CN205182237U - Crystal system - Google Patents

Crystal system Download PDF

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Publication number
CN205182237U
CN205182237U CN201520975011.1U CN201520975011U CN205182237U CN 205182237 U CN205182237 U CN 205182237U CN 201520975011 U CN201520975011 U CN 201520975011U CN 205182237 U CN205182237 U CN 205182237U
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China
Prior art keywords
storage device
tank
coil
crystallization apparatus
crystal system
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CN201520975011.1U
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Chinese (zh)
Inventor
张长春
钱丽娜
刘大鹏
崔健
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Sino Us Huashitong Biomedical Technology Wuhan Co ltd
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Waterstone Pharmaceuticals Wuhan Co Ltd
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Abstract

The utility model discloses a crystal system, include: crystallization device, sample storage device, first solvent storage device, second solvent storage device and motor, the crystallization device is by compriseing the jar body, tank deck and tank bottoms, and a jar external wall has a temperature control components, and at least one feed inlet has been offered to the tank deck, jar internal and be provided with the two layer filtering device near tank bottoms department, and at least one discharge gate has been offered to the tank bottoms, the first feed inlet that sample storage device passes through the tank deck links to each other with the crystallization device, the second feed inlet that first solvent storage device passes through the tank deck links to each other with the crystallization device, third feed inlet and crystallization device that second solvent storage device passes through the tank deck link to each other, the motor is connected with faciola form screw propeller blade. Utilizing this system, can carrying out ration, constant speed, efficient crystallization and screening to the sample, the operation is very convenient, and can guarantee crystal quality, and crystallization technological parameter also is convenient for confirm by on the other hand.

