CN109157863A - Theophylline sodium salt Continuous Cooling Crystallization device and method - Google Patents
Theophylline sodium salt Continuous Cooling Crystallization device and method Download PDFInfo
- Publication number
- CN109157863A CN109157863A CN201811143544.8A CN201811143544A CN109157863A CN 109157863 A CN109157863 A CN 109157863A CN 201811143544 A CN201811143544 A CN 201811143544A CN 109157863 A CN109157863 A CN 109157863A
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- Prior art keywords
- crystallizer
- sodium salt
- cooler
- theophylline sodium
- theophylline
- Prior art date
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- IHJVDPWMLXFQAI-UHFFFAOYSA-N 1,3-dimethyl-7h-purine-2,6-dione;sodium Chemical compound [Na].O=C1N(C)C(=O)N(C)C2=C1NC=N2 IHJVDPWMLXFQAI-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 238000002425 crystallisation Methods 0.000 title claims abstract description 38
- 230000008025 crystallization Effects 0.000 title claims abstract description 33
- 238000001816 cooling Methods 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 49
- 239000000463 material Substances 0.000 claims abstract description 14
- 239000013078 crystal Substances 0.000 claims description 52
- 239000012452 mother liquor Substances 0.000 claims description 12
- 108010016634 Seed Storage Proteins Proteins 0.000 claims description 9
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 238000003860 storage Methods 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 239000000243 solution Substances 0.000 abstract description 15
- 239000012266 salt solution Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 3
- ZFXYFBGIUFBOJW-UHFFFAOYSA-N theophylline Chemical compound O=C1N(C)C(=O)N(C)C2=C1NC=N2 ZFXYFBGIUFBOJW-UHFFFAOYSA-N 0.000 description 22
- 229960000278 theophylline Drugs 0.000 description 11
- 159000000000 sodium salts Chemical class 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 8
- MLIREBYILWEBDM-UHFFFAOYSA-N cyanoacetic acid Chemical compound OC(=O)CC#N MLIREBYILWEBDM-UHFFFAOYSA-N 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- 239000002245 particle Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- QVGLHVDBDYLFON-UHFFFAOYSA-M sodium;1,3-dimethylpurin-7-ide-2,6-dione Chemical compound [Na+].O=C1N(C)C(=O)N(C)C2=C1[N-]C=N2 QVGLHVDBDYLFON-UHFFFAOYSA-M 0.000 description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 2
- MGJKQDOBUOMPEZ-UHFFFAOYSA-N N,N'-dimethylurea Chemical compound CNC(=O)NC MGJKQDOBUOMPEZ-UHFFFAOYSA-N 0.000 description 2
- LKZUYXCUDBKOKW-UHFFFAOYSA-N N-carbamoylacetamide oxalonitrile Chemical compound C(C)(=O)NC(=O)N.N#CC#N LKZUYXCUDBKOKW-UHFFFAOYSA-N 0.000 description 2
- RYYVLZVUVIJVGH-UHFFFAOYSA-N caffeine Chemical compound CN1C(=O)N(C)C(=O)C2=C1N=CN2C RYYVLZVUVIJVGH-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 235000019253 formic acid Nutrition 0.000 description 2
- QHTPSODXPLCXJB-UHFFFAOYSA-N piperazine;urea Chemical compound NC(N)=O.C1CNCCN1 QHTPSODXPLCXJB-UHFFFAOYSA-N 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000004886 process control Methods 0.000 description 2
- 238000007363 ring formation reaction Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- VFGRNTYELNYSKJ-UHFFFAOYSA-N 6-amino-1,3-dimethylpyrimidine-2,4-dione Chemical compound CN1C(N)=CC(=O)N(C)C1=O VFGRNTYELNYSKJ-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- LPHGQDQBBGAPDZ-UHFFFAOYSA-N Isocaffeine Natural products CN1C(=O)N(C)C(=O)C2=C1N(C)C=N2 LPHGQDQBBGAPDZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 229960001948 caffeine Drugs 0.000 description 1
- VJEONQKOZGKCAK-UHFFFAOYSA-N caffeine Natural products CN1C(=O)N(C)C(=O)C2=C1C=CN2C VJEONQKOZGKCAK-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000009935 nitrosation Effects 0.000 description 1
- 238000007034 nitrosation reaction Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 239000012047 saturated solution Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 235000010288 sodium nitrite Nutrition 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0004—Crystallisation cooling by heat exchange
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0063—Control or regulation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D2009/0086—Processes or apparatus therefor
Abstract
The invention discloses a kind of theophylline sodium salt Continuous Cooling Crystallization device and methods.The device includes crystallizer and cooler, and the supersaturated solution feed inlet of the crystallizer is connected with the liquid outlet of the cooler, and the material liquid outlet of the crystallizer is connected with the inlet of the cooler.Theophylline sodium salt Continuous Cooling Crystallization device provided by the present invention, cooler and crystallizer are used in combination, pass through the cooling effect of cooler, substantially reduce the theophylline sodium salt solubility in theophylline sodium salt solution, feed liquid forms supersaturated solution, and excessive theophylline sodium salt is precipitated in supersaturated solution in a crystallizer, obtains required theophylline sodium salt.
