CN209286707U - Device for evaporative crystallization - Google Patents

Device for evaporative crystallization Download PDF

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Publication number
CN209286707U
CN209286707U CN201821784240.5U CN201821784240U CN209286707U CN 209286707 U CN209286707 U CN 209286707U CN 201821784240 U CN201821784240 U CN 201821784240U CN 209286707 U CN209286707 U CN 209286707U
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China
Prior art keywords
circulation
evaporation
container
inlet pipe
crystallisation vessel
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CN201821784240.5U
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Chinese (zh)
Inventor
陈志荣
刘金龙
邱贵生
王志轩
马啸
周有桂
陈卫勇
刘晓庆
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shandong Xin He Cheng Jing Hua Technology Co Ltd
SHANDONG XINHECHENG AMINO ACID Co Ltd
SHANDONG XINHECHENG PHARMACEUTICAL CO Ltd
Zhejiang University ZJU
Zhejiang NHU Co Ltd
Shandong Xinhecheng Fine Chemical Technology Co Ltd
Original Assignee
Shandong Xin He Cheng Jing Hua Technology Co Ltd
SHANDONG XINHECHENG AMINO ACID Co Ltd
SHANDONG XINHECHENG PHARMACEUTICAL CO Ltd
Zhejiang University ZJU
Zhejiang NHU Co Ltd
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Application filed by Shandong Xin He Cheng Jing Hua Technology Co Ltd, SHANDONG XINHECHENG AMINO ACID Co Ltd, SHANDONG XINHECHENG PHARMACEUTICAL CO Ltd, Zhejiang University ZJU, Zhejiang NHU Co Ltd filed Critical Shandong Xin He Cheng Jing Hua Technology Co Ltd
Priority to CN201821784240.5U priority Critical patent/CN209286707U/en
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Publication of CN209286707U publication Critical patent/CN209286707U/en
Priority to PCT/CN2019/112400 priority patent/WO2020088294A1/en
Priority to DE112019001119.7T priority patent/DE112019001119T5/en
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Abstract

The utility model provides a kind of device for evaporative crystallization, the device includes container for evaporation, crystallisation vessel, the device for evaporative crystallization further includes first circulation unit and second circulation unit, first circulation unit include sequentially connected first be in charge of, first circulation pump, first circulation inlet pipe;The second circulation unit include described sequentially connected second be in charge of, second circulation pump, heater and second circulation inlet pipe, first circulation inlet pipe and second circulation inlet pipe are connected in container for evaporation.By being provided with additional first circulation circuit, and part fine grain is imported into crystallisation vessel as nucleus again, finally obtains the product that particle is more uniform and grain diameter is controllable.