Description

Crystal system
Technical field
The utility model belongs to medicine synthesis technique apparatus field, concrete, relates to a kind of crystal system.
Background technology
Crystallization belongs to the conventional operating procedure in pharmaceutical synthesis field, can obtain highly purified product by crystallization, and drug-specific crystal formation directly can affect follow-up preparation process and play a crucial role for drug effect performance.But the crystallization operation of laboratory stage conventional at present carries out usually in uncovered beaker, focuses on screening recrystallisation solvent, and very not strict for the control of Crystallization Process parameter.And well known to a person skilled in the art and be, the process that solute is separated out from solution based on crystallization, nucleus can be divided into generate (nucleation) and two stages of crystal growth, need the regular hour, except having screening to recrystallisation solvent, procedure parameter for operations step all needs to control, and this is also conducive to obtaining target crystal formation.
Therefore, be existingly suitable for screening the crystal system that obtains specific products crystal formation and method for crystallising is further improved.
Utility model content
The utility model is intended to solve at least to a certain extent one of technical problem existed in prior art or at least provides a kind of useful business to select.For this reason, an object of the present utility model is that providing a kind of is suitable for screening the crystal system and method for crystallising that obtain specific products crystal formation, utilize this system, can carry out quantitatively sample, constant speed, efficiently crystallization and screening, easy to operate, and can crystalline quality be ensured, on the other hand, be also convenient to determine crystallization processes parameter.
For this reason, in the first aspect of utility model, the utility model proposes a kind of crystal system.According to embodiment of the present utility model, this system comprises:
Crystallization apparatus, described crystallization apparatus forms by the bottom of tank body, tank deck and tank, and described tank wall has temperature control assembly, and described tank deck offers at least one charging aperture, described tank body is interior and close tank bottom is provided with two-layer filter, offers at least one discharging opening at the bottom of described tank;
Sample storage device, described sample storage device is connected with described crystallization apparatus by the first charging aperture of described tank deck;
First solvent storage device, described first solvent storage device is connected with described crystallization apparatus by the second charging aperture of described tank deck, and the first solvent storage device has first flow control device;
Second solvent storage device, described second solvent storage device is connected with described crystallization apparatus by the 3rd charging aperture of tank deck, and the second solvent storage device has second amount control device; And
Motor, described motor is connected with faciola shape propeller blade, and described faciola shape propeller blade is arranged in the tank body of described crystallization apparatus, and can move up and down along tank body.
Inventor is surprised to find, crystal system of the present utility model is suitable for screening and obtains specific products crystal formation, thus, utilize this crystal system, can quantitatively, constant speed, realize treating the process of crystallized sample efficiently, and be convenient to grope, determine the kind of different recrystallisation solvent, addition to the impact of crystalline product by crystal system of the present utility model.The product formed in crystal system tank body, processes via faciola shape propeller blade, can avoid producing excessive crystal block, and pulverizes the fine crystals of process of doing over again, thus proceeds Crystallization Process, can improve crystalline product yield thus.
In addition, according to the crystal system of the utility model embodiment, following additional technical feature can also be had:
According to embodiment of the present utility model,
Described temperature control assembly comprises:
Temperature control chuck, described temperature control chuck is arranged on the outer wall of described tank body;
Cooling/heating apparatus, described cooling/heating apparatus is arranged in described temperature control chuck, described cooling/heating apparatus comprises heat(ing) coil controlled separately and cooling coil, described heat(ing) coil has heating medium inlet and Crude product input, and described heat(ing) coil has the first valve control device and the first temperature controller; Described cooling coil has cooling medium entrance and cooling medium outlet, and described cooling coil has the second valve control device and the second temperature controller;
Heater, it is outer and be connected with described heat(ing) coil that described heater is arranged on described crystallization apparatus;
Cooler, it is outer and be connected with described cooling coil that described cooler is arranged on described crystallization apparatus.
Thus, crystallization process can be met, to the dissolving of sample and the demand of cooling crystallization.By the first temperature controller and the second temperature controller, the adjustment to temperature parameter in crystallization can be realized.
The conventional method of carrying out crystal screening is common slow cooling, and mainly because adopt fast cooling easily to cause crystal successfully not separate out, or product quality is not high.But, for specific products crystal formation, adopt the fast cooling of certain amplitude, can be conducive to obtaining product.Therefore, state modulator is carried out for temperature-fall period to be conducive to obtaining specific products crystal formation.
According to embodiment of the present utility model, described crystallization apparatus tank deck offers crystal seed further and adds entrance.。Thus, be convenient to difficult crystalline product and obtain target crystal formation fast.
According to embodiment of the present utility model, described crystallization apparatus tank deck is provided with visual windows.Thus, be convenient to observe Product Status in crystal system.When finding excessive crystal block, can motor be opened, regulating faciola shape propeller blade position, and making it smash excessive crystal block.
According to embodiment of the present utility model, described crystallization apparatus tank body is provided with temperature indicating device.Thus, be convenient to monitor the temperature in different conditions lower tank, to accumulate the temperature parameter in crystallization processes.
According to embodiment of the present utility model, the dismountable particle diameter being provided with large and small two kinds of different meshes of described two-layer filter selects module.The selection of order number can regulate according to the actual requirements.By two-layer filter, the crystal meeting Particle size requirements is present in the middle of it.And particle diameter excessive still stay in tank body, processed by faciola shape propeller blade; The crystal that particle diameter is too small, can unify to take out, return tank body crystallization again.The yield of target crystal can be improved thus.
