CN104194005B - A kind of powder ELUTION METHOD and device - Google Patents

A kind of powder ELUTION METHOD and device Download PDF

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Publication number
CN104194005B
CN104194005B CN201410372958.3A CN201410372958A CN104194005B CN 104194005 B CN104194005 B CN 104194005B CN 201410372958 A CN201410372958 A CN 201410372958A CN 104194005 B CN104194005 B CN 104194005B
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elution
eluent
eluant
tower
eluted
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CN104194005A (en
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张代军
王林志
谭陆西
黎静
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Chongqing Institute of Green and Intelligent Technology of CAS
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Chongqing Institute of Green and Intelligent Technology of CAS
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/582Recycling of unreacted starting or intermediate materials

Abstract

The invention discloses a kind of powder ELUTION METHOD, this method is specially:Raw material to be eluted is added in elution tower, eluant, eluent is added in separated device, and eluant, eluent gasifies in separated device and enters condenser, elution tower is entered after condenser liquefies and is fully contacted with by raw material to be eluted;The mixing liquid eluted, carries out initial gross separation in recovery tower, and remaining then flows back to separated device, so completes a circulation.Without manually nursing after present invention charging etc. is stable, automatically continuously production can be achieved, operating cost is low;Do not have in lessivation outside escape, volatilization pollution air will not be produced and cause eluant, eluent to lose;This device can meet the requirement of laboratory and back yard industry production simultaneously;Eluant, eluent can be recycled, and substrate matter is reclaimed after can also handling and used, and realizes green production.