Description

Device for evaporative crystallization
Technical field
The utility model relates to chemical equipment fields, more particularly to a kind of device for evaporative crystallization.
Background technique
In state Behavior of Continuous Crystallization Processes, through the method frequently with evaporation solvent crystallization.Its corresponding device generally comprises evaporation Container, crystallisation vessel and circulation loop, the device are difficult to carry out Effective Regulation to the partial size of crystal, cause particle size distribution not , regular crystal forms degree is poor, and crystallization purity is low, to influence the quality of product.In addition, the crystalline rate of the device is also relatively low.
Utility model content
In view of the above-mentioned problems, the utility model provides a kind of crystalline rate the high device for evaporative crystallization.
The utility model provides a kind of device for evaporative crystallization comprising:
Container for evaporation, for the container for evaporation for evaporating solvent, diversion pipe is arranged in the bottom of the container for evaporation, described Boil-off gas outlet is additionally provided at the top of container for evaporation;
Crystallisation vessel, for the crystallisation vessel for crystallizing, the crystallisation vessel is located at the lower section of the container for evaporation, described Diversion pipe extends in the crystallisation vessel, and is connected with crystallisation vessel, and the bottom of the crystallisation vessel is equipped with magma discharge port; Wherein, the side wall of the crystallisation vessel is connected with recycle stock outlet pipe, and the recycle stock outlet pipe is branched into first and is in charge of and second It is in charge of;
The device for evaporative crystallization further includes first circulation unit and second circulation unit, the first circulation list Member include described first be in charge of, first circulation pump, first circulation inlet pipe, described first is in charge of and first circulation pump connects;Institute First circulation inlet pipe is stated with first end and second end, first end and the first circulation of the first circulation inlet pipe pump phase Even, the second end of the first circulation inlet pipe is connected in the container for evaporation;
The second circulation unit include described second be in charge of, second circulation pump, heater and second circulation inlet pipe, it is described Second is in charge of and successively connect with second circulation pump, heater, and the second circulation inlet pipe is described with third end and the 4th end The third end of second circulation inlet pipe is connected with the heater, and the 4th end of the second circulation inlet pipe is connected in the evaporation and holds Device;
The device for evaporative crystallization further includes material liquid inlet pipe, which is connected to this and second is in charge of, And for material liquid to be pumped to the heater by second circulation.
Rectification clasfficiator is additionally provided in the crystallisation vessel, the rectification clasfficiator includes multiple channels, the channel The ratio of the size of the upper end in the size of lower end and the channel is 1.1:1~10:1.
The size of the upper end in the channel is 3 millimeters~100 millimeters.
The percent opening in the channel is 5%~50%.
The inside of the container for evaporation is equipped with defoaming demister close to the boil-off gas exit.
The side wall of the container for evaporation and the side wall of the crystallisation vessel are additionally provided with balance pipe, and the balance pipe is connected to institute State container for evaporation and crystallisation vessel.
The device for evaporative crystallization has the advantage that
Due to multiply active force (fluid force come from the container for evaporation, by discharging bring active force, by First circulation pump, second circulation pump bring active force) effect under so that in the crystallisation vessel crystal solution be in turbulence state, The generation that can effectively avoid crystal from reuniting, so that it is controllable that crystalline particle size is precipitated;Meanwhile turbulence state has more promoted size brilliant The separation of body, and under the action of first circulation pump, second circulation pump, so that the fine grain particle circulation in crystalline particle is imported into In heater and container for evaporation.The part fine grain particle that circulation imported into container for evaporation can be used as the crystalline substance of next period recrystallization Core so that later crystallization particle is faster precipitated, and forms the crystalline particle of size more evenly.
Described second is in charge of middle setting heater, can give material liquid or the second mother liquor heat that second circulation unit is transported Amount, and promotes its evaporation section solvent in container for evaporation, be more advantageous to material liquid or the second mother liquor the crystallisation vessel into Row crystallization.The device can realize being formed continuously for crystalline particle, and crystalline rate is higher, be applicable to industrialized production.