Description
Technical field
The present invention relates to crystallisation by cooling fields, and are specifically related to a kind of theophylline sodium salt Continuous Cooling Crystallization device and method.
Background technique
Theophylline sodium salt, i.e. 1,3- dimethyl xanthine sodium salt, as theophylline intermediate and be widely used.It is existing
The conventional production method of theophylline sodium salt are as follows: be condensed with cyanoacetic acid and dimethyl urea, generate 1,3- dimethyl cyanogen acetylurea, then in alkali
Property under the conditions of cyclization 1,3- dimethyl -4- imino group urea piperazine is made, then nitrosation and restore to obtain 1,3- dimethyl -4,5- diamino
Finally the product are made with the acylated simultaneously cyclization of formic acid in base urea piperazine.Currently, the precipitation mode of crystal used by theophylline sodium salt is nature
Sedimentation either stirring decrease temperature crystalline, not only short time consumption is long for these methods, and efficiency is very low, large labor intensity.
Summary of the invention
The main purpose of the present invention is to provide a kind of theophylline sodium salt Continuous Cooling Crystallization device and methods, to optimize theophylline
The efficiency of sodium salt Continuous Cooling Crystallization.
For this purpose, provide a kind of theophylline sodium salt Continuous Cooling Crystallization device in the present invention, the device include crystallizer and
The supersaturated solution feed inlet of cooler, the crystallizer is connected with the liquid outlet of the cooler, the material of the crystallizer
Liquid outlet is connected with the inlet of the cooler.
Preferably, the crystallizer has vertical structure, and is formed with and the knot in the bottom inside of the crystallizer
The theophylline sodium salt crystal seed storage groove that brilliant device inner cavity is connected；It is preferred that the crystallizer has inverted cone-shaped structure, the more preferable knot
The conical lower portion of brilliant device is as theophylline sodium salt crystal seed storage groove.
Preferably, the inside of the crystallizer is formed with feed pipe, and the arrival end of the feed pipe extends to described
The outside of crystallizer is connected with the liquid outlet of the cooler, and the outlet end of the feed pipe is prolonged in the inside of the crystallizer
It stretches, and extends close to and be higher than the position of the theophylline sodium salt crystal seed storage groove.
Preferably, crystal discharge port is formed on the side wall of the crystallizer, the setting of the crystal discharge port is in height
In the position of the outlet end of the feed pipe；It is preferred that along multiple crystal discharge ports that are vertically arranged with of the crystallizer, it is more excellent
Along the longitudinal direction of the crystallizer, the aperture of each crystal discharge port is sequentially reduced from the bottom to top for choosing.
Preferably, blender is provided in the crystallizer, the outlet end of the feed pipe is arranged in the blender
Between the crystalliser feet, the preferably described blender is located in the theophylline sodium salt crystal grain storage groove.
Preferably, described device includes feed liquid circulation pump, and the feed liquid that the crystallizer is arranged in the feed liquid circulation pump goes out
Between mouth and the inlet of the cooler.
