CN108992965A - A kind of uniform one is hydrated sodium hypophosphite bulky grain Continuous Cooling Crystallization preparation process and device - Google Patents
A kind of uniform one is hydrated sodium hypophosphite bulky grain Continuous Cooling Crystallization preparation process and device Download PDFInfo
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- CN108992965A CN108992965A CN201810940749.2A CN201810940749A CN108992965A CN 108992965 A CN108992965 A CN 108992965A CN 201810940749 A CN201810940749 A CN 201810940749A CN 108992965 A CN108992965 A CN 108992965A
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Abstract
The invention discloses an a kind of uniform hydration sodium hypophosphite bulky grain Continuous Cooling Crystallization preparation process and devices.The technique is that material liquid is transferred to Continuous Cooling Crystallization device, after liquid level reaches requirement, open stirring, circulating pump, recirculated cooling water etc., slow cooling, when solution temperature is before crystal point out, a hydration sodium hypophosphite crystal seed is added, continue slow cooling, until temperature is down to outlet temperature, mother liquor as continuous crystallisation, continue transferring raw material liquid to Continuous Cooling Crystallization device, one hydration sodium hypophosphite magma is continuously delivered to concentrate transfer tank by magma pump, control crystal growth time, then centrifuge separation, washing, it is dried to obtain uniform hydration sodium hypophosphite grain products, external circulation heat exchanging device is used to carry out heat exchange to maintain the temperature of crystal system to stablize.There is the present invention preparation large grained one of continuous-stable to be hydrated sodium hypophosphite product, even particle size distribution, the high effect of product purity.
Description
Technical field
The present invention relates to the stability techniques fields of solubility object system's Continuous Cooling Crystallization operation, in particular to a kind of uniform
One hydration sodium hypophosphite bulky grain Continuous Cooling Crystallization preparation process and device.
Background technique
One hydration sodium hypophosphite, molecular formula NaH2PO2·H2O, molecular weight 105.99, crystalline density 1.388g/cm3, readily soluble
Yu Shui, glycerol, alcohol, do not dissolve in ether, and aqueous solution is in neutrality.At 25 DEG C, solubility in water is 100g/100g water,
Solubility is 667g/100g water at 100 DEG C.
Sodium hypophosphite is mainly used for chemical deposit.Make workpiece surface that nature catalysis occur also using the strong reducing property of this product
Original reaction, in one phosphorus amorphous alloy of workpiece surface plated nickel.After having this coating, workpiece surface hardware is resistance to up to HV850 or more
Mill property greatly improves, and because coating is amorphous state, imporosity, therefore chemical resistance is splendid, and coating surface is glossy, therefore can plate
On ornament.It is suitable for complex-shaped metal and is coated with, and is especially suitable for nonmetal parts and is coated with, and is easy to use.
When the crystallization process of current hydration sodium hypophosphite is by being concentrated into 46-49Be ° by the feed liquid handled well, send
Entering periodic crystallisation kettle (cooling jacket or built-in cooling coil) and carries out crystallisation by cooling, refrigerant is recirculated cooling water, the one of advantages of good crystallization
Hydration sodium hypophosphite by drying to obtain finished product and is packed after centrifuge is separated off mother liquor.
Traditional batch crystallisation by cooling process scabs there are heat exchange interface influences the heat exchange efficiency in later period, secondly because interval is cold
But the wider distribution of product crystal granularity, a hydration of certain chemical company caused by the degree of supersaturation control of crystallization process is more difficult
The Granularity Distribution of sodium hypophosphite is as follows:
| Sieve (mesh) | <20 | 20~30 | 30~40 | 40~60 | 60~80 | >80 |
| Mass fraction | 0.153 | 0.32 | 0.28 | 0.136 | 0.078 | 0.033 |
State Behavior of Continuous Crystallization Processes is relative to periodic crystallisation with product granularity is uniform, stability is high, equipment takes up little area, automates
The outstanding advantages such as controlling extent is high, energy efficiency is high, cost of labor is low, are particularly suitable for being mass produced.Continuous crystalizer
Operation has following items requirement: controlling satisfactory Granularity Distribution；Crystallizer has production intensity as high as possible；To the greatest extent
Amount reduces the rate of crystalline scale, to extend the period of crystallizer normal operation；Maintain the stability of crystallizer.