According to embodiment of the present utility model, the tank body specification of described crystallization apparatus is one of 1L, 2L, 5L, 10L, 20L, 50L, 100L, 200L and 500L.Crystal system of the present utility model goes for the medicine synthesising process of different scales thus.
According to embodiment of the present utility model, described heat(ing) coil and described cooling coil are coiled in described temperature control chuck side by side in the shape of a spiral.
According to embodiment of the present utility model, described heat(ing) coil and described cooling coil are separately Stainless Steel Coil or glass coil pipe.。When crystallization apparatus specification is less, glass material can be selected, to reduce costs.When crystallization apparatus specification is larger, can stainless steel be selected, to extend life of product, and can be withstand voltage.
Additional aspect of the present utility model and advantage will part provide in the following description, and part will become obvious from the following description, or be recognized by practice of the present utility model.
Accompanying drawing explanation
Fig. 1 is the crystal system structural representation according to the utility model embodiment;
Fig. 2 is the jacket structured schematic diagram of temperature control in the crystal system according to the utility model embodiment;
Fig. 3 is two-layer filter apparatus configuration schematic diagram in the crystal system according to the utility model embodiment.
Detailed description of the invention
Be described below in detail embodiment of the present utility model, the example of described embodiment is shown in the drawings, and wherein same or similar label represents same or similar element or has element that is identical or similar functions from start to finish.Be exemplary below by the embodiment be described with reference to the drawings, be intended to for explaining the utility model, and can not be interpreted as restriction of the present utility model.
In description of the present utility model, it will be appreciated that, term " " center ", " longitudinal direction ", " transverse direction ", " length ", " width ", " thickness ", " on ", D score, " front ", " afterwards ", " left side ", " right side ", " vertically ", " level ", " top ", " end ", " interior ", " outward ", " clockwise ", " counterclockwise ", " axis ", " radial direction ", orientation or the position relationship of the instruction such as " circumference " are based on orientation shown in the drawings or position relationship, only the utility model and simplified characterization for convenience of description, instead of indicate or imply that the device of indication or element must have specific orientation, with specific azimuth configuration and operation, therefore can not be interpreted as restriction of the present utility model.
In addition, term " first ", " second " only for describing object, and can not be interpreted as instruction or hint relative importance or imply the quantity indicating indicated technical characteristic.Thus, be limited with " first ", the feature of " second " can express or impliedly comprise at least one this feature.In description of the present utility model, the implication of " multiple " is at least two, such as two, three etc., unless otherwise expressly limited specifically.
In the utility model, unless otherwise clearly defined and limited, the term such as term " installation ", " being connected ", " connection ", " fixing " should be interpreted broadly, and such as, can be fixedly connected with, also can be removably connect, or integral; Can be mechanical connection, also can be electrical connection; Can be directly be connected, also indirectly can be connected by intermediary, can be the connection of two element internals or the interaction relationship of two elements, unless otherwise clear and definite restriction.For the ordinary skill in the art, the concrete meaning of above-mentioned term in the utility model can be understood as the case may be.
In the utility model, unless otherwise clearly defined and limited, fisrt feature second feature " on " or D score can be that the first and second features directly contact, or the first and second features are by intermediary mediate contact.And, fisrt feature second feature " on ", " top " and " above " but fisrt feature directly over second feature or oblique upper, or only represent that fisrt feature level height is higher than second feature.Fisrt feature second feature " under ", " below " and " below " can be fisrt feature immediately below second feature or tiltedly below, or only represent that fisrt feature level height is less than second feature.
Below with reference to Fig. 1-Fig. 3, the crystal system of the utility model embodiment is described in detail:
According to embodiment of the present utility model, crystal system 1000 of the present utility model comprises: crystallization apparatus 100, sample storage device 200, first solvent storage device 300, second solvent storage device 400 and motor 500.
According to embodiment of the present utility model, crystallization apparatus 100 is by 130 forming at the bottom of tank body 110, tank deck 120 and tank, and tank body 110 outer wall has temperature control assembly 111, tank deck 120 offers at least one charging aperture, tank body is interior and 130 places at the bottom of close tank are provided with two-layer filter 131, offers at least one discharging opening 132 at the bottom of tank.Thus, according to the needs of sample to be separated, at least one solvent storage device can be set.Usual employing 2.
According to embodiment of the present utility model, sample storage device 200 is connected with crystallization apparatus 100 by the first charging aperture 121 of tank deck 120.
According to embodiment of the present utility model, the first solvent storage device 300 is connected with crystallization apparatus 100 by the second charging aperture 122 of tank deck 120, and the first solvent storage device 300 has first flow control device 310.Thus, the flow velocity of solvent in the first solvent storage device 300 can be regulated by second amount control device 310.
According to embodiment of the present utility model, the second solvent storage device 400 is connected with crystallization apparatus 100 by the 3rd charging aperture 123 of tank deck, and the second solvent storage device 400 has second amount control device 410.Thus, the flow velocity of solvent in the second solvent storage device 400 can be regulated by the 3rd volume control device 410.
According to embodiment of the present utility model, motor 500 is connected with faciola shape propeller blade 510, and faciola shape propeller blade 510 is arranged in the tank body 110 of crystallization apparatus 100, and can move up and down along tank body 110.
Thus, crystal system 1000 of the present utility model is suitable for screening and obtains specific products crystal formation, utilize this crystal system 1000, can quantitatively, constant speed, realize treating the process of crystallized sample efficiently, and be convenient to grope, determine the kind of different recrystallisation solvent, addition to the impact of crystalline product by crystal system 1000 of the present utility model.The product formed in crystal system 1000 tank body 100, process via faciola shape propeller blade 510, can avoid producing excessive crystal block, and the fine crystals of process of doing over again is pulverized, thus proceed Crystallization Process, crystalline product yield can be improved thus.
