CN201445824U - Ultrasonic strengthened tri-pentaerythritol crystallizer - Google Patents
Ultrasonic strengthened tri-pentaerythritol crystallizer Download PDFInfo
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- CN201445824U CN201445824U CN2009200429064U CN200920042906U CN201445824U CN 201445824 U CN201445824 U CN 201445824U CN 2009200429064 U CN2009200429064 U CN 2009200429064U CN 200920042906 U CN200920042906 U CN 200920042906U CN 201445824 U CN201445824 U CN 201445824U
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- tripentaerythritol
- crystallization
- ultrasonic transducer
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Abstract
The utility model discloses an ultrasonic strengthened tri-pentaerythritol crystallizer, which comprises a vessel, an axial-flow type stirrer, a solution inlet (4) and a crystallization liquid outlet (5). The crystallizer is characterized in that the solution inlet (4) is formed at the upper part of the vessel; the crystallization liquid outlet (5) is formed at the bottom end of the vessel; the axial-flow type stirrer is fixed at the top end of the vessel; an ultrasonic transducer mounting hole (6) is formed on the side of the vessel; and an ultrasonic transducer (3) is mounted in the ultrasonic transducer mounting hole. The utility model overcomes the defects in the prior art that the crystallization time is long, the supersaturation degree is reduced and insufficient, the content of tri-pentaerythritol in the solution is high.
Description
Technical field
The utility model relates to a kind of crystallization apparatus, especially relates to the crystallization apparatus of tripentaerythritol.
Background technology
Tripentaerythritol is a kind of important polyalcohol product, is applied to aspects such as organic synthesis and medicine synthesize.The production method of tripentaerythritol normally adopts formaldehyde, acetaldehyde and base catalyst to synthesize.Because tripentaerythritol solubility is very little, tripentaerythritol is separated out with regard to crystallization when reaction, but because the tripentaerythritol molecular weight causes sterically hindered greatly greatly, tripentaerythritol is separated out from condensation liquid needs 24-36 hour crystallization time.
" fine-chemical intermediate " the 33rd volume first phase has been reported " the synthetic and separating technology research of tripentaerythritol ".This method has been introduced the particle diameter that the method that adds the hole enlargement agent before reaction increases tripentaerythritol.The hole enlargement agent is a kind of chemical substance, and its adding must be brought new impurity into to product, thereby influences product quality.
Publication number is that the Chinese invention patent of CN1408691A discloses " a kind of new technology and suction filter that three pentaerythrite is separated " from condensation liquid, the disclosed suction filter of this patent of invention is a kind of vacuum filter, this employing suction filter separates the means of tripentaerythritol, there is not fully to reduce the degree of supersaturation of tripentaerythritol, thereby be easy to blocking filter, operational efficiency is low.
In the actual production, tripentaerythritol is the by-product when formaldehyde, acetaldehyde and base catalyst are the raw material synthesis of pentaerythritol, along with reaction is constantly carried out tripentaerythritol concentration and improved constantly.Tripentaerythritol is a hypersaturated state in the condensation liquid, and because of the tripentaerythritol molecular weight is big, crystallization is very difficult, and the part tripentaerythritol is separated out and fouling on the reactor cooling coil, influences the heat-transfer effect of reactor.
Above-mentioned filter plant commonly used is removed before in the tripentaerythritol separation method, if degree of supersaturation height in the solution, tripentaerythritol will have crystallization to separate out when filtering, and separate out crystallization attached on the filter medium, thereby it is frequent to make that filter medium upgrades, and filter efficiency descends.For the tripentaerythritol sufficient crystallising that makes condensation liquid comes out, at present mostly by using precipitation apparatus promptly to adopt the way of sedimentation crystallization, usually want sedimentation 24-36 hour, sedimentation time is very long, and the sedimentation crystallization is not because of there being the crystallization enhancements, degree of supersaturation does not reduce fully, contains too much three seasons in the condensation liquid after the filtration, influences product quality.
Summary of the invention
The purpose of this utility model is in order to overcome the deficiencies in the prior art, provides that a kind of crystallization time is short, degree of supersaturation reduces fully, crystal can be attached to tank skin, can not bring the ultrasound-enhanced tripentaerythritol crystallization apparatus of new impurity to product into.