Stability and controllability are the key that continuous crystallizing systems, and degree of supersaturation is the core of crystallization process, nucleation speed
Rate, the second process such as crystal growth rate, aggregation are all closely related with degree of supersaturation,
However, this system, in state Behavior of Continuous Crystallization Processes, there are some particular difficulties, so that a hydration sodium hypophosphite is continuous
Crystallization processes are difficult to realize to be stablized, and causes product also much not as good as the product of periodic crystallisation.From macroscopic perspective, the reason is that
The solubility of sodium hypophosphite in water is very high, cause 1. material liquid density it is high ,~48Be ° when, density reaches 1500kg/m3, knot
The density of brilliant post mother liquor is about 1370kg/m3, and the density of a hydration sodium hypophosphite crystal is 1388kg/m3, the density contrast of the two
It is minimum, cause particle settling rates very slow, can not achieve for DTB, OSLO etc. efficiently continuous crystalizer and divide well
Grade effect；2. the viscosity of feed liquid is high, the crystalline content in crystalline mother solution reaches 50% or more (1m3Material liquid can crystallize generation
700kg crystal), the viscosity of suspension magma will increase dramatically, and it is totally unfavorable to the growth of crystal, before strict control nucleus quantity
It puts, the crystal growth time for needing to grow very much, if bad at nuclear control, will lead to magma and deteriorate into milk shape slurries, crystal
Chance is difficult to grow (as shown in Figure 1), and high viscosity crystallization process, trace impurity are readily adsorbed in plane of crystal, it is not easy to
It is washed clean, influence the purity of product.The microscopic reason for above-mentioned phenomenon occur is, sodium hypophosphite in aqueous solution with moisture
Son forms very strong hydrogen bond action, and this hydrogen bond action, results in high-dissolvability, and then it is high, viscous to result in solution density
High macroscopic appearance is spent, hydrogen bond action how is weakened, reducing viscosity is the key that realize steady and continuous crystallization.
One hydration sodium hypophosphite belongs to sticky physical property in the crystallization of aqueous solution, grows crystallization process slowly, and the country does not have also at present
There is the relevant report of continuous crystallisation, for dope crystallizing system, is continuously tied frequently with the lower horizontal more locellus of production efficiency
Brilliant device or tower continuous crystalizer etc., the crystal growth residence time generally requires tens hours, and DTB, OSLO etc. efficiently connect
Continuous crystallizer cannot then stablize use.
Summary of the invention
One or more to solve the above-mentioned problems, the present invention provides a kind of uniform hydration sodium hypophosphite bulky grains
Continuous Cooling Crystallization preparation process and device.
The uniform hydration sodium hypophosphite bulky grain Continuous Cooling Crystallization preparation process of the one kind, comprising the following steps: will be secondary
Concentration flow container is added in sodium radio-phosphate,P-32 solution, carries out the concentrate that concentration forms 85 DEG C~95 DEG C, a certain proportion of reduction is then added
Bonding solvents form material liquid；
Material liquid is input to Continuous Cooling Crystallization device by the first delivery pump, after liquid level reaches requirement, is opened continuous
Mixing part, circulating pump and recirculated cooling water of equipment of crystallisation by cooling etc., slow cooling, rate of temperature fall is 2~5 DEG C/h, when molten
At 1~3 DEG C, a hydration sodium hypophosphite crystal seed is added before crystal point out in liquid temperature, continues slow cooling, and rate of temperature fall is 3~8
DEG C/h, and until temperature is down to 40~45 DEG C, the mother liquor as continuous crystallisation；
First delivery pump continues even speed and material liquid is continuously conveyed to Continuous Cooling Crystallization device, and magma pumps continuously by one
Hydration sodium hypophosphite magma is delivered to magma transfer tank, wherein Continuous Cooling Crystallization device uses outer circulation tubular heat exchanger
Heat exchange is carried out to maintain the temperature of crystal system to stablize, in Continuous Cooling Crystallization device, macroscopical crystal growth residence time is controlled
System is in 2~8h；
The magma of magma transfer tank processing continuously enters centrifuge, and magma is by centrifuge centrifuge separation, washing, dry
To uniform hydration sodium hypophosphite bulky grain product.
In some embodiments, 46-48Be ° of the Baume degrees of concentrate, solution density 1420-1500kg/m3。
In some embodiments, the temperature of concentrate is 90 DEG C.