According to embodiments more of the present utility model, as shown in Figure 2, temperature control assembly comprises: temperature control chuck 111, cooling/heating apparatus, heater 11-5 and cooler 12-5.Wherein, temperature control chuck 111 is arranged on the outer wall of described tank body 110; Cooling/heating apparatus is arranged in temperature control chuck 111, and cooling/heating apparatus comprises heat(ing) coil 11 controlled separately and cooling coil 12; Heat(ing) coil 11 has heating medium inlet 11-1 and Crude product input 11-2, and heat(ing) coil 11 has the first valve control device 11-3 and the first temperature controller 11-4; Cooling coil 12 has cooling medium entrance 12-1 and cooling medium outlet 12-2, and described cooling coil 12 has the second valve control device 12-3 and the second temperature controller 12-4; It is outer and be connected with heat(ing) coil 11 that heater 11-5 is arranged on crystallization apparatus; It is outer and be connected with cooling coil 12 that cooler 12-5 is arranged on crystallization apparatus.Thus, the demand to the dissolving of sample and cooling crystallization in crystallization process can be met.By the first temperature controller 11-4 and the second temperature controller 12-4, the adjustment to temperature parameter in crystallization can be realized.Heat(ing) coil 11 and cooling coil 12 are connected to heater 11-5 and cooler 12-5.
According to embodiments more of the present utility model, crystallization apparatus 100 tank deck 120 offers crystal seed further and adds entrance 124.Thus, be convenient to difficult crystalline product and obtain target crystal formation fast.
According to embodiments more of the present utility model, crystallization apparatus tank deck 120 is provided with visual windows 125.Thus, be convenient to observe Product Status in crystal system.When finding excessive crystal block, motor 500 can be opened, regulating faciola shape propeller blade 510 position, and making it smash excessive crystal block.
According to embodiments more of the present utility model, crystallization apparatus tank body 110 is provided with temperature indicating device 13.Thus, be convenient to monitor the temperature in different conditions lower tank 110, to accumulate the temperature parameter in crystallization processes.
According to embodiments more of the present utility model, as shown in Figure 3, the dismountable particle diameter being provided with large and small two kinds of different meshes of two-layer filter 131 selects module 131-1 and 131-2.The selection of order number can regulate according to the actual requirements.By two-layer filter 131, make the crystal meeting Particle size requirements be present in particle diameter and select in the middle of module 131-1 and 131-2.And particle diameter excessive still stay in tank body, processed by faciola shape propeller blade 510; The crystal that particle diameter is too small, can unify to take out, return tank body 110 crystallization again.The yield of target crystal can be improved thus.
According to embodiments more of the present utility model, tank body 110 specification of crystallization apparatus is one of 1L, 2L, 5L, 10L, 20L, 50L, 100L, 200L and 500L.Crystal system of the present utility model goes for the medicine synthesising process of different scales thus.
According to specific embodiment of the utility model, heat(ing) coil 11 and cooling coil 12 are coiled in temperature control chuck 111 side by side in the shape of a spiral.
According to embodiments more of the present utility model, heat(ing) coil 11 and cooling coil 12 are separately Stainless Steel Coil or glass coil pipe.When crystallization apparatus 100 specification is less, glass material can be selected, to reduce costs.When crystallization apparatus 100 specification is larger, can stainless steel be selected, to extend life of product, and can be withstand voltage.
Conveniently understand, below the method utilizing crystal system 1000 of the present utility model to carry out crystallization is described in detail.According to embodiment of the present utility model, this method for crystallising comprises the following steps:
(1) sample to be crystallized is deposited in sample storage device 200, make it enter in crystallization apparatus tank body 110 by the first charging aperture 121;
(2) join in tank body by the first solvent in the first solvent storage device by the second charging aperture, the heater in opening temp. control assembly, heats tank body, and the sample to be crystallized in tank body is dissolved completely;
(3) join in tank body by the second solvent in the second solvent storage device by the 3rd charging aperture, the cooler in opening temp. control assembly, cools tank body, makes the sample solution cooling crystallization to be crystallized in tank body;
(4), after crystallization completes, by the two-layer filter 131 at the bottom of tank, the crystal of appropriate particle size is obtained.
According to specific embodiment of the utility model, add while the first solvent enters into tank body 110 via the first solvent storage device 300 in step (2), open the first valve control device 11-3, make heat medium enter heat(ing) coil 11, thus sample to be crystallized is dissolved completely.
According to specific embodiment of the utility model, step (2) terminates rear releasing heat medium, and closes the first valve control device 11-3.
According to specific embodiment of the utility model, step (3) is via the second solvent storage device 400, and quantitative, constant speed adds the second solvent and enters into tank body 110, opens the second valve control device 12-3 simultaneously, makes cooling medium enter cooling coil.
According to specific embodiment of the utility model, by the second temperature controller 12-4, constant speed regulates cooldown rate, makes sample solution cooling crystallization to be crystallized.
Method of the present utility model is applicable to be suitable for screening and obtains specific products crystal formation, thus, utilizes this method for crystallising, can carry out quantitatively sample, constant speed, efficiently crystallization and screening, easy to operate, and can crystalline quality be ensured, on the other hand, be also convenient to determine crystallization processes parameter.
It should be noted that, be above-mentionedly equally applicable to method for crystallising of the present utility model for the feature and advantage described by crystal system 1000, repeat no more herein.
In the description of this description, specific features, structure, material or feature that the description of reference term " embodiment ", " some embodiments ", " example ", " concrete example " or " some examples " etc. means to describe in conjunction with this embodiment or example are contained at least one embodiment of the present utility model or example.In this manual, to the schematic representation of above-mentioned term not must for be identical embodiment or example.And the specific features of description, structure, material or feature can combine in one or more embodiment in office or example in an appropriate manner.In addition, when not conflicting, the feature of the different embodiment described in this description or example and different embodiment or example can carry out combining and combining by those skilled in the art.
Although illustrate and described embodiment of the present utility model above, be understandable that, above-described embodiment is exemplary, can not be interpreted as restriction of the present utility model, those of ordinary skill in the art can change above-described embodiment, revises, replace and modification in scope of the present utility model.

