | 2012-07-20 | 2013-03-27 | 江苏南天农科化工有限公司 | Acrylamide crystal equipment |
| CN203494209U (en) * | 2013-07-30 | 2014-03-26 | 旭阳化学技术研究院有限公司 | Vacuum evaporative crystallization device of dihydroxy acetone aqueous solution |
| CN204767573U (en) * | 2015-06-17 | 2015-11-18 | 上海试四赫维化工有限公司 | Closed crystal system |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10156102A (en) * | 1996-11-28 | 1998-06-16 | Kashimakita Kyodo Hatsuden Kk | Continuous crystallization method |
| JP2004216331A (en) * | 2003-01-17 | 2004-08-05 | Mitsubishi Chemicals Corp | Method of and apparatus for crystallizing aromatic carboxylic acid |
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2015
- 2015-06-17 CN CN201510338284.XA patent/CN104888492B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202822846U (en) * | 2012-07-20 | 2013-03-27 | 江苏南天农科化工有限公司 | Acrylamide crystal equipment |
| CN203494209U (en) * | 2013-07-30 | 2014-03-26 | 旭阳化学技术研究院有限公司 | Vacuum evaporative crystallization device of dihydroxy acetone aqueous solution |
| CN204767573U (en) * | 2015-06-17 | 2015-11-18 | 上海试四赫维化工有限公司 | Closed crystal system |
Non-Patent Citations (1)
| Title |
|---|
| 氯化亚锡结晶工艺技术改造;曾文;《大众科技》;20120428(第1期);第126-127页 * |
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