Further, when being additionally provided with rectification clasfficiator in the crystallisation vessel, which can comb crystallisation vessel Chaotic Flow Field Distribution in (when without rectification clasfficiator), so that the liquid stream operation length below rectification clasfficiator reaches unanimity, Each stock liquid flowing speed reaches unanimity, and keeps Flow Field Distribution regular, promotes the precipitation of crystalline particle more evenly.Meanwhile rectification point Current difference is formd with below rectification clasfficiator in grade device channel, due to the powerless lasting entrainment of the low flow velocity below rectification clasfficiator Biggish crystalline particle, so that biggish crystalline particle occurs during the low flow velocity fluid carry-over being rectified below clasfficiator Precipitating, and be rectified the fine crystals that liquid stream below clasfficiator is entrained to rectification clasfficiator passage proximate, then it can be rectified classification In device channel high flow rate liquid stream entrainment, and recycle imported into heater reheat dissolution and circulation imported into evaporation hold Nucleus is used as in device.Whole process can reach screening, separation crystalline substance by adjusting size ratio above and below the percent opening in channel and channel The effect of body, so that finally obtaining the more uniform and controllable product of crystal particle diameter.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the device for evaporative crystallization of the utility model embodiment 1.
Fig. 2 is the structural schematic diagram of the device for evaporative crystallization of the utility model embodiment 2.
Fig. 3 is structural schematic diagram of the Fig. 2 for the rectification clasfficiator in the device of evaporative crystallization.
Wherein, 1, material liquid inlet pipe;2a, first are in charge of;2b, second are in charge of;3, second circulation pumps;4, heater;5, Two circulation inlet pipes;6, container for evaporation;7, diversion pipe;8, crystallisation vessel;9, demister is defoamed;10, boil-off gas exports;11, it puts down Weighing apparatus pipe;12, recycle stock outlet pipe;13, first circulation pumps;14, first circulation inlet pipe;15, magma discharge port;16, centrifuge; 17, clasfficiator is rectified;18, channel.
Specific embodiment
The technical solution in the utility model embodiment will be clearly and completely described below, it is clear that described Embodiment be only a part of embodiment of the utility model, rather than whole embodiment.Based on the utility model In embodiment, all other implementation obtained by those of ordinary skill in the art without making creative efforts Mode is fallen within the protection scope of the utility model.
Referring to Fig. 1, the utility model embodiment 1 provides a kind of device for evaporative crystallization.It is described to be tied for evaporating Brilliant device includes container for evaporation 6, crystallisation vessel 8, and crystallisation vessel 8 is located at the lower section of container for evaporation 6, and container for evaporation 6 is used for will Solvent evaporation, for crystallisation vessel 8 for crystallizing, the top of container for evaporation 6 is provided with boil-off gas outlet 10, the bottom of container for evaporation 6 Diversion pipe 7 is arranged in portion, and diversion pipe 7 extends in crystallisation vessel 8, and is connected with crystallisation vessel 8, and the side wall of crystallisation vessel 8 is connected with Recycle stock outlet pipe 12, recycle stock outlet pipe 12, which is branched into first, to be in charge of 2a and second and is in charge of 2b.
Described for evaporative crystallization further includes first circulation unit and second circulation unit, and first circulation unit includes the One is in charge of 2a, first circulation pumps 13, first circulation inlet pipe 14, and first, which is in charge of 2a and first circulation, pumps 13 and connect, first circulation into Pipe 14 has first end and second end, and the first end of first circulation inlet pipe 14 is connected with first circulation pump 13, first circulation inlet pipe 14 second end is connected in container for evaporation 6.
Second circulation unit includes described second being in charge of 2b, second circulation pump 3, heater 4 and second circulation inlet pipe 5, the Two, which are in charge of 2b, successively connect with second circulation pump 3, heater 4, and second circulation inlet pipe 5 has third end and the 4th end, and second follows The third end of ring inlet pipe 5 is connected with the heater 4, and the 4th end of second circulation inlet pipe 5 is connected in container for evaporation 6.
The device for evaporative crystallization further includes material liquid inlet pipe 1, and material liquid inlet pipe 1 is connected to this and second is in charge of 2b, and for being given material liquid by second circulation pump 3 to heater 4.
There are two circulation loops with except container for evaporation 6 for the crystallisation vessel 8.(corresponding first follows first circulation loop Ring element) are as follows: crystallisation vessel 8, recycle stock outlet pipe 12, first are in charge of 2a, first circulation pump 13, first circulation inlet pipe 14, steam Send out container 6;Second circulation loop (corresponding second circulation unit) are as follows: crystallisation vessel 8, recycle stock outlet pipe 12, second are in charge of 2b, second circulation pump 3, heater 4, second circulation inlet pipe 5, container for evaporation 6.Wherein, second is in charge of 2b and also takes on and raw material Liquid inlet pipe 1 connects, and material liquid is continuously introduced into the effect in second circulation circuit.