Claims (9)

1. a crystal system, is characterized in that, comprising:
Crystallization apparatus, described crystallization apparatus forms by by the bottom of tank body, tank deck and tank, and described tank wall has temperature control assembly, and described tank deck offers at least one charging aperture, described tank body is interior and close tank bottom is provided with two-layer filter, offers at least one discharging opening at the bottom of described tank;
Sample storage device, described sample storage device is connected with described crystallization apparatus by the first charging aperture of described tank deck;
First solvent storage device, described first solvent storage device is connected with described crystallization apparatus by the second charging aperture of described tank deck, and the first solvent storage device has first flow control device;
Second solvent storage device, described second solvent storage device is connected with described crystallization apparatus by the 3rd charging aperture of tank deck, and the second solvent storage device has second amount control device; And
Motor, described motor is connected with faciola shape propeller blade, and described faciola shape propeller blade is arranged in the tank body of described crystallization apparatus, and can move up and down along tank body.
2. crystal system according to claim 1, is characterized in that, described temperature control assembly comprises:
Temperature control chuck, described temperature control chuck is arranged on the outer wall of described tank body;
Cooling/heating apparatus, described cooling/heating apparatus is arranged in described temperature control chuck, described cooling/heating apparatus comprises heat(ing) coil controlled separately and cooling coil, described heat(ing) coil has heating medium inlet and Crude product input, and described heat(ing) coil has the first valve control device and the first temperature controller;
Described cooling coil has cooling medium entrance and cooling medium outlet, and described cooling coil has the second valve control device and the second temperature controller;
Heater, it is outer and be connected with described heat(ing) coil that described heater is arranged on described crystallization apparatus;
Cooler, it is outer and be connected with described cooling coil that described cooler is arranged on described crystallization apparatus.
3. crystal system according to claim 1, is characterized in that, described crystallization apparatus tank deck is provided with crystal seed further and adds entrance.
4. crystal system according to claim 1, is characterized in that, described crystallization apparatus tank deck is provided with visual windows.
5. crystal system according to claim 1, is characterized in that, described crystallization apparatus tank body is provided with temperature indicating device.
6. crystal system according to claim 1, is characterized in that, the dismountable particle diameter being provided with large and small two kinds of different meshes of described two-layer filter selects module.
7. crystal system according to claim 2, is characterized in that, the tank body specification of described crystallization apparatus is one of 1L, 2L, 5L, 10L, 20L, 50L, 100L, 200L and 500L.
8. crystal system according to claim 2, is characterized in that, described heat(ing) coil and described cooling coil are coiled in described temperature control chuck side by side in the shape of a spiral.
9. crystal system according to claim 8, is characterized in that, described heat(ing) coil and described cooling coil are separately Stainless Steel Coil or glass coil pipe.
CN201520975011.1U 2015-11-30 2015-11-30 Crystal system Active CN205182237U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106807106A (en) * 2015-11-30 2017-06-09 中美华世通生物医药科技(武汉)有限公司 Crystal system and method for crystallising

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106807106A (en) * 2015-11-30 2017-06-09 中美华世通生物医药科技(武汉)有限公司 Crystal system and method for crystallising

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Address after: 430075 Guanggu Biological City B3-4, 666 High-tech Avenue, Donghu New Technology Development Zone, Wuhan City, Hubei Province

Patentee after: Sino US huashitong biomedical technology (Wuhan) Co.,Ltd.

Address before: 430075 Guanggu Biological City B3-4, 666 High-tech Avenue, Donghu New Technology Development Zone, Wuhan City, Hubei Province

Patentee before: WATERSTONE PHARMACEUTICALS(WUHAN) Co.,Ltd.