CN107433177A - A kind of dynamic pipe reaction device and method thereof for preparing micro-nano powder - Google Patents

A kind of dynamic pipe reaction device and method thereof for preparing micro-nano powder Download PDF

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Publication number
CN107433177A
CN107433177A CN201710628945.1A CN201710628945A CN107433177A CN 107433177 A CN107433177 A CN 107433177A CN 201710628945 A CN201710628945 A CN 201710628945A CN 107433177 A CN107433177 A CN 107433177A
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CN
China
Prior art keywords
dynamic
tubular reactor
material treatment
nano powder
constant flow
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201710628945.1A
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Chinese (zh)
Inventor
李立良
陈冬梅
宋兰英
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.)
Neville Technology (shenzhen) Co Ltd
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Neville Technology (shenzhen) Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Priority to CN201710628945.1A priority Critical patent/CN107433177A/en
Publication of CN107433177A publication Critical patent/CN107433177A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18Stationary reactors having moving elements inside
    • B01J19/1812Tubular reactors
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00Other mixers; Mixing plants; Combinations of mixers
    • B01F33/80Mixing plants; Combinations of mixers
    • B01F33/82Combinations of dissimilar mixers
    • B01F33/822Combinations of dissimilar mixers with moving and non-moving stirring devices in the same receptacle
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F2101/00Mixing characterised by the nature of the mixed materials or by the application field
    • B01F2101/2204Mixing chemical components in generals in order to improve chemical treatment or reactions, independently from the specific application

Abstract

A kind of dynamic pipe reaction device and method thereof for preparing micro-nano powder, the present invention relates to micro-nano powder preparing technical field;No.1 material treatment trough and No. two material treatment troughs are connected with by pipeline respectively in two openings of the lower end T-shape impinging streams mixer of dynamic tubular reactor;No.1 constant flow pump is connected with connecting pipe between described No.1 material treatment trough and dynamic tubular reactor;No. two constant flow pumps are connected with connecting pipe between No. two material treatment troughs and dynamic tubular reactor;The inside of described dynamic tubular reactor is provided with dynamic mixer;The lower end of described dynamic mixer and the output axis connection of electric rotating machine;The upper end of described dynamic tubular reactor is connected by pipeline with ultrasonic aging groove.The mixing of its mass transfer is fast, and continuous-stable, controllability is strong, and amplification is easy, and energy-saving, it has very strong universality.