The first circulation circuit be used for by crystallisation vessel 8 partial mother liquid (being defined as the first mother liquor) and crystallization obtain Part fine grain particle (being defined as the first fine grain) be directed directly to container for evaporation 6, the fine grain particle of the part can be used as next week The crystallization nucleus of phase, to can induce to obtain crystalline particle more evenly.It should be noted that first fine grain can continue to grow up Bigger and crystalline particle more evenly is obtained, meanwhile, the first fine grain, which reenters crystallisation vessel 8 also, can induce more crystallizations Grain is formed in an orderly manner, that is to say, that the effect in the first circulation circuit is divided into two aspects: first is that making more crystallization Particle is formed;Second is that fine grain particle is made to be grown to uniform crystalline particle.
The second circulation circuit is used for another part mother liquor (being defined as the second mother liquor) in crystallisation vessel 8 and crystallizes To another part fine grain particle (being defined as the second fine grain) enter container for evaporation 6 by the effect of heater 4, solvent evaporation Afterwards, the crystallization in next period is carried out into crystallisation vessel 8.
The material liquid or that the container for evaporation 6 flowed into typically without additional heating by the second circulation inlet pipe 5 Two mother liquors are after the heating by heater 4, and temperature can rise, and therefore, material liquid or the second mother liquor can be described The solvent of part is evaporated in container for evaporation 6.In order to avoid the product of part is walked in the foam entrainment generated in solvent evaporation process, Yield losses are caused, defoaming demister 9 is equipped at boil-off gas outlet 10 in the inside of container for evaporation 6, defoams demister 9 It can be mesh structure or other types of defoaming demister.
The side wall of the container for evaporation 6 and the side wall of crystallisation vessel 8 are additionally provided with balance pipe 11, the connection evaporation of balance pipe 11 Container 6 and crystallisation vessel 8.
The bottom of the crystallisation vessel 8 is equipped with magma discharge port 15.
Referring to Fig. 2, the utility model embodiment 2 provides a kind of device for evaporative crystallization.This is used for evaporative crystallization Device and the device for evaporative crystallization of embodiment 1 structure it is essentially identical, difference be: set in crystallisation vessel 8 Rectify clasfficiator 17.Referring to Fig. 3, the rectification clasfficiator 17 includes multiple channels 18.The effect of the rectification clasfficiator 17 To obtain crystalline particle more evenly.
The size of the lower end in the channel 18 is greater than the purpose of design of the size of the upper end in the channel 18 there are two aspect: (1) generation of particle " back-mixing " phenomenon is prevented;(2) possibility of the blocking of channel 18 is avoided.The shaft section in the channel 18 can be with For but be not limited to trapezoidal, bowl-type, water-drop-shaped.
The ratio of the size of the upper end in the size of the lower end in the channel 18 and the channel 18 is 1.1:1~10:1, excellent Choosing, the ratio of the size of the upper end in the size of the lower end in the channel 18 and the channel 18 is 1.5:1~5:1.
The size of the upper end in the channel 18 is 3 millimeters~100 millimeters, preferably 5 millimeters~50 millimeters.
The percent opening in multiple channels 18 is (that is, the sum of the area of upper end in channel accounts for the upper table of the rectification clasfficiator The percentage of the area in face) it is 5%~50%, preferably 10%~30%.
The device for evaporative crystallization has the advantage that
The container for evaporation 6 is used to evaporate solvent in material liquid, and crystallisation vessel 8 is for crystallizing, by by recycle stock Outlet pipe 12, which is branched into first, to be in charge of 2a and second and is in charge of 2b, and first is in charge of 2a for crystallizing material liquid in the crystalline particle to be formed Fine grain particle be directed in container for evaporation 6 again, which can be used as the nucleus of next Periodical crystallization, to induce Crystalline particle more and more evenly is formed;Described second is in charge of setting heater 4 in 2b, can give material liquid or the second mother Liquid heat, and in container for evaporation 6 solvent portion evaporate, be more advantageous to material liquid or the second mother liquor the crystallisation vessel 8 into Row crystallization.
The device can be used for being formed continuously for crystal grain.Particularly, it is suitable for vitamin B6, saccharinic acid, Sucralose, ethyl Maltol, methionine, 2-KLG, citric acid, threonine, tryptophan, sodium gluconate, glucose, glutamic acid, lysine or The evaporation and crystal process of sorbierite.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited In contradiction, all should be considered as described in this specification.
Above-described embodiments merely represent several embodiments of the utility model, the description thereof is more specific and detailed, But it cannot be understood as the limitations to utility model patent range.It should be pointed out that for the common skill of this field For art personnel, without departing from the concept of the premise utility, various modifications and improvements can be made, these are belonged to The protection scope of the utility model.Therefore, the scope of protection shall be subject to the appended claims for the utility model patent.

