CN102872612B - Ultrasonic crystallizer - Google Patents

Ultrasonic crystallizer Download PDF

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Publication number
CN102872612B
CN102872612B CN2012103905251A CN201210390525A CN102872612B CN 102872612 B CN102872612 B CN 102872612B CN 2012103905251 A CN2012103905251 A CN 2012103905251A CN 201210390525 A CN201210390525 A CN 201210390525A CN 102872612 B CN102872612 B CN 102872612B
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ultrasonic
reactor
vibrating bar
ultrasound wave
wave vibrating
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CN102872612A (en
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徐瑞娟
康彬
黄辉
马华
刘渝
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Institute of Chemical Material of CAEP
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Institute of Chemical Material of CAEP
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Abstract

The invention discloses an ultrasonic crystallizer. The ultrasonic crystallizer comprises an ultrasonic generator, a reaction kettle and at least one ultrasonic vibrating bar, wherein the ultrasonic generator is arranged outside the reaction kettle; the ultrasonic vibrating bar is arranged in the reaction kettle, and is electrically connected with the ultrasonic generator through a signal wire; the reaction kettle comprises a stirrer for mixing materials; and the stirrer is used for stirring the materials inside the reaction kettle. By the ultrasonic crystallizer, ultrasonic energy can directly act on the materials, so that the energy can be prevented from being lost. Compared with other ultrasonic crystallizer with equal acting effects, the ultrasonic crystallizer has the advantages that the ultrasonic crystallizer is low in ultrasonic power; ultrasonic fields are uniformly distributed in the materials; the cavitation corrosion condition of the ultrasonic vibrating bar is easy to detect, and the ultrasonic vibrating bar is easy to replace; and the ultrasonic vibrating bar has a baffle stirring effect in the kettle, so that the materials can be uniformly mixed.