Description

A kind of dynamic pipe reaction device and method thereof for preparing micro-nano powder
Technical field
The present invention relates to micro-nano powder preparing technical field, and in particular to a kind of dynamic tubular type for preparing micro-nano powder Consersion unit and its method.
Background technology
Micro-nano powder material is a kind of solid particle material for the transitional region having a common boundary between elementide and macro object Material, its bulk effect, quantum size effect for being in nanoscale scope, showing uniqueness at least one-dimensional in three dimensions Should, skin effect and macro quanta tunnel effect, have completely different in the electricity of bulk material, magnetics, optics, calorifics, change The property such as or mechanics, is widely used in electronic device, medical science and health, space flight, aviation and space exploration, environment, resource With energy and biotechnology field, have broad application prospects and huge economic benefit.
The preparation method of micro Nano material largely determines the performance, price and application of micro Nano material, is Its basis applied.Therefore, in the evolution of micro Nano material, the technology of preparing of micro Nano material is always the heat studied Point and difficult point.The research of recent two decades, the method for manually preparing micro Nano material have obtained very big development, wherein with atom, Molecule is elementary cell, and the technology path of micro nano structure is built into raw material by atom, the aggregation of molecule and assembling It is less demanding, there is the characteristics of energy-saving, green, be to prepare the route that micro-nano powder generally uses at present.Wherein Chemical liquid phase reaction have that equipment is simple, raw material is readily available, purity is high, uniformity is good, chemical composition control is accurate, is easy to put The advantages that big, become the preparation method of micro-nano powder widely used in current laboratory and industrial production.Generally, it is chemical Liquid phase method prepare micro-nano powder be since the glass container in laboratory, then by lab scale, pilot scale until industrialization by Level amplification, puts into by prolonged research and development and substantial amounts of manpower and materials, scale amount is finally realized in the reactor of big volume Production.
Industrial typical still reaction operation is typically the various reaction raw materials of order addition into reactor, is stirred in machinery Mix lower reaction and prepare micro-nano powder.This still reaction mode is for those reaction speeds are slow, mass-and heat-transfer is less demanding Reaction is that suitable, slower reaction speed has ensured that enough mass-and heat-transfer mixing require so that before reaching reaction and starting, Uniform mass-and heat-transfer mixing is had been realized in require.But for reaction speed is fast, product is sticky or one kind of free settling for generation For reaction, because the churned mechanically mass transfer of still reaction and scattered intensity are relatively low, it, which stirs mass transfer, makes what material was well mixed Speed disperses the ability of sticky or easy sedimentation products not far below the speed that reaction is carried out, and the relatively low intensity that is stirred Foot, so that preparation-obtained micro-nano powder is present, serious Size Distribution is wide, reunite serious, stability and uniformity difference etc. Problems.
A kind of SiO is given to solve deficiency, patent of invention CN102120585B existing for still reaction2Micro-nano ball Preparation method and micro- reaction system, it uses a kind of micro-reaction device of intensified by ultrasonic wave to realize the positive silicic acid second of ammonia catalyzing hydrolysis Ester prepares SiO2Rapid mass transfer and mixing require, the reaction unit for prepare viscosity is low, product settle it is slow such as SiO2It is suspended A kind of Newtonian fluid product of liquid is suitable.Patent of invention CN102151533B is using micro mixing device and strengthens micro- reaction dress The mode of combination is put, two processes of mixing and reaction is carried out respectively in different devices, SiO can be realized2、Ni、Fe3O4 Deng the preparation of nano particle.But for such as MgCl2+ 2NaOH=Mg (OH)2↓+2NaCl a kind of contact is reacted and reaction production Thing is the supper-fast reaction of very sticky non-newtonian fluid, and such as 2AgNO3+2N2H4·H2O=2Ag ↓+2NH4NO3+N2↑+H2O A kind of contact i.e. reaction and the ultrafast response of reaction product free settling separation for, patent CN102151533B use The method of segmentation mixing and reaction is not just suitable for the supper-fast reaction that contact is reacted, and patent in different reaction units The microreactor of mixed cell internals is provided with the microchannel that CN102120585B is used, as easily blocking and not applying to In the reaction that the reaction product or product free settling of non-Newton fluid characteristic separate.
Therefore, it is sticky non-newtonian fluid or product free settling point for this one kind contact i.e. reaction and reaction product From reaction, it is necessary to change thinking, design new reaction unit and develop new technology of preparing.
The content of the invention
It is reasonable in design, make in view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of simple in construction With the dynamic pipe reaction device and method thereof for easily preparing micro-nano powder, the mixing of its mass transfer is fast, continuous-stable, controllability By force, amplification is easy, and energy-saving, it has very strong universality, can be applied to many contacts and react, and reaction product is The laboratory of sticky non-newtonian fluid or the micro-nano powder of product free settling separation is prepared until industrialized production.
To achieve the above object, the technical solution adopted by the present invention is:It includes No.1 material treatment trough, at No. two materials Manage groove, dynamic tubular reactor, electric rotating machine, No.1 constant flow pump, No. two constant flow pumps, dynamic mixer, ultrasonic aging groove;It is described Dynamic tubular reactor two of lower end T-shape impinging streams mixer openings on No.1 material is connected with by pipeline respectively Treatment trough and No. two material treatment troughs;Connect on connecting pipe between described No.1 material treatment trough and dynamic tubular reactor It is connected to No.1 constant flow pump;No. two are connected with connecting pipe between No. two described material treatment troughs and dynamic tubular reactor Constant flow pump;The inside of described dynamic tubular reactor is provided with dynamic mixer;The lower end of described dynamic mixer and rotation The output axis connection of motor;The upper end of described dynamic tubular reactor is connected by pipeline with ultrasonic aging groove.
The preparation process of the present invention is as follows:
1st, dissolved the reaction mass necessarily matched in No.1 material treatment trough, No. two material treatment troughs respectively, The processing such as heating;
2nd, will be handled well simultaneously in No.1 material treatment trough, No. two material treatment troughs with No.1 constant flow pump, No. two constant flow pumps Reaction solution at a high speed be pumped into opposite directions in dynamic tubular reactor;
3 while electric rotating machine is opened, dynamic mixer is rotated in dynamic tubular reactor;
4th, the product come out from dynamic tubular reactor is flowed into ultrasonic aging groove, carries out ultrasonic agitation ageing wherein Processing;
5th, the good product of ripening is filtered, washs, dries, that is, obtains desired micro-nano powder.
Further, it is 0.5~5m/s flow velocity to be reacted in described step 2.
Further, the rotating speed of dynamic mixer is 50~1500rpm in described step 3.
After said structure, the present invention has the beneficial effect that:A kind of dynamic for preparing micro-nano powder of the present invention Pipe reaction device and method thereof, the mixing of its mass transfer is fast, and continuous-stable, controllability is strong, and amplification is easy, and energy-saving, it has Very strong universality, many contacts can be applied to and reacted, and reaction product is that sticky non-newtonian fluid or product are easily heavy The laboratory for dropping the micro-nano powder of separation is prepared until industrialized production, and the present invention has simple in construction, and it is reasonable to set, and makes Low cost and other advantages.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing There is the required accompanying drawing used in technology description to be briefly described, it should be apparent that, drawings in the following description are only this Some embodiments of invention, for those of ordinary skill in the art, without having to pay creative labor, may be used also To obtain other accompanying drawings according to these accompanying drawings.
Fig. 1 is the structural representation of the present invention.
Description of reference numerals:
1, No. two material treatment trough 2 of No.1 material treatment trough, dynamic tubular reactor 3, electric rotating machine 4,
No.1 constant flow pump 5, No. two constant flow pumps 6, dynamic mixer 7, ultrasonic aging grooves 8.
Embodiment
The present invention is further illustrated below in conjunction with the accompanying drawings.
Referring to as shown in figure 1, the technical scheme that present embodiment uses is:It includes No.1 material treatment trough 1, two Number material treatment trough 2, dynamic tubular reactor 3, electric rotating machine 4,5, No. two constant flow pumps 6 of No.1 constant flow pump, dynamic mixer 7, Ultrasonic aging groove 8;Pass through respectively in two openings of the lower end T-shape impinging streams mixer of described dynamic tubular reactor 3 Pipeline is connected with No.1 material treatment trough 1 and No. two material treatment troughs 2;Described No.1 material treatment trough 1 is anti-with dynamic tubular type Answer and No.1 constant flow pump 5 is connected with the connecting pipe between device 3;No. two described material treatment troughs 2 and dynamic tubular reactor 3 Between connecting pipe on be connected with No. two constant flow pumps 6;The inside of described dynamic tubular reactor 3 is provided with dynamic mixer 7; The lower end of described dynamic mixer 7 and the output axis connection of electric rotating machine 4;The upper end of described dynamic tubular reactor 3 leads to Piping is connected with ultrasonic aging groove 8.
The operation principle of present embodiment:Dynamic tubular reactor 3 is the core component of reaction system, combines and hits The double dominant of stream and tubular type dynamic mixing is hit, its underpart is the T-shape impinging streams mixer of an opening upwards, can be two kinds of bodies The liquid that product flow is more or less the same, high flow rate hit quick mixing in opposite directions, realize that quick mass transfer mixing and reaction require, tentatively The material of hybrid reaction flows up through the dynamic mixer 7 being placed in dynamic tubular reactor 3, and dynamic mixer 7 is rotating Under the drive of motor 4, further agitation mixing is carried out to the material flowed through, on the one hand strong agitation further enhances anti- The progress answered, on the other hand greatly improve the mobility of the sticky reaction product of non-newtonian fluid and reduce free settling production The sedimentation separation of thing, so as to prevent the lasting progress of the blocking of reacting pipe and reaction;Ultrasonic aging groove therein is to stir The bottom for mixing bucket is provided with ultrasonic oscillator, and ultrasonic wave has the function that to promote crystallization and prevents micro-nano granules from reuniting, so as to Ripening temperature can be reduced and reduce the ripening time.
The preparation process of present embodiment is as follows:
1st, the reaction mass necessarily matched is carried out in 1, No. two material treatment trough 2 of No.1 material treatment trough respectively molten The processing such as solution, heating;
2nd, will be located simultaneously in 1, No. two material treatment trough 2 of No.1 material treatment trough with 5, No. two constant flow pumps 6 of No.1 constant flow pump The reaction solution managed is pumped into dynamic tubular reactor 3 at a high speed in opposite directions, and reaction solution flow control scope is in 0.5~5m/s;
3 while electric rotating machine 4 is opened, dynamic mixer 7 is rotated in dynamic tubular reactor 3, dynamic mixes The range of speeds of device 7 is in 50~1500rpm;
4th, the product come out from dynamic tubular reactor 3 is flowed into ultrasonic aging groove 8, carries out being stirred by ultrasonic wherein old Change is handled;
5th, the good product of ripening is filtered, washs, dries, that is, obtains desired micro-nano powder.
After said structure, present embodiment has the beneficial effect that:It is prepared by one kind described in present embodiment The dynamic pipe reaction device and method thereof of micro-nano powder, the mixing of its mass transfer is fast, and continuous-stable, controllability is strong, and amplification is easy, Energy-saving, it has very strong universality, can be applied to many contacts and react, and reaction product is sticky non newtonian The laboratory of fluid or the micro-nano powder of product free settling separation prepares until industrialized production, the present invention have structure letter Single, it is reasonable to set, the advantages that low manufacture cost.
It is described above, it is merely illustrative of the technical solution of the present invention and unrestricted, those of ordinary skill in the art are to this hair The other modifications or equivalent substitution that bright technical scheme is made, without departing from the spirit and scope of technical solution of the present invention, It all should cover among scope of the presently claimed invention.