The purpose of this utility model is achieved in that ultrasound-enhanced tripentaerythritol crystallization apparatus, comprise container, axial flow type stirrer, solution inlet port, crystal solution outlet, solution inlet port is arranged on the top of container, the crystal solution outlet is arranged on the bottom of container, axial flow type stirrer is fixed in the top of container, it is characterized in that being provided with the ultrasonic transducer installing hole, in this ultrasonic transducer installing hole, ultrasonic transducer is installed in the side of container.
Further, described container is a conical vessel.
Further, described axial flow type stirrer is the adjustable speed axial flow type stirrer.
Further, described ultrasonic transducer is the ultrasonic transducer of power output adjustable size.
So-called solution crystallization is the solute process that crystallization is separated out from liquid solution. and solute crystallizes out from solution and will experience two steps: nucleation process and crystal growing process. and nucleation process is that solute produces the core of the crystal grain of microcosmic as crystallization, i.e. nucleus in solution; Nucleus is grown up in solution and is grown into the crystal of macroscopic view, i.e. crystal growth. and in certain solution system, the speed of crystallization nucleation can be expressed as JN=K exp[-A/ (ln β) 2].In the formula, JN is the function of supersaturation ratio β for the quantity of unit interval unit volume formation nucleus.Supersaturation ratio is defined as real solution concentration C and equilibrium concentration CS ratio.A is the energy term energy level.According to diffusion theory, crystal growth rate can be expressed as JC=k (C-Cs) n, and k is a mass tranfer coefficient, and the n value is between 1-2.Hence one can see that, and nucleation rate and crystal growth rate all depend on mass transfer effect.Mass transfer effect directly affects the speed of nucleus formation and crystal growth, and the speed of these two processes affects the granularity and the size distribution of crystal in the crystalline product.Extremely important factor when therefore, the mass transfer mode is crystallization process.
Adopt technique scheme, the ultrasonic wave radiation has strong orienting effect, and replenishing being arranged and strengthen is to form the required wave action of critical nucleus, so can quicken crystallization process.Ultrasonic wave mainly concentrates on influence to the crystallization nucleation process to the influence of crystallization process, additional sound field in supersaturated solution, because ultrasonic cavitation, the fluctuation of energy of system is very big, and intermolecular force is weakened, and solution viscosity descends, increase the collision opportunity between solute molecule and be easy to nucleation, and pressure and cloud bubble that bubble-break produces help to reduce interface energy, make the nucleus particle with fresh surface become comparatively stable, are continued to grow up to be nucleus.The size that forms crystal is subjected to supersonic frequency and strength control, can obtain varigrained uniform crystal precipitation by the control ultrasonication.Experiment finds, ultrasonic the tripentaerythritol crystallization carried out under low relatively degree of supersaturation, significantly shortened nucleation time, improved crystalline rate, and tripentaerythritol grain size number distribution is diminished.
The power output adjustable size of ultrasonic transducer is suitable for producing the crystalline particle of needs.
Be pooled to the awl end when adopting conical vessel to help tripentaerythritol crystallization gravitational settling.The stirring of adjustable speed axial-flow type helps making the tripentaerythritol of crystallization to be suspended in the solution and is unlikely the excessive shearing force of generation, helps the mass transfer of tripentaerythritol crystallization.Yet mass transfer makes the tripentaerythritol crystalline particle very thin too soon, is unfavorable for the isolated by filtration of tripentaerythritol, so select mixing speed very important according to practical condition.
Condensation liquid tripentaerythritol during use pumps into conical vessel, starts axial-flow type and stirs and supersonic generator, strengthens crystallization and finishes crystallization in 1-6 hour.
The utility model has overcome that the tripentaerythritol crystallization time that prior art exists is long, degree of supersaturation reduces tripentaerythritol content high deficiency in insufficient, the solution during crystallization.With respect to prior art, have following characteristics:
1) adopt awl end formula structure and axial flow to stir, the tripentaerythritol crystallization compiles effect obviously, and tripentaerythritol crystalline particle and solution effect of mass transmitting are strengthened;
2) adopt the adjustable speed agitator, make solution be in best mixing speed, shearing force is little, can obtain suitable tripentaerythritol crystalline form;
3) ultrasonic transducer of employing power output adjustable size can obtain best crystalline particle, and crystallization time shortens greatly;
4) degree of supersaturation reduces fully, and tripentaerythritol content is low in the condensation liquid.