Description

Ultrasonic crystallizer
Technical field
The present invention relates to a kind of crystallizer, be specifically related to a kind of ultrasonic crystallizer.
Background technology
In recent years, ultrasonic technology has been subject to extensive concern and the application of the research fields such as chemical industry, food, biology, medicine.Utilize the ultrasonic cavitation effect, can accelerate the reaction speed in chemical reaction process, improve reaction yield.For the compound crystallization process, can effectively control product particle form, crystal quality and size distribution.Therefore, the application in the industrial crystallization field has important function to ultrasonic crystallizer for the development ultrasonic technology.
How ultrasonic energy being introduced in crystallization kettle effectively, is the key of ultrasonic crystallizer success.At present, on market, existing ultrasonic introducing mode mainly contains following several types: 1, luffing rod-type ultrasonic reactor.As patent 2004201028.2 vertical cutting type high temperature ultrasonic processors, the ultrasonic wave liquid phase treating apparatus that patent 200620064182 is announced, and the ultrasonic processor of patent 200820189096 announcements etc.This class ultrasonic reactor is too concentrated and is caused the ultrasonic probe surface to be subjected to cavitation corrosion serious due to energy on the one hand, has the reaction liquid from polluting problem, is subjected on the other hand action space and energy limited, is difficult to carry out the through engineering approaches amplification.2, directly in reactor surface, ultrasonic transducer is installed.The patent US7244307B2 that U.S. 2007 application is arranged that belongs to this class ultrasonic reactor, the patent WO0035579 of Britain's application in 2007, Chinese 200810030364 patents, 200620035230.2 patents and 200520080907 etc.This class ultrasonic reactor is that ultrasonic transducer is directly installed on the outer wall of metallic conduit or canister, and this device makes metallic conduit or canister wall surface bored a hole by cavitation corrosion, thereby causes scrapping of whole ultrasonic reactor.3, at the outside ultrasonic vibrating plate that sealing is installed of reactor, ultrasonic transducer is packaged in ultrasonic vibrating plate, and ultrasonic vibrating plate and reactor outer wall form the interlayer that can supply heat exchange medium to pass through.What belong to this class ultrasonic reactor has a Chinese patent 200510042563.The advantage of this class ultrasonic reactor is that ultrasonic vibrating plate is easy to after by cavitation corrosion change, but shortcoming is that the ultrasonic energy utilization rate is low, ultrasonic wave is after passing through heat exchange medium, the loss of reactor wall reflection multilayer, the energy that is applied to material in reactor becomes very low, in addition, these class ultrasonic reactor mechanical oscillation are large, and noise is large.
Summary of the invention
The present invention has overcome the deficiencies in the prior art, and a kind of ultrasonic crystallizer is provided, and perishable to reactor wall in prior art to be solved, the ultrasonic energy utilization rate is low, and mechanical oscillation are large, the large problem of noise.
For solving above-mentioned technical problem, the present invention by the following technical solutions:
A kind of ultrasound wave vibrating bar, described ultrasound wave vibrating bar comprise a hollow cylinder and at least one ultrasonic transducer, and described ultrasonic transducer is arranged on the hollow cylinder inwall.
Further technical scheme is that the hollow cylinder top is provided with connecting rod, and the connecting rod top is provided with the flange connector, and described ultrasound wave vibrating bar is connected on the reactor end socket by bump joint.
Further technical scheme is that connecting rod lower end and hollow cylinder are tightly connected, and connecting rod upper end and the flange connector of described ultrasound wave vibrating bar are tightly connected.
Further technical scheme is that the supersonic transducer frequency scope is 10 KHz to 135 KHzs.
Further technical scheme is mounted on the hollow cylinder inwall ultrasonic transducer according to the grouping of upper, middle and lower, installation site, and independent start and stop, to meet different liquid level instructions for uses.
Further technical scheme is a kind of ultrasonic crystallizer, comprises supersonic generator, reactor, and supersonic generator is arranged on outside reactor; Described ultrasonic crystallizer also comprises ultrasound wave vibrating bar, and ultrasound wave vibrating bar is arranged in reactor, is fixed on the reactor end socket by flange; Described ultrasound wave vibrating bar is electrically connected to supersonic generator by holding wire; Described reactor comprises: for the agitator of mixing of materials, described agitator is for the stirring of reactor materials inside.
Further technical scheme is that reactor also comprises that described interlayer is arranged on the reactor outer wall be used to controlling the interlayer of temperature.
Further technical scheme is that described agitator comprises shaft, stirring vane, and described shaft is arranged on the central shaft position of reactor.
Further technical scheme is, on described reactor end socket, the bump joint more than 1 or 1 is arranged.
Further technical scheme is that ultrasound wave vibrating bar is more than 1 or 1, and described 1 above ultrasound wave vibrating bar is symmetrical around shaft.
Further technical scheme is that the ultrasound wave vibrating bar bottom level is positioned on stirring vane.
Further technical scheme is that the hollow cylinder upper end height of ultrasound wave vibrating bar is positioned at reactor and uses below liquid level.
Compared with prior art, the invention has the beneficial effects as follows: can avoid energy loss by the ultrasonic energy direct effect to material, compare other ultrasonic crystallizer of equivalent effect effect, ultrasonic power is less; Ultrasonic field distributes more even in material; For the Under Ultrasonic Vibration rod, be subjected to the cavitation corrosion situation to be easy to check and change; Ultrasonic wave shake the rod in still, also can play the effect of mixing baffle, make mixing of materials more even; According to the reactor size, the ultrasonic wave excellent size (as length and width) of shaking is adjustable, and the quantity of ultrasonic transducer can be according to the ultrasonic wave excellent size adjustment of shaking, and ultrasonic power is easy to industry and amplifies.
The accompanying drawing explanation
Fig. 1 is the ultrasound wave vibrating bar structural representation of one embodiment of the invention.
Fig. 2 is the ultrasonic mold structure schematic diagram of another embodiment of the present invention.
The specific embodiment
The present invention is further elaborated below in conjunction with accompanying drawing.