In some embodiments, reduction bonding solvents be nonaqueous solvents, reduction bonding solvents be methanol, ethyl alcohol, propyl alcohol,
One or more of isopropanol.
In some embodiments, the volume ratio for weakening bonding solvents and sodium hypophosphite solution is 1:3~1:10.
In some embodiments, in Continuous Cooling Crystallization device, macroscopical crystal growth residence time is 3~6h.
In some embodiments, in the clear mother liquor discharge port of magma transfer tank and centrifuge centrifuge mother liquor discharge port
Place, a part of mother liquor return to concentration flow container, and it is close to reduce internal magma suspension that a part of mother liquor returns to Continuous Cooling Crystallization device
Degree, magma suspension density are controlled in 300~500kg/m3Magma.
In some embodiments, magma suspension density is 400~500kg/m3Magma.
In some embodiments, the granularity of a hydration sodium hypophosphite crystal seed is about 0.1~0.3mm, and additional amount is 5~
20‰。
The present invention provides efficient, the steady and continuous cooling and crystallizing process skills of a kind of uniform hydration sodium hypophosphite bulky grain
Art, the present invention has the beneficial effect that compared with prior art first, this technique is suitable for the sticky material of slow crystal growth
System, it is 0.6~1.2mm and hydration sodium hypophosphite crystal (10~40 mesh crystal of graininess one of even particle size distribution that granularity, which is made,
90%) accounting is greater than.Compared with prior art and patent of invention, there is process to stablize, do not occur milk shape phenomenon, a product
The advantages that purity is high, monodisperse, good fluidity, storage and transportational process are not agglomerated.
According to an aspect of the present invention, a kind of uniform hydration sodium hypophosphite bulky grain Continuous Cooling Crystallization is additionally provided
Preparation facilities, including concentration flow container, flow control valve, the first delivery pump, Continuous Cooling Crystallization device, magma pump, magma transfer
Tank and centrifuge,
The import of concentration flow container, flow control valve and the first delivery pump is sequentially connected by pipeline,
The outlet of first delivery pump is connected to the feeding inlet of Continuous Cooling Crystallization device, Continuous Cooling Crystallization device by pipeline
Discharge port by pipeline be connected to magma pump import, magma pump outlet by pipeline be connected to magma transfer tank upper end, crystalline substance
The magma discharge port for starching transfer tank is connected to centrifuge, and the outlet for product of centrifuge obtains hydration sodium hypophosphite bulky grain production
Product,
The clear mother liquor discharge port of magma transfer tank is connected to the centrifuge mother liquor discharge port of centrifuge by pipeline, and passes through pipe
Line a part returns to Continuous Cooling Crystallization device, and a part is back to concentration flow container.
Continuous Cooling Crystallization device is DTB Continuous Cooling Crystallization device or OSLO Continuous Cooling Crystallization device.The present invention with
The prior art is simple with structure compared to the present invention is had the beneficial effect that, operates control convenient and easy to automate
The advantages that.
Detailed description of the invention
Fig. 1 is the photo of the milk shape slurries of the prior art；
Fig. 2 is the process of the Continuous Cooling Crystallization preparation process of a hydration sodium hypophosphite particle of an embodiment of the present invention
Schematic diagram；
Fig. 3 is the photo of a hydration sodium hypophosphite product prepared by the embodiment of the present invention 1；
Fig. 4 is the photo of a hydration sodium hypophosphite product prepared by the embodiment of the present invention 2；
Fig. 5 is the photo of a hydration sodium hypophosphite product prepared by the embodiment of the present invention 3；
Table 1 is the particle size distribution data (screening) of a hydration sodium hypophosphite product prepared by the embodiment of the present invention 1；
Table 2 is the particle size distribution data (screening) of a hydration sodium hypophosphite product prepared by the embodiment of the present invention 2；
Table 3 is the particle size distribution data (screening) of a hydration sodium hypophosphite product prepared by the embodiment of the present invention 3.
Specific embodiment
With reference to the accompanying drawing and specific embodiment the present invention is described in further detail.