Preferably, feed liquid conveyance conduit is configured between the material liquid outlet of the crystallizer and the cooler inlet,
Masterbatch feed inlet and/or material inlet are provided on the feed liquid conveyance conduit.
Preferably, the cooler is cartridge type cooler, is enclosed with muff on the outside of the cooler；The cooler
Liquid outlet be higher than inlet, the media outlet of the muff is higher than medium inlet.
Meanwhile a kind of theophylline sodium salt Continuous Cooling Crystallization method is additionally provided in the present invention, this method comprises: S1, general
It reacts obtained theophylline sodium salt mother liquor and is cooled to 30-60 DEG C, obtain supersaturated solution；S2, by the supersaturated solution and theophylline
Stirred crystallization processing is carried out after the mixing of sodium salt crystal seed, and while obtaining theophylline crystals of sodium salt, obtains feed liquid；S3, will be described
Feed liquid is back in step S1.
Preferably, the theophylline sodium salt crystal seed is theophylline sodium salt solid of the D50 range at 75~150 μm.
Theophylline sodium salt Continuous Cooling Crystallization device provided by the present invention, cooler and crystallizer are used in combination, passed through
The cooling effect of cooler substantially reduces the theophylline sodium salt solubility in theophylline sodium salt solution, and feed liquid forms supersaturated solution,
And excessive theophylline sodium salt is precipitated in supersaturated solution in a crystallizer, obtains required theophylline sodium salt.This Continuous Cooling Crystallization dress
The production efficiency that can greatly improve theophylline sodium salt is set, centralized layout reduces land occupation；It is able to produce that granularity is larger and uniform crystalline substance
Body；Process control system realizes the operation of DCS system platform, carries out full-automatic centralized control to technological parameter, it is ensured that production technology
Stability, improve technique production the degree of automation, reduce labor intensity.
Detailed description of the invention
The drawings are intended to provide a further understanding of the invention, and constitutes part of specification, with following tool
Body embodiment is used to explain the present invention together, but is not construed as limiting the invention.In the accompanying drawings:
Fig. 1 is the theophylline sodium salt Continuous Cooling Crystallization device according to the embodiment of the present invention 1.
In figure: 10 being crystallizer, 11 be feed pipe, 12 be crystal discharge port, 20 be cooler, 30 be feed liquid delivery pipe
Road, 31 be masterbatch feed inlet, 32 be material inlet, 40 be feed liquid circulation pump.
Specific embodiment
Embodiment one
A kind of theophylline sodium salt Continuous Cooling Crystallization device is provided in this embodiment, as shown in Figure 1, the device includes
Crystallizer 10 and cooler 20, the supersaturated solution feed inlet of the crystallizer 10 are connected with the liquid outlet of the cooler 20
Logical, the material liquid outlet of the crystallizer 10 is connected with the inlet of the cooler 20.
Theophylline sodium salt Continuous Cooling Crystallization device provided by the present invention, cooler and crystallizer are used in combination, passed through
The cooling effect of cooler substantially reduces the theophylline sodium salt solubility in theophylline sodium salt solution, and feed liquid forms supersaturated solution,
And excessive theophylline sodium salt is precipitated in supersaturated solution in a crystallizer, obtains required theophylline sodium salt.This Continuous Cooling Crystallization dress
The production efficiency that can greatly improve theophylline sodium salt is set, centralized layout reduces land occupation；It is able to produce that granularity is larger and uniform crystalline substance
Body；Process control system realizes the operation of DCS system platform, carries out full-automatic centralized control to technological parameter, it is ensured that production technology
Stability, improve technique production the degree of automation, reduce labor intensity.
In this embodiment, crystallizer can be using any existing commercial device.Under preferable case, the crystallizer
10 have vertical structure, and the theophylline being connected with 10 inner cavity of crystallizer is formed in the bottom inside of the crystallizer 10
Sodium salt crystal seed storage groove；It is preferred that the crystallizer 10 has inverted cone-shaped structure, the conical lower portion of the more preferable crystallizer 10 is made
For theophylline sodium salt crystal seed storage groove.In this configuration, it can be deposited by the way that theophylline sodium salt crystal seed is arranged in 10 inner cavity of crystallizer
Slot is put to store theophylline sodium salt, utilizes the percent crystallization in massecuite and crystallization purity of the presence optimization theophylline sodium salt of theophylline sodium salt crystal seed.