Claims (6)

1. a kind of device for evaporative crystallization comprising:
Container for evaporation, for the container for evaporation for evaporating solvent, diversion pipe, the evaporation is arranged in the bottom of the container for evaporation Boil-off gas outlet is additionally provided at the top of container;
Crystallisation vessel, for the crystallisation vessel for crystallizing, the crystallisation vessel is located at the lower section of the container for evaporation, the water conservancy diversion Pipe extends in the crystallisation vessel, and is connected with crystallisation vessel, and the bottom of the crystallisation vessel is equipped with magma discharge port;It is special Sign is,
The side wall of the crystallisation vessel is connected with recycle stock outlet pipe, and the recycle stock outlet pipe is branched into first and is in charge of and second point Pipe;
The device for evaporative crystallization further includes first circulation unit and second circulation unit, the first circulation unit packet Include described first be in charge of, first circulation pump, first circulation inlet pipe, described first is in charge of and first circulation pump connects;Described One circulation inlet pipe has first end and second end, and the first end of the first circulation inlet pipe is connected with first circulation pump, institute The second end for stating first circulation inlet pipe is connected in the container for evaporation;
The second circulation unit include described second be in charge of, second circulation pump, heater and second circulation inlet pipe, described second It to be in charge of and successively connect with second circulation pump, heater, the second circulation inlet pipe is with third end and the 4th end, and described second The third end of circulation inlet pipe is connected with the heater, and the 4th end of the second circulation inlet pipe is connected in the container for evaporation;
The device for evaporative crystallization further includes material liquid inlet pipe, which is connected to this and second is in charge of, and is used in combination In material liquid is pumped to the heater by second circulation.
2. being used for the device of evaporative crystallization as described in claim 1, which is characterized in that be additionally provided with rectification in the crystallisation vessel Clasfficiator, the rectification clasfficiator include multiple channels, the size of the size of the lower end in the channel and the upper end in the channel Ratio be 1.1:1~10:1.
3. being used for the device of evaporative crystallization as claimed in claim 2, which is characterized in that the size of the upper end in the channel is 3 Millimeter~100 millimeters.
4. as claimed in claim 2 be used for evaporative crystallization device, which is characterized in that the percent opening in the channel be 5%~ 50%.
5. being used for the device of evaporative crystallization as described in claim 1, which is characterized in that the inside of the container for evaporation is close to institute It states boil-off gas exit and is equipped with defoaming demister.
6. being used for the device of evaporative crystallization as described in claim 1, which is characterized in that the side wall of the container for evaporation and institute The side wall for stating crystallisation vessel is additionally provided with balance pipe, and the balance pipe is connected to the container for evaporation and crystallisation vessel.
CN201821784240.5U 2018-10-31 2018-10-31 Device for evaporative crystallization Active CN209286707U (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
CN201821784240.5U CN209286707U (en) 2018-10-31 2018-10-31 Device for evaporative crystallization
PCT/CN2019/112400 WO2020088294A1 (en) 2018-10-31 2019-10-22 Device for evaporation and crystallization
DE112019001119.7T DE112019001119T5 (en) 2018-10-31 2019-10-22 Evaporation crystallization device

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CN201821784240.5U CN209286707U (en) 2018-10-31 2018-10-31 Device for evaporative crystallization

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109289234A (en) * 2018-10-31 2019-02-01 浙江新和成股份有限公司 For the device of evaporative crystallization, the method for crystallising of vitamin B6
CN109289233A (en) * 2018-10-31 2019-02-01 浙江新和成股份有限公司 For the device of evaporative crystallization, the method for crystallising of methionine
CN109289235A (en) * 2018-10-31 2019-02-01 浙江新和成股份有限公司 Device, ascorbic method for crystallising for evaporative crystallization
CN109453539A (en) * 2018-10-31 2019-03-12 浙江新和成股份有限公司 For the device of evaporative crystallization, the method for crystallising of Sucralose
CN109513232A (en) * 2018-10-31 2019-03-26 浙江新和成股份有限公司 For the device of evaporative crystallization, the method for crystallising of ethylmaltol
WO2020088294A1 (en) * 2018-10-31 2020-05-07 浙江新和成股份有限公司 Device for evaporation and crystallization

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109289234A (en) * 2018-10-31 2019-02-01 浙江新和成股份有限公司 For the device of evaporative crystallization, the method for crystallising of vitamin B6
CN109289233A (en) * 2018-10-31 2019-02-01 浙江新和成股份有限公司 For the device of evaporative crystallization, the method for crystallising of methionine
CN109289235A (en) * 2018-10-31 2019-02-01 浙江新和成股份有限公司 Device, ascorbic method for crystallising for evaporative crystallization
CN109453539A (en) * 2018-10-31 2019-03-12 浙江新和成股份有限公司 For the device of evaporative crystallization, the method for crystallising of Sucralose
CN109513232A (en) * 2018-10-31 2019-03-26 浙江新和成股份有限公司 For the device of evaporative crystallization, the method for crystallising of ethylmaltol
WO2020088294A1 (en) * 2018-10-31 2020-05-07 浙江新和成股份有限公司 Device for evaporation and crystallization
CN109289235B (en) * 2018-10-31 2020-12-15 浙江新和成股份有限公司 Device for evaporative crystallization and crystallization method of vitamin C
CN109513232B (en) * 2018-10-31 2020-12-15 浙江新和成股份有限公司 Device for evaporative crystallization and crystallization method of ethyl maltol
CN109453539B (en) * 2018-10-31 2020-12-15 浙江新和成股份有限公司 Device for evaporative crystallization and method for crystallizing sucralose
CN109289233B (en) * 2018-10-31 2020-12-15 浙江新和成股份有限公司 Device for evaporative crystallization and method for crystallizing methionine
CN109289234B (en) * 2018-10-31 2020-12-15 浙江新和成股份有限公司 Device for evaporative crystallization and crystallization method of vitamin B6

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