Embodiment 1
Concentration flow container 1 is added in sodium hypophosphite solution, concentration is carried out and forms concentrate, the temperature of concentrate is 90 DEG C, dense
The concentration of contracting liquid is~48Be ° (Baume degrees), and the solution density of concentrate is 1500kg/m3,
Bonding solvents (ethyl alcohol) will be weakened according to 1:4 (volume ratio, VSolvent: VSodium hypophosphite solution) concentrate is added, form material liquid；
Material liquid is inputted into Continuous Cooling Crystallization device 4 through the first delivery pump 3, after liquid level reaches requirement, opens stirring
Paddle 41, outer circulation pump 42 and recirculated water, slow cooling, rate of temperature fall are 4 DEG C/h, (are approximately higher than when solution temperature reaches 80 DEG C
2 DEG C of crystal point out), a hydration sodium hypophosphite crystal seed is added, granularity is about 0.25mm (60~65 mesh), and additional amount is 15 ‰, is continued
Cooling, rate of temperature fall are 5 DEG C/h, until temperature is down to~45 DEG C, form mother liquor；
Material liquid is continuously conveyed to Continuous Cooling Crystallization device 4 with the first delivery pump 3, magma pump 5 is continuously by a water
It closing sodium hypophosphite magma and is delivered to magma transfer tank 6, macroscopical crystal growth time of Continuous Cooling Crystallization device 4 is controlled in 4h,
It is centrifugated, washs through centrifuge 7 after, being dried to obtain uniform hydration sodium hypophosphite grain products, a part of mother liquor returns
It is back to concentration flow container 1, a part of centrifuge mother liquor returns to Continuous Cooling Crystallization device 4 to reduce magma suspension density, and magma suspends
Density domination is in~450kg/m3Magma, Continuous Cooling Crystallization device use outer circulation tubular heat exchanger to carry out heat exchange to tie up
The temperature for holding crystal system is stablized.
In the embodiment, a hydration sodium hypophosphite product form is as shown in figure 3, the granularity of a hydration sodium hypophosphite product is divided
See Table 1 for details for cloth data, average particle size 0.95mm, 10~40 mesh crystal accountings 92.5%.
Embodiment 2
Concentration flow container 1 is added in sodium hypophosphite solution, concentration is carried out and forms concentrate, the temperature of concentrate is 90 DEG C, dense
The concentration of contracting liquid is~47Be ° (Baume degrees), and the solution density of concentrate is 1460kg/m3,
Bonding solvents (methanol) will be weakened according to 1:9 (volume ratio, VSolvent: VSodium hypophosphite solution) concentrate is added, form material liquid；
Material liquid is inputted into Continuous Cooling Crystallization device 4 through the first delivery pump 3, after liquid level reaches requirement, opens stirring
Paddle 41, outer circulation pump 42 and recirculated water, slow cooling, rate of temperature fall are 4 DEG C/h, (are approximately higher than when solution temperature reaches 80 DEG C
2 DEG C of crystal point out), a hydration sodium hypophosphite crystal seed is added, granularity is about 0.25mm (60~65 mesh), and additional amount is 20 ‰, is continued
Cooling, rate of temperature fall are 4 DEG C/h, until temperature is down to~45 DEG C, form mother liquor；
Material liquid is continuously conveyed to Continuous Cooling Crystallization device 4 with the first delivery pump 3, magma pump 5 is continuously by a water
It closes sodium hypophosphite magma and is delivered to magma transfer tank 6, the crystal growth time of Continuous Cooling Crystallization device 4 is controlled in 3h, then
It is centrifugated, washs through centrifuge 7, being dried to obtain uniform hydration sodium hypophosphite grain products, a part of mother liquor is back to
Flow container 1 is concentrated, a part of centrifuge mother liquor returns to Continuous Cooling Crystallization device 4 to reduce magma suspension density, magma suspension density
Control is in~500kg/m3Magma, Continuous Cooling Crystallization device 4 use outer circulation tubular heat exchanger to carry out heat exchange to maintain
The temperature of crystal system is stablized.
In the embodiment, a hydration sodium hypophosphite product form is as shown in figure 4, the granularity of a hydration sodium hypophosphite product is divided
See Table 2 for details for cloth data, and the average particle size of a hydration sodium hypophosphite product is 0.9mm, 10~40 mesh crystal accountings 91.3%.