In the case of in this embodiment it is preferred that, the inside of the crystallizer 10 is formed with feed pipe 11, the charging
The outside that the arrival end of pipeline 11 extends to the crystallizer 10 is connected with the liquid outlet of the cooler 20, the feed pipe
11 outlet end and extends close in the internal stretch of the crystallizer 10 and is higher than the theophylline sodium salt crystal seed storage groove
Position.In this configuration, by controlling the position of 11 outlet end of feed pipe, so that the theophylline flowed by feed pipe 11
Sodium salt mother liquor can come into full contact with the theophylline sodium salt crystal seed inside crystallizer 10, and then optimize the percent crystallization in massecuite and knot of theophylline sodium salt
Brilliant purity.
In the case of in this embodiment it is preferred that, crystal discharge port 12, institute are formed on the side wall of the crystallizer 10
State the position of the outlet end for being positioned above the feed pipe 11 of crystal discharge port 12；It is preferred that along the vertical of the crystallizer 10
To being provided with multiple crystal discharge ports 12, the more preferably longitudinal direction along the crystallizer 10, the aperture of each crystal discharge port 12
It is sequentially reduced from the bottom to top.In this configuration, by the way that crystal discharge port 12 is arranged according to pre-defined rule, being conducive to collect has
The theophylline sodium salt particle of predetermined size, to correspond to subsequent requirement.
In the case of in this embodiment it is preferred that, blender is provided in the crystallizer 10, the blender setting exists
Between 10 bottom of outlet end and the crystallizer of the feed pipe 11, it is brilliant that the preferably described blender is located at the theophylline sodium salt
In grain storage groove.In this configuration, by the way that blender is arranged, be conducive to that the theophylline sodium salt positioned at 10 bottom of crystallizer is promoted to transport
It is dynamic, and promote theophylline sodium salt mother liquor that can come into full contact with the theophylline sodium salt crystal seed inside crystallizer 10, and then optimize theophylline sodium
The percent crystallization in massecuite and crystallization purity of salt.
In the case of in this embodiment it is preferred that, described device includes feed liquid circulation pump 40, and the feed liquid circulation pump 40 is set
It sets between the material liquid outlet of the crystallizer 10 and the inlet of the cooler 20.In this configuration, expected by setting
Liquid circulating pump 40 is conducive to control recycling for supersaturated solution, and then can be with the efficiency of comprehensively control theophylline sodium salt crystal
With percent crystallization in massecuite.
In the case of in this embodiment it is preferred that, the material liquid outlet of the crystallizer 10 and 20 inlet of cooler
Between be configured with feed liquid conveyance conduit 30, be provided with masterbatch feed inlet 31 and/or feedstock on the feed liquid conveyance conduit 30
Mouth 32.In this configuration by being provided with masterbatch feed inlet 31 and/or material inlet 32 on feed liquid conveyance conduit 30, have
Conducive to so that theophylline sodium salt mother liquor and/or other raw materials are sufficiently mixed with supersaturated solution, to improve while Optimizing Flow
Efficiency.
In the case of in this embodiment it is preferred that, the cooler is cartridge type cooler, and the outside of the cooler is wrapped up
There is muff；The liquid outlet of the cooler is higher than inlet, and the media outlet of the muff is higher than medium inlet.
Embodiment two
In this embodiment, a kind of theophylline sodium salt Continuous Cooling Crystallization method is provided, this method comprises:
S1, the theophylline sodium salt mother liquor for obtaining reaction obtain supersaturated solution through cooling treatment (preferably)；
S2, stirred crystallization processing is carried out after mixing the supersaturated solution with theophylline sodium salt crystal seed, and obtaining theophylline
While crystals of sodium salt, feed liquid is obtained；
S3, the feed liquid is back in step S1.