Description

A kind of powder ELUTION METHOD and device
Technical field
The present invention relates to a kind of ELUTION METHOD of powder, and in particular to a kind of that 3D printing material elute to obtain nodularization The high powder body material of rate.
Background technology
3D printing technique is the focus studied in currently advanced manufacture field, belongs to multi-crossed disciplines convergence and science and technology wound Newly, the characteristics of green manufacturing, intelligence manufacture and socialization are manufactured is embodied.Its achievement in research has been widely used in consumption electricity The fields such as son, automobile, Aero-Space, mould, defence and military, industrial design, regenerative medicine.European and American developed countries pay much attention to, Think that 3D printing technique will promote third time industry to remove from office together with other Digitized Manufacturing Technologies such as network technology, robot technology Life.Various countries have also carried out corresponding layout and policy guide, such as China《National medium & long term sci-tech development program outline (2006-2020)》、《National " 12 " scientific and technological development planning》, and the U.S.《The advanced manufacturing strategy meter of country Draw》Deng.Extensive use of the 3D printing technique in industry manufacture field is realized, also needs to solve the problems, such as a series of technical bottleneck, Such as 3D printing precision and efficiency, printed material, printed design and printing equipment problem.
The material of current 3D printing is mainly solution based on metal, polymer and composite, it is thread, bar-shaped and Powder body material.In terms of material, the restriction wide variety of maximum bottleneck problem of 3D printing technique is the material category for being adapted to printing Less, expensive, shortage feature.Therefore, for the technical need in different application field, 3D printing material rational design is studied Principle and method, develop feature printed material technology of preparing, realize the prepare with scale of printed material, and not only development is printed Technical industry has important impetus, and the development to new material industry also is played into highly important facilitation.
In industrial application, the demand of 3D printing technique progressively increases, and high Oxygen potential powder body material is to improve printing eventually One of precision and intensity key factor of end-apparatus part.3D printer based on Selective Laser Sintering (SLS), it is desirable to The powder body material used has high Oxygen potential, ultra-fine grain diameter and narrow particle diameter distribution, to ensure powder body material in print procedure High fluidity, high-bulk-density and low porosity.Because existing engineering plastics fine powder is limited by preparation technology and physicochemical property, The nodularization of powder and purification technique shortcoming.Observed under the microscope with commercially available powder body material, mainly show random It is shape, granular, block or bar-shaped.Powder is presented as lazy flow, low printing precision, low-intensity and easily reunited in printing technology Characteristic;Such as easily there is hollow, deformation, caved at the phenomenon in the device of 3D printing, it is impossible to meet industrial to end print device Precision and strength demand.Compare, the mobility of high Oxygen potential powder body material is high, is conducive to the tiling of powder bed, can reach Most dense packing, reduces the voidage of print device, improves mechanical strength.Therefore, in the urgent need to research is directed to PEEK, PTFE Deng for representative, with high-performance, the engineering plastics superfine powder nodularization of high added value and purifying process, industrial quarters is met to end Hold the demand of engineering plastics print device precision and intensity.Although many currently used for solid-liquid or the solid equipment separated admittedly, all It there are problems to have much room for improvement, the factor such as high pollution, high energy consumption, high cost.Using the apparatus,Soxhlet's in laboratory as Example, in terms of the continuity and solvent recycling of production, also compares shortcoming.The present invention considers the deficiency of the above, develops A kind of brand-new closed elution device, solves laboratory, back yard industry production and the demand produced greatly.
Present technology is small due to wash out amount, and elution speed is slow, and elution efficiency is relatively low can not to meet the requirement of part Experiment, and There is eluent volatile quantity greatly in now industrial most of elution device, cost is high again, cause air pollution, and reclaim profit With the low problem of rate.Instant invention overcomes problem above, continuous production, zero release of pollutant, with wide application can be achieved Prospect.
The content of the invention
In consideration of it, the present invention provides a kind of powder ELUTION METHOD, this method can be cleaned to 3D printing material, obtained The high material of Oxygen potential;The present invention also provides a kind of powder elution device simultaneously, can be achieved continuously to produce, zero release of pollutant, Have broad application prospects.
To reach one of above-mentioned purpose, the present invention provides following technical scheme:A kind of powder ELUTION METHOD, will treat that elution is former Material is added in elution tower, and eluant, eluent is added in separated device, and eluant, eluent gasifies in separated device and enters condenser, Enter elution tower after condenser liquefies fully to contact with by raw material to be eluted;The mixing liquid eluted, in recovery tower Interior carry out initial gross separation, remaining then flows back to separated device, so completes a circulation.
Further, flow velocity when elution raw material is eluted using booster pump quickening eluant, eluent is being treated.
To reach the two of above-mentioned purpose, the present invention provides following technical scheme:A kind of powder elution device, including connect successively Elution tower, separated device and the condenser connect, the elution tower is connected with condenser;The elution tower is used to complete to wait to elute The cleaning of raw material;The separated device is used to gasify eluant, eluent, and the separated device is used to separate eluant, eluent and mixing Liquid;The condensing tower is used to the eluant, eluent of gasification being liquefied as liquid, and eluant, eluent is sent in elution tower.
Further, in addition to gas boosting pump, the gas boosting pump is connected with elution tower, the stream for increasing eluant, eluent Speed.
Further, the elution tower bottom is provided with micropore ceramic filter element, for separating raw material and mixed liquor after elution Body.
Further, temperature controller is additionally provided with the separated device, for the temperature for controlling separated device to distill Degree.
As a result of above technical scheme, the present invention has following advantageous effects:
1. automatically continuously production can be achieved without manually nursing after charging etc. is stable, operating cost is low;
2. there is no solvent leakage outside in lessivation, volatilization pollution air will not be produced and cause eluant, eluent to lose;
3. this device can meet the requirement of laboratory and back yard industry production simultaneously;
4. eluant, eluent can be recycled, substrate matter is reclaimed after can also handling and used, and realizes green production.
Brief description of the drawings
In order that the object, technical solutions and advantages of the present invention are clearer, below in conjunction with accompanying drawing the present invention is made into The detailed description of one step, wherein:
Fig. 1 is the structure chart of elution device of the present invention.
Embodiment
Below with reference to accompanying drawing, the preferred embodiments of the present invention are described in detail;It should be appreciated that preferred embodiment Only for the explanation present invention, the protection domain being not intended to be limiting of the invention.
Embodiment 1
The present invention provides a kind of powder ELUTION METHOD, is specially:Powder body material to be eluted is added in elution tower, elution Agent is added in separated device, and temperature is set as 85 DEG C, and eluant, eluent gasifies in separated device and enters condenser, through supercooling Enter elution tower after condenser liquefaction fully to contact with by raw material to be eluted;Under gravity, the mesh of elution is from top to bottom reached 's;The mixing liquid eluted, carries out initial gross separation in recovery tower, and remaining then flows back to separated device, so completes one Individual circulation, after one hour, stops elution and takes out the powder that elution is completed, drying preserves stand-by.
In the present embodiment, powder body material to be eluted is PEEK nodularization powders, and eluant, eluent is ethanol.
As the improvement to the present embodiment, stream when elution raw material is eluted using booster pump quickening eluant, eluent is being treated Speed.
Before whole device work, according to the different vapo(u)rizing temperature of different raw material to be eluted settings and elution time.
Embodiment 2
As shown in figure 1, a kind of powder elution device, including elution tower, separated device and the condenser being sequentially connected, institute Elution tower is stated to be connected with condenser;The elution tower is used for the cleaning for completing raw material to be eluted;The separated device is used for will Eluant, eluent gasifies, and the separated device is used to separate eluant, eluent and mixing liquid;The condensing tower is used for the elution of gasification Agent is liquefied as liquid, and eluant, eluent is sent in elution tower.
PS nodularization powders are added in elution tower, water is added in separated device, and temperature is set as 110 DEG C, and water exists Separated device gasifies and enters condenser, and elution tower is entered after condenser liquefies with being treated that PS powders are fully contacted; Under Action of Gravity Field effect, the purpose of elution is from top to bottom reached;The mixing liquid eluted, is tentatively divided in recovery tower From remaining then flows back to separated device, so completes after a circulation, 40min, stops elution and takes out PS powders, drying is preserved It is stand-by.
As the improvement to the present embodiment, in addition to gas boosting pump, the gas boosting pump is connected with elution tower, is used for Increase the flow velocity of eluant, eluent.
The elution tower bottom is provided with micropore ceramic filter element, for separating raw material and mixing liquid after elution.Simultaneously Filter core can be changed as needed.
As the improvement to the present embodiment, temperature controller is additionally provided with the separated device, for controlling distillation The temperature of separator distillation.
The separated device uses electrical heating, and its inwall is stainless steel lining, applicable most of reagent.
Described condenser is cold using air cooling or liquid, it is possible to adjust chilling temperature, controls cooling effect.
The present invention need not be nursed manually after charging etc. is stable in the course of the work, and automatically continuously production, fortune can be achieved Row cost is low, does not have in lessivation outside solvent leakage, will not produce volatilization pollution air and cause eluant, eluent to lose;Together When whole elution circuit constitute complete circulation, repetitive cycling uses green non-pollution;The liquid phase being eluted can also be weighed It is multiple to use (or reusing after treatment), meet the no pollution emission request of green production.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, it is clear that those skilled in the art Member can carry out various changes and modification to the present invention without departing from the spirit and scope of the present invention.So, if the present invention These modifications and variations belong within the scope of the claims in the present invention and its equivalent technologies, then the present invention is also intended to include these Including change and modification.