Embodiment 3
Concentration flow container 1 is added in sodium hypophosphite solution, concentration is carried out and forms concentrate, the temperature of concentrate is 90 DEG C, dense
The concentration of contracting liquid is~46Be ° (Baume degrees), and the solution density of concentrate is 1420kg/m3,
Bonding solvents (isopropanol) will be weakened according to 1:3 (volume ratio, VSolvent: VSodium hypophosphite solution) concentrate is added, form raw material
Liquid；
Material liquid is inputted into Continuous Cooling Crystallization device 4 through the first delivery pump 3, after liquid level reaches requirement, opens stirring
Paddle 41, outer circulation pump 42 and recirculated water, slow cooling, rate of temperature fall are 5 DEG C/h, (are approximately higher than when solution temperature reaches 80 DEG C
2 DEG C of crystal point out), a hydration sodium hypophosphite crystal seed is added, granularity is about 0.25mm (60~65 mesh), and additional amount is 12 ‰, is continued
Cooling, rate of temperature fall are 5 DEG C/h, until temperature is down to~45 DEG C, form mother liquor；
Material liquid is continuously conveyed to Continuous Cooling Crystallization device 4 with the first delivery pump 3, magma pump 5 is continuously by a water
It closes sodium hypophosphite magma and is delivered to magma transfer tank 6, the crystal growth time of Continuous Cooling Crystallization device 4 is controlled in 6h, then
It is centrifugated, washs through centrifuge 7, being dried to obtain uniform hydration sodium hypophosphite grain products, a part of mother liquor is back to
Flow container 1 is concentrated, a part of centrifuge mother liquor returns to Continuous Cooling Crystallization device 4 to reduce magma suspension density, magma suspension density
Control is in~400kg/m3Magma, Continuous Cooling Crystallization device 4 use outer circulation tubular heat exchanger to carry out heat exchange to maintain
The temperature of crystal system is stablized.
In the embodiment, a hydration sodium hypophosphite product form is as shown in figure 5, the granularity of a hydration sodium hypophosphite product is divided
See Table 3 for details for cloth data, and the average particle size of a hydration sodium hypophosphite product is 0.85mm, 10~40 mesh crystal accountings 90.5%.
Above-described is only some embodiments of the present invention.For those of ordinary skill in the art, not
Under the premise of being detached from the invention design, various modifications and improvements can be made, these belong to protection model of the invention
It encloses.
Claims (10)
1. a kind of uniform hydration sodium hypophosphite bulky grain Continuous Cooling Crystallization preparation process, which is characterized in that including following step
It is rapid:
Concentration flow container (1) is added in sodium hypophosphite solution, carries out the concentrate that concentration forms 85 DEG C~95 DEG C, is then added certain
The reduction bonding solvents of ratio form material liquid；
The material liquid is input to Continuous Cooling Crystallization device (4) by the first delivery pump (3) to open after liquid level reaches requirement
Open mixing part (41), circulating pump (42) and the recirculated cooling water etc. of the Continuous Cooling Crystallization device (4), slow cooling, drop
Warm rate is 2~5 DEG C/h, when 1~3 DEG C before crystal point out of solution temperature, a hydration sodium hypophosphite crystal seed is added, continues slow
Cooling, rate of temperature fall is 3~8 DEG C/h, until temperature is down to 40~45 DEG C, the mother liquor as continuous crystallisation；
First delivery pump (3) continues even speed and the material liquid is continuously conveyed to the Continuous Cooling Crystallization device (4),
One hydration sodium hypophosphite magma is continuously delivered to magma transfer tank (6) by magma pump (5), wherein the Continuous Cooling Crystallization dress
Setting (4) uses the progress heat exchange of outer circulation tubular heat exchanger to maintain the temperature of crystal system to stablize, the continuous coo1ing knot
In brilliant device (4), macroscopical crystal growth residence time control is in 2~8h；
The magma of magma transfer tank (6) processing continuously enters centrifuge (7), and magma is by the centrifuge (7) centrifugation point
From, wash, be dried to obtain it is uniform one hydration sodium hypophosphite bulky grain product.
2. the uniform hydration sodium hypophosphite bulky grain Continuous Cooling Crystallization preparation process of one kind according to claim 1,
It is characterized in that, 46-48Be ° of the Baume degrees of the concentrate, solution density 1420-1500kg/m3。
3. the uniform hydration sodium hypophosphite bulky grain Continuous Cooling Crystallization preparation process of one kind according to claim 1,
It is characterized in that, the temperature of the concentrate is 90 DEG C.