In this embodiment, in step S1 the temperature of cooling treatment within the scope of 30~60 DEG C.Have within the scope of this
Reach hypersaturated state conducive to theophylline sodium salt solution.
In this embodiment, theophylline sodium salt crystal seed employed in step S2 is to grow naturally from theophylline sodium salt mother liquor
Crystal seed out, granularity is within 75~150 μ ms.There is granularity by using this crystal seed and saturated solution stirred crystallization
Uniformly, advantage with high purity.
In this embodiment, the condition of stirred crystallization includes in step S2, temperature be 15~30 DEG C, the time be 30~
60min carries out the precipitation that crystallization is conducive to theophylline sodium salt continuous-stable under these conditions.
The embodiment is further illustrated below in conjunction with specific embodiment.
Theophylline sodium salt is the intermediate of caffeine, and preparation process has disclosed, and process is as follows:
Cyanoacetic acid is reacted with dimethyl urea generates diformazan cyanogen acetylurea；Diformazan cyanogen acetylurea is reacted with liquid alkaline generates 6- amino-
1,3- dimethyl uracil (diformazan -4AU)；Diformazan -4AU is reacted with sodium nitrite in acid condition generates diformazan-NAU；Two
First-NAU is diformazan-DAU by hydrogen reducing in the presence of a catalyst.Diformazan-DAU is reacted with formic acid generates diformazan-FAU, and two
First-FAU reacts production theophylline sodium salt solution with liquid alkaline.
Embodiment 1:
Device: theophylline sodium salt Continuous Cooling Crystallization device shown in FIG. 1 is used；
Method: the theophylline sodium salt mother liquor of aforementioned preparation is squeezed into cooler by feed liquid conveyance conduit 30, feed liquid circulation pump 40
In 20, it is cooled to 15~30 DEG C in cooler 20, is entered in crystallizer 10 (volume is equal to 50L) by feed pipe 11 afterwards,
With the theophylline sodium for being 75~150 μm positioned at granularity in theophylline sodium salt crystal seed storage groove, being grown naturally from theophylline sodium salt mother liquor
The mixing of salt crystal seed crystallizes 30~60min, and from the crystal discharge port output theophylline on the side wall of crystallizer at 15~30 DEG C
Crystals of sodium salt product.
Conclusion: the theophylline sodium salt mother liquor that aforementioned device with continuous feed, can handle 5kg only needs 0.5~1.5h, and from knot
Crystal discharge port on the side wall of brilliant device can be 75~150 μm with the even-grained crystal of output, particle size range, it can be seen that
Using with device, being not only able to improve the efficiency of crystallization treatment, and it is relatively thin to obtain granularity according to the method for the present invention
Small theophylline crystals of sodium salt.
Comparative example 1
Device: commercially available conventional crystallization device (not including cooler)；
The theophylline sodium salt mother liquor of aforementioned preparation is delivered in conventional crystallization apparatus by method, under agitation, cooling
To 20~25 DEG C of temperature, 8~10h of crystallisation by cooling is carried out, obtains theophylline crystals of sodium salt product.
Conclusion: aforementioned device is intermittent feeding device, and the theophylline sodium salt mother liquor for handling 5kg needs 8~10h, Er Qiesuo
The crystal size of output be 200~350 μm, it can be seen that using according to the method in the prior art with device, crystallization treatment
It is inefficient, and theophylline crystals of sodium salt granularity is comparatively coarse, and particle size range difference is larger.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, is equivalent, replacement, improvement etc. should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of theophylline sodium salt Continuous Cooling Crystallization device, which is characterized in that described device includes crystallizer (10) and cooler
(20), the supersaturated solution feed inlet of the crystallizer (10) is connected with the liquid outlet of the cooler (20), the crystallization
The material liquid outlet of device (10) is connected with the inlet of the cooler (20).
2. the apparatus according to claim 1, which is characterized in that the crystallizer (10) has vertical structure, and described
The bottom inside of crystallizer (10) is formed with the theophylline sodium salt crystal seed storage groove being connected with the crystallizer (10) inner cavity；It is preferred that
The crystallizer (10) has inverted cone-shaped structure, and the conical lower portion of the more preferable crystallizer (10) is deposited as theophylline sodium salt crystal seed
Put slot.