The ultrasound-enhanced tripentaerythritol crystallization apparatus of the utility model can be used for operating process such as tripentaerythritol reactive crystallization, the operation of tripentaerythritol crystalline element and tripentaerythritol crystallization sedimentation.
Description of drawings
Accompanying drawing is a structure chart of the present utility model.
Among the figure: 1, conical vessel, 2, the adjustable speed axial flow type stirrer, 3, ultrasonic transducer, 4, solution inlet port, 5, the crystal solution outlet, 6, the ultrasonic transducer installing hole.
The specific embodiment
The utility model is described in further detail below in conjunction with drawings and Examples.
Among the embodiment as shown in the figure, ultrasound-enhanced tripentaerythritol crystallization apparatus, comprise conical vessel 1, be provided with solution inlet port 4 on the top of conical vessel 1, be provided with crystal solution outlet 5 in the bottom of conical vessel 1, be fixed with adjustable speed axial flow type stirrer 2 on the top of conical vessel 1, be provided with 4 ultrasonic transducer installing holes 6 in the side of conical vessel 1, the ultrasonic transducer 3 of power output adjustable size is installed in each ultrasonic transducer installing hole 6.
Claims (4)
1. ultrasound-enhanced tripentaerythritol crystallization apparatus, comprise container, axial flow type stirrer, solution inlet port (4), crystal solution outlet (5), solution inlet port (4) is arranged on the top of container, crystal solution outlet (5) is arranged on the bottom of container, axial flow type stirrer is fixed in the top of container, it is characterized in that being provided with ultrasonic transducer installing hole (6), ultrasonic transducer (3) is installed in this ultrasonic transducer installing hole in the side of container.
2. ultrasound-enhanced tripentaerythritol crystallization apparatus according to claim 1 is characterized in that described container is conical vessel (1).
3. ultrasound-enhanced tripentaerythritol crystallization apparatus according to claim 1 is characterized in that described axial flow type stirrer is adjustable speed axial flow type stirrer (2).
4. according to claim 1,2 or 3 described ultrasound-enhanced tripentaerythritol crystallization apparatus, it is characterized in that described ultrasonic transducer (3) is the ultrasonic transducer of power output adjustable size.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009200429064U CN201445824U (en) | 2009-06-29 | 2009-06-29 | Ultrasonic strengthened tri-pentaerythritol crystallizer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009200429064U CN201445824U (en) | 2009-06-29 | 2009-06-29 | Ultrasonic strengthened tri-pentaerythritol crystallizer |
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| Publication Number | Publication Date |
|---|---|
| CN201445824U true CN201445824U (en) | 2010-05-05 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2009200429064U Expired - Fee Related CN201445824U (en) | 2009-06-29 | 2009-06-29 | Ultrasonic strengthened tri-pentaerythritol crystallizer |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102872612A (en) * | 2012-10-15 | 2013-01-16 | 中国工程物理研究院化工材料研究所 | Ultrasonic crystallizer |
| CN110354777A (en) * | 2019-07-31 | 2019-10-22 | 河北兰升生物科技有限公司 | Reaction unit of a kind of ultrasonic wave added crystallization and application thereof and preparation method using the device |
-
2009
- 2009-06-29 CN CN2009200429064U patent/CN201445824U/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102872612A (en) * | 2012-10-15 | 2013-01-16 | 中国工程物理研究院化工材料研究所 | Ultrasonic crystallizer |
| CN102872612B (en) * | 2012-10-15 | 2013-11-27 | 中国工程物理研究院化工材料研究所 | Ultrasonic crystallizer |
| CN110354777A (en) * | 2019-07-31 | 2019-10-22 | 河北兰升生物科技有限公司 | Reaction unit of a kind of ultrasonic wave added crystallization and application thereof and preparation method using the device |
| CN110354777B (en) * | 2019-07-31 | 2024-03-12 | 兰升生物科技集团股份有限公司 | Method for preparing cis-para-substituted cyclohexylamino nitrile maleate by using reaction device of ultrasonic-assisted crystallization |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20100505 Termination date: 20160629 |
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| CF01 | Termination of patent right due to non-payment of annual fee |