4. the uniform hydration sodium hypophosphite bulky grain Continuous Cooling Crystallization preparation process of one kind according to claim 1,
It is characterized in that, the reduction bonding solvents are nonaqueous solvents, and the reduction bonding solvents are methanol, in ethyl alcohol, propyl alcohol, isopropanol
One or more.
5. the uniform hydration sodium hypophosphite bulky grain Continuous Cooling Crystallization preparation process of one kind according to claim 1,
It is characterized in that, the volume ratio of the reduction bonding solvents and the sodium hypophosphite solution is 1:3~1:10.
6. the uniform hydration sodium hypophosphite bulky grain Continuous Cooling Crystallization preparation process of one kind according to claim 1,
It is characterized in that, in the Continuous Cooling Crystallization device (4), the macroscopic view crystal growth residence time is 3~6h.
7. the uniform hydration sodium hypophosphite bulky grain Continuous Cooling Crystallization preparation process of one kind according to claim 1,
It is characterized in that, in the clear mother liquor discharge port and the centrifuge (7) centrifuge mother liquor discharge outlet of the magma transfer tank (6),
A part of mother liquor returns to the concentration flow container (1), and a part of mother liquor returns to the Continuous Cooling Crystallization device (4) to reduce inside
Magma suspension density, magma suspension density are controlled in 300~500kg/m3Magma.
8. the uniform hydration sodium hypophosphite bulky grain Continuous Cooling Crystallization preparation process of one kind according to claim 1,
It is characterized in that, the magma suspension density is 400~500kg/m3Magma.
9. the uniform hydration sodium hypophosphite bulky grain Continuous Cooling Crystallization preparation process of one kind according to claim 1,
It is characterized in that, the granularity of the hydration sodium hypophosphite crystal seed is about 0.1~0.3mm, and additional amount is 5~20 ‰.
10. a kind of uniform hydration sodium hypophosphite bulky grain Continuous Cooling Crystallization preparation facilities, which is characterized in that including concentrate
Tank (1), flow control valve (2), the first delivery pump (3), Continuous Cooling Crystallization device (4), magma pump (5), magma transfer tank (6)
And centrifuge (7),
The import of concentration flow container (1), the flow control valve (2) and first delivery pump (3) passes through pipeline successively
Connection,
The outlet of first delivery pump (3) is connected to the feeding inlet of the Continuous Cooling Crystallization device (4), the company by pipeline
The discharge port of continuous equipment of crystallisation by cooling (4) is connected to the import of the magma pump (5), the outlet of the magma pump (5) by pipeline
The upper end of the magma transfer tank (6) is connected to by pipeline, the magma discharge port of the magma transfer tank (6) is connected to the centrifugation
Machine (7), the outlet for product of the centrifuge (7) obtain a hydration sodium hypophosphite bulky grain product,
The clear mother liquor discharge port of the magma transfer tank (6) and the centrifuge mother liquor discharge port of the centrifuge (7) are connected by pipeline
It is logical, and the Continuous Cooling Crystallization device (4) is returned to by pipeline a part, a part is back to the concentration flow container (1).
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| CN110052075A (en) * | 2019-06-05 | 2019-07-26 | 太仓塑料助剂厂有限公司 | The separation method and system of cumyl peroxide |
| CN111514604A (en) * | 2020-04-17 | 2020-08-11 | 深圳大学 | Method for preparing high-purity crystal by fractional evaporation crystallization |
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| CN105236439A (en) * | 2015-09-07 | 2016-01-13 | 成都程德化工科技有限责任公司 | Large-granular boric acid, continuously cooling recrystallization preparation process and continuously cooling recrystallization preparation method thereof |
| EP3228599A1 (en) * | 2016-04-08 | 2017-10-11 | Eliquo Stulz GmbH | Device and method for the extraction of phosphorus from waste water |
| CN106395777A (en) * | 2016-08-30 | 2017-02-15 | 湖北永绍科技股份有限公司 | Comprehensive utilization method of phosphoric acid waste liquid |
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| CN110052075A (en) * | 2019-06-05 | 2019-07-26 | 太仓塑料助剂厂有限公司 | The separation method and system of cumyl peroxide |
| CN111514604A (en) * | 2020-04-17 | 2020-08-11 | 深圳大学 | Method for preparing high-purity crystal by fractional evaporation crystallization |
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