3. the apparatus of claim 2, which is characterized in that the inside of the crystallizer (10) is formed with feed pipe
(11), the arrival end of the feed pipe (11) extends to the outside of the crystallizer (10) and the liquid out of the cooler (20)
Mouthful it is connected, the outlet end of the feed pipe (11) and extends close to and is higher than in the internal stretch of the crystallizer (10)
The position of the theophylline sodium salt crystal seed storage groove.
4. device according to claim 3, which is characterized in that be formed with crystal on the side wall of the crystallizer (10) and go out
Material mouth (12), the crystal discharge port (12) are positioned above the position of the outlet end of the feed pipe (11)；It is preferred that along institute
That states crystallizer (10) is vertically arranged with multiple crystal discharge ports (12), the more preferably longitudinal direction along the crystallizer (10), each institute
The aperture for stating crystal discharge port (12) is sequentially reduced from the bottom to top.
5. device according to claim 3, which is characterized in that it is provided with blender in the crystallizer (10), it is described to stir
It mixes device to be arranged between the outlet end and the crystallizer (10) bottom of the feed pipe (11), the preferably described blender is located at
In the theophylline sodium salt crystal grain storage groove.
6. the apparatus according to claim 1, which is characterized in that described device includes feed liquid circulation pump (40), the feed liquid
Circulating pump (40) is arranged between the material liquid outlet of the crystallizer (10) and the inlet of the cooler (20).
7. the apparatus according to claim 1, which is characterized in that the material liquid outlet and the cooler of the crystallizer (10)
(20) feed liquid conveyance conduit (30) are configured between inlet, are provided with theophylline sodium salt masterbatch on the feed liquid conveyance conduit (30)
Feed inlet (31) and/or other material inlets (32) to be crystallized.
8. the apparatus according to claim 1, which is characterized in that the cooler (10) is cartridge type cooler, the cooling
Device is enclosed with muff on the outside of (10)；The liquid outlet of the cooler (10) is higher than inlet, and the medium of the muff goes out
Mouth is higher than medium inlet.
9. a kind of theophylline sodium salt Continuous Cooling Crystallization method, which is characterized in that the described method includes:
S1, the theophylline sodium salt mother liquor that reaction obtains is cooled to 30~60 DEG C, obtains supersaturated solution；
S2, stirred crystallization processing is carried out after mixing the supersaturated solution with theophylline sodium salt crystal seed, and obtaining theophylline sodium salt
While crystal, feed liquid is obtained；
S3, the feed liquid is back in step S1.
10. according to the method described in claim 9, it is characterized in that, the theophylline sodium salt crystal seed is D50 range in 75~150 μ
The theophylline sodium salt solid of m.
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| CN201811143544.8A CN109157863A (en) | 2018-09-28 | 2018-09-28 | Theophylline sodium salt Continuous Cooling Crystallization device and method |
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| CN201811143544.8A CN109157863A (en) | 2018-09-28 | 2018-09-28 | Theophylline sodium salt Continuous Cooling Crystallization device and method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113457200A (en) * | 2021-07-09 | 2021-10-01 | 西安航天华威化工生物工程有限公司 | Accurate path control continuous crystallization system for nickel sulfate |
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| CZ2014207A3 (en) * | 2014-03-28 | 2015-05-27 | Bochemie A.S. | Discontinuous crystallization unit for producing spherical crystals |
| CN204841004U (en) * | 2015-06-15 | 2015-12-09 | 江阴市江中设备制造有限公司 | Continuous crystallization equipment of phosphate |
| CN105797422A (en) * | 2016-04-20 | 2016-07-27 | 西安航天华威化工生物工程有限公司 | Citric acid continuous cooling crystallization system and method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113457200A (en) * | 2021-07-09 | 2021-10-01 | 西安航天华威化工生物工程有限公司 | Accurate path control continuous crystallization system for nickel sulfate |
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