As shown in Figure 1, Fig. 1 shows the ultrasound wave vibrating bar structural representation of one embodiment of the invention.The present embodiment ultrasound wave vibrating bar, as shown in Figure 1, in the present embodiment, ultrasound wave vibrating bar comprises hollow cylinder 5, hollow cylinder 5 can be used to installing ultrasonic transducer 6 section within it, specific embodiment is mounted on the inwall of hollow cylinder 5, in the present embodiment, ultrasonic transducer 6 can be arranged on the optional position of hollow cylinder 5 inwalls, if be bottom, can be also on wall, specific embodiment is, in the present embodiment, ultrasonic transducer 6 is arranged on wall and the bottom of hollow cylinder 5, can take full advantage of the hollow cylinder inner space like this, reach largeizationr of function.The shape of hollow cylinder 5 can be the cylinder type hollow cylinder, it can be also the multi-edge column-shaped hollow cylinder, or other can install other shape hollow cylinders that ultrasonic transducer is realized identical functions, specific embodiment is that the shape of the present embodiment hollow core cylinder 5 is circular hollow cylinders.The top of hollow cylinder 5 is provided with connecting rod 4, connecting rod 4 tops are provided with flange connector 3, arranging of flange connector 3 can be played the good effect that is connected and fixed and certain sealing function, and the present embodiment ultrasound wave vibrating bar is connected on the reactor end socket by bump joint 3.Thereby realize detachable being fixed in reactor.As preferred embodiment, in this enforcement, the bottom of connecting rod 4 and hollow cylinder 5 are tightly connected, and concrete embodiment is, the bottom of connecting rod 4 and hollow cylinder 5 seal weldings in this enforcement, seal welding can make connecting rod 4 better with the connection sealing of hollow cylinder 5; The top of connecting rod 4 and flange connector 3 are tightly connected.Ultrasonic transducer 6 in the present embodiment ultrasound wave vibrating bar has one at least, a plurality of ultrasonic transducers can the intensified response effect, the quantity of ultrasonic transducer 6 can be regulated according to hollow cylinder 5 size dimensions, the size dimension of hollow cylinder 5 can be determined according to the space of reactor and actual needs, specific embodiment is, in this enforcement, the quantity of ultrasonic transducer 6 is 9, to meet actual needs.Ultrasonic transducer 6 in the present embodiment ultrasound wave vibrating bar can divide into groups according to installation site, every group of independence start and stop, the grouping number requires by liquid level according to reactor and the length of hollow cylinder 5 is determined, specific embodiment is that in this enforcement, 9 ultrasonic transducers 6 are divided into three groups of upper, middle and lowers.In the present embodiment, the frequency range of ultrasonic transducer 6 is 10 KHz to 135 KHzs, and concrete frequency can be regulated according to actual needs.Ultrasonic transducer 6 is electrically connected to outside single group supersonic generator 1 by holding wire 2, list organize supersonic generator 1 can a plurality of combinations and ultrasonic transducer 6 be used in conjunction with and realize its function.
As shown in Figure 2, Fig. 2 shows the structural representation of the ultrasonic crystallizer of another embodiment of the present invention.The ultrasonic crystallizer of the present embodiment as shown in Figure 2, comprises the ultrasound wave vibrating bar 16 described in first embodiment in reactor and at least one this specification, and in this enforcement, ultrasound wave vibrating bar 16 is electrically connected to combination ultrasonic generator 12 by holding wire.Ultrasound wave vibrating bar 16 is connected with the reactor end socket 14 on reactor by flange connector 15, thereby is fixed in reactor.The ultrasonic crystallizer of the present embodiment also comprises agitator, stirring for mixing of materials, agitator comprises stirring motor 11, shaft 13 and stirring vane 18, stirring motor 11 is arranged on the top of reactor, shaft 13 is connected with the power transmission shaft of stirring motor, when stirring motor rotates, drives the rotation of shaft 13, and stirring vane 18 is arranged on the bottom of shaft 13, shaft 13 drives the rotation of stirring vane, thereby realizes the agitating function of mixing of materials.As preferred embodiment, in the present embodiment, shaft 13 is arranged on the central shaft position of reactor, can better realize stirring evenly of mixing of materials like this.In the present embodiment, ultrasound wave vibrating bar 16 can be a plurality of, preferred embodiment, a plurality of ultrasound wave vibrating bars are evenly arranged in around shaft 13, make like this ultrasonic field in reactor more even, played simultaneously the effect of material baffle, strengthen the material mixed effect, specific embodiment is, in the present embodiment, ultrasound wave vibrating bar 16 is four, four ultrasound wave vibrating bars be symmetricly set on shaft 13 around, four ultrasound wave vibrating bars are electrically connected to two combination ultrasonic generators 12 by holding wire respectively.As preferred embodiment, in this enforcement, the outer wall of reactor is provided with the interlayer 17 be used to controlling temperature, thereby interlayer 17 is controlled the interior temperature of still of reaction by the water that injects relevant temperature.As preferred embodiment, in this enforcement, ultrasound wave vibrating bar 16 bottom level are positioned on stirring vane 18.The hollow cylinder upper end height of ultrasound wave vibrating bar 16 is positioned at reactor to be used below liquid level.
" embodiment " who speaks of in this manual, " another embodiment ", " embodiment ", etc., refer to specific features, structure or the characteristics in conjunction with this embodiment, described and be included at least one embodiment that the application's generality describes.A plurality of local appearance statement of the same race is not necessarily to refer to same embodiment in specification.Furthermore, while in conjunction with any embodiment, describing a specific features, structure or characteristics, what advocate is to realize that in conjunction with other embodiment this feature, structure or characteristics also fall within the scope of the invention.
Although invention has been described with reference to a plurality of explanatory embodiment invented here, but, should be appreciated that, those skilled in the art can design a lot of other modification and embodiments, and these are revised and within embodiment will drop on the disclosed principle scope and spirit of the application.More particularly, in the scope of, accompanying drawing open in the application and claim, can carry out multiple modification and improvement to building block and/or the layout of subject combination layout.Except modification that building block and/or layout are carried out with improving, to those skilled in the art, other purposes will be also obvious.