Claims (4)

  1. A kind of 1. dynamic pipe reaction equipment for preparing micro-nano powder, it is characterised in that:It includes No.1 material treatment trough, two Number material treatment trough, dynamic tubular reactor, electric rotating machine, No.1 constant flow pump, No. two constant flow pumps, dynamic mixer, ultrasound are old Change groove;Connected respectively by pipeline in two openings of the lower end T-shape impinging streams mixer of described dynamic tubular reactor There are No.1 material treatment trough and No. two material treatment troughs;Company between described No.1 material treatment trough and dynamic tubular reactor No.1 constant flow pump is connected with adapter road;On connecting pipe between No. two described material treatment troughs and dynamic tubular reactor It is connected with No. two constant flow pumps;The inside of described dynamic tubular reactor is provided with dynamic mixer;Described dynamic mixer Lower end and the output axis connection of electric rotating machine;The upper end of described dynamic tubular reactor is connected by pipeline and ultrasonic aging groove Connect.
  2. A kind of 2. method for preparing micro-nano powder, it is characterised in that:Its preparation process is as follows:
    (1), the reaction mass necessarily matched is dissolved in No.1 material treatment trough, No. two material treatment troughs respectively, added The processing such as heat;
    (2), will be handled well simultaneously in No.1 material treatment trough, No. two material treatment troughs with No.1 constant flow pump, No. two constant flow pumps Reaction solution is pumped into dynamic tubular reactor at a high speed in opposite directions;
    (3) while electric rotating machine is opened, dynamic mixer is rotated in dynamic tubular reactor;
    (4), the product come out from dynamic tubular reactor is flowed into ultrasonic aging groove, carries out being stirred by ultrasonic at ageing wherein Reason;
    (5), the good product of ripening is filtered, washs, dries, that is, obtains desired micro-nano powder.
  3. A kind of 3. method for preparing micro-nano powder according to claim 2, it is characterised in that:In described step (2) Reaction flow velocity is 0.5~5m/s.
  4. A kind of 4. method for preparing micro-nano powder according to claim 2, it is characterised in that:In described step (3) The rotating speed of dynamic mixer is 50~1500rpm.
CN201710628945.1A 2017-07-28 2017-07-28 A kind of dynamic pipe reaction device and method thereof for preparing micro-nano powder Pending CN107433177A (en)

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CN201710628945.1A CN107433177A (en) 2017-07-28 2017-07-28 A kind of dynamic pipe reaction device and method thereof for preparing micro-nano powder

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Application Number Priority Date Filing Date Title
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112657442A (en) * 2020-12-04 2021-04-16 中北大学 Multi-module impact-coalescence reactor and use method thereof
CN116443834A (en) * 2023-04-13 2023-07-18 云南云天化股份有限公司 Method for continuously synthesizing ferric phosphate by using microreactor

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102151533A (en) * 2011-01-26 2011-08-17 深圳航天科技创新研究院 Preparation method of micro-nanometer powder, reinforced micro-reaction device and micro-reaction system
CN103203213A (en) * 2012-01-16 2013-07-17 清华大学 Liquid phase impinging stream reactor with controllable acidity
US20150202598A1 (en) * 2012-07-06 2015-07-23 Teknologisk Institut Method of preparing a catalytic structure
CN207042475U (en) * 2017-07-28 2018-02-27 纳威科技(深圳)有限公司 A kind of dynamic pipe reaction device for preparing micro-nano powder

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102151533A (en) * 2011-01-26 2011-08-17 深圳航天科技创新研究院 Preparation method of micro-nanometer powder, reinforced micro-reaction device and micro-reaction system
CN103203213A (en) * 2012-01-16 2013-07-17 清华大学 Liquid phase impinging stream reactor with controllable acidity
US20150202598A1 (en) * 2012-07-06 2015-07-23 Teknologisk Institut Method of preparing a catalytic structure
CN207042475U (en) * 2017-07-28 2018-02-27 纳威科技(深圳)有限公司 A kind of dynamic pipe reaction device for preparing micro-nano powder

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
冯若, 南京大学出版社 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112657442A (en) * 2020-12-04 2021-04-16 中北大学 Multi-module impact-coalescence reactor and use method thereof
CN116443834A (en) * 2023-04-13 2023-07-18 云南云天化股份有限公司 Method for continuously synthesizing ferric phosphate by using microreactor

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Application publication date: 20171205

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