Claims (5)

1. a kind of powder ELUTION METHOD, it is characterised in that:Raw material to be eluted is added to bottom and is provided with micropore ceramic filter element Elute in tower, eluant, eluent is added in separated device, eluant, eluent gasifies in separated device and enters condenser, by condensation Enter elution tower after device liquefaction fully to contact with by raw material to be eluted, under gravity, powder is eluted;Elute Mixing liquid, initial gross separation is carried out in recovery tower, remaining then flows back to separated device, so complete one circulation.
2. powder ELUTION METHOD according to claim 1, it is characterised in that:Used treating when elution raw material is eluted Booster pump accelerates the flow velocity of eluant, eluent.
3. a kind of powder elution device, it is characterised in that:Including the elution tower, separated device and condenser being sequentially connected, institute Elution tower is stated to be connected with condenser;
The elution tower is used for the cleaning for completing raw material to be eluted;
The separated device is used to gasify eluant, eluent, and the separated device is used to separate eluant, eluent and mixing liquid;
The condensing tower is used to the eluant, eluent of gasification being liquefied as liquid, and eluant, eluent is sent in elution tower, makees in gravity Under, powder is eluted;The elution tower bottom is provided with micropore ceramic filter element, for separating the raw material after elution and mixing Close liquid.
4. powder elution device according to claim 3, it is characterised in that:Also include gas boosting pump, the gas increases Press pump is connected with elution tower, the flow velocity for increasing eluant, eluent.
5. according to claim 3 without described powder elution device, it is characterised in that:Temperature is additionally provided with the separated device Controller is spent, for the temperature for controlling separated device to distill.
CN201410372958.3A 2014-07-31 2014-07-31 A kind of powder ELUTION METHOD and device Active CN104194005B (en)

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Application Number Priority Date Filing Date Title
CN201410372958.3A CN104194005B (en) 2014-07-31 2014-07-31 A kind of powder ELUTION METHOD and device

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CN105819887A (en) * 2016-03-08 2016-08-03 武汉大学 Preparation method of non-sintered ceramsite with ammonia nitrogen adsorption function
CN105819891A (en) * 2016-03-08 2016-08-03 武汉大学 Preparation method of sludge ceramsite used for medium and low concentration ammonia nitrogen wastewater treatment
CN109957105A (en) * 2019-04-03 2019-07-02 张家港祥成医用材料科技有限公司 A kind of method and apparatus of polyether ketone ketone cycling elution
CN110201452B (en) * 2019-06-18 2021-05-07 宁波心思为三维科技有限公司 Filter for recycling and cleaning 3D product residue alcohol and using method thereof

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GB0113053D0 (en) * 2001-05-30 2001-07-18 Victrex Mfg Ltd Polyketones
CN1269872C (en) * 2004-12-09 2006-08-16 四川大学 Method for purifying poly ether-ether-ketone
CN103709406B (en) * 2013-11-29 2016-05-11 金发科技股份有限公司 A kind of method of preparing light polyether sulfone/polyether-ether-ketone resin

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