Claims (1)

1. a ultrasonic crystallizer, comprise supersonic generator, reactor, and supersonic generator is arranged on outside reactor; It is characterized in that described ultrasonic crystallizer also comprises ultrasound wave vibrating bar, described ultrasound wave vibrating bar comprises a hollow cylinder and at least one ultrasonic transducer, and described ultrasonic transducer is arranged on the hollow cylinder inwall; Described hollow cylinder top is provided with connecting rod, and the connecting rod top is provided with the flange connector, and described ultrasound wave vibrating bar is connected on the reactor end socket by the flange connector; Connecting rod lower end and hollow cylinder are tightly connected, and connecting rod upper end and the flange connector of described ultrasound wave vibrating bar are tightly connected; Described ultrasonic transducer divides into groups according to installation site, every group of independence start and stop, and the supersonic transducer frequency scope is 10 KHz to 135 KHzs; Ultrasound wave vibrating bar is arranged in reactor, and described ultrasound wave vibrating bar is electrically connected to supersonic generator by holding wire; Described reactor comprises: for the agitator of mixing of materials, described agitator is for the stirring of reactor materials inside; Described reactor also comprises that described interlayer is arranged on the reactor outer wall be used to controlling the interlayer of temperature; Described agitator comprises shaft, stirring vane, and described shaft is arranged on the central shaft position of reactor; Described ultrasound wave vibrating bar is more than 1 or 1, and described 1 above ultrasound wave vibrating bar is symmetrical around shaft; Described ultrasound wave vibrating bar bottom level is positioned on stirring vane, and the hollow cylinder upper end height of described ultrasound wave vibrating bar is positioned at reactor to be used below liquid level.
CN2012103905251A 2012-10-15 2012-10-15 Ultrasonic crystallizer Active CN102872612B (en)

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CN103172476A (en) * 2013-04-08 2013-06-26 中国工程物理研究院化工材料研究所 Preparation method of submicron particle 1-oxo-diamino-3, 5-dinitropyrazine explosive
CN103301648A (en) * 2013-06-14 2013-09-18 宿迁科思化学有限公司 P-hydroxy benzaldehyde crystallizing kettle
CN105346871A (en) * 2015-11-27 2016-02-24 安徽六国化工股份有限公司 Storing tank for corrosive medium
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

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1169711A (en) * 1994-12-15 1998-01-07 纳幕尔杜邦公司 Crystallization of adipic acid
CN2582764Y (en) * 2002-12-10 2003-10-29 英菲龙超声科技(深圳)有限公司 Tubular ultrasonic vibration generator
CN101274157A (en) * 2006-12-31 2008-10-01 中国科学院过程工程研究所 Cross current intrinsic cycle ultrasonic and microwave leaching reactor and leaching method thereof
CN101636223A (en) * 2007-03-19 2010-01-27 普罗索尼克斯有限公司 The method for preparing crystal
CN201445824U (en) * 2009-06-29 2010-05-05 江苏瑞阳化工股份有限公司 Ultrasonic strengthened tri-pentaerythritol crystallizer
CN102423545A (en) * 2011-10-21 2012-04-25 北京弘祥隆生物技术股份有限公司 Ultrasonic crystallizing equipment used in natural product or chemical agent crystallization and purification

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7244307B2 (en) * 2002-05-31 2007-07-17 Accentus Plc Production of crystalline materials by using high intensity ultrasound

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1169711A (en) * 1994-12-15 1998-01-07 纳幕尔杜邦公司 Crystallization of adipic acid
CN2582764Y (en) * 2002-12-10 2003-10-29 英菲龙超声科技(深圳)有限公司 Tubular ultrasonic vibration generator
CN101274157A (en) * 2006-12-31 2008-10-01 中国科学院过程工程研究所 Cross current intrinsic cycle ultrasonic and microwave leaching reactor and leaching method thereof
CN101636223A (en) * 2007-03-19 2010-01-27 普罗索尼克斯有限公司 The method for preparing crystal
CN201445824U (en) * 2009-06-29 2010-05-05 江苏瑞阳化工股份有限公司 Ultrasonic strengthened tri-pentaerythritol crystallizer
CN102423545A (en) * 2011-10-21 2012-04-25 北京弘祥隆生物技术股份有限公司 Ultrasonic crystallizing equipment used in natural product or chemical agent crystallization and purification

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