CN100336582C

CN100336582C - Mixture device for multiple nozzle pollision flow

Info

Publication number: CN100336582C
Application number: CNB2005100268181A
Authority: CN
Inventors: 阎建民; 赵亚平; 罗先金; 于文利
Original assignee: Shanghai Jiaotong University
Current assignee: Shanghai Jiaotong University
Priority date: 2005-06-16
Filing date: 2005-06-16
Publication date: 2007-09-12
Anticipated expiration: 2025-06-16
Also published as: CN1724132A

Abstract

The present invention discloses a collision flow mixing device with multiple nozzles, which comprises a nozzle core, annular distribution grooves, a fixing plate, and a V-shaped top cover, wherein the nozzle core is fixed in the middle of the distribution grooves by screw threads or in a welding mode; annular fluid channels are arranged between the nozzle core and the annular distribution grooves, and the annular distribution grooves are fixed on the fixing plate by screws; the fixing plate is clamped on the V-shaped top cover of which the lower part is connected with a crystallization container. The present invention has the advantages that the device of the present invention is used for preparing micro nanometer particles by supercritical fluid, and the prepared micro nanometer particles have small and even particle sizes; the device of the present invention is convenient to process and to manufacture and has good mixing performance.

Description

Mixture device for multiple nozzle pollision flow

Technical field:

The present invention relates to a kind of chemical industry equipment, particularly a kind of mixture device for multiple nozzle pollision flow for preparing micro-nano granules is used for preparing micro-nano granules by supercritical fluid.

Technical background:

Using super critical fluid technology can be finished many thermal sensitivity medicines and explosive, easily the particulate of degradation material is processed, and tool environmental protection characteristics, thereby becomes a present research focus.Supercritical solution rapid expanding method (RESS) is applicable to handles the supercritical fluid solable matter, relevant patent (Zhao Yaping. etc., CN02111918.X) the flared nozzle aperture and the shape of nozzle have been done design.At present, various supercritical fluid anti-solvent technologies (SAS) more people pay close attention to (Jung J ﹠amp; Perrut M.Journal of SupercriticalFluids 20:179,2001).The SAS technology is mixed supercritical fluid (SCF) with the processing substance solution, finish the partial crystallization process under supercriticality.Existing result of study shows, the crystal formation of final grain products, size distribution mix and mass transport process closely related (Francisco C, Pablo D, etc.AIChE J42:3156,2003) with microcosmic under the nucleation condition.The same with conventional partial crystallization process, the SAS technology has comprised nucleation and two steps of grain growth.As ideal situation, the mixed process of SCF and solution should be complete mixing flow, and SCF should be fully little with the characteristic time that mixes of the substance solution of handling, to obtain even-grained micro-nano granules.Simultaneously, should keep laminar flow after mixing, avoid generating the back-mixing of the particle and the substance solution of handling.SEDS (reinforced solution dispersion) is a kind of of SAS technology, require SCF and solution to inject simultaneously, the most approaching this ideal situation can realize that the crystal formation of particulate product is controlled (Kordikowski A, Shekunov T, York P.Pharm Res 18:682.2001).

According to the microcosmic application of mixture theory, the kinematic viscosity reduction of mixing of microcosmic characteristic time with system reduces, and the increase of mixed process energy dissipation speed simultaneously also can be shortened mixing of the microcosmic characteristic time.The key factor that mixed process also need be considered is the ratio of mixing, and the SEDS technology is finished partial crystallization, and the volume of the SCF fluid of requirement participation mixing is much larger than processing substance solution volume usually.

In the bibliographical information, the hybrid mode that the SEDS technology is the most general is to adopt the multichannel coaxial nozzle at present, and there is following problem in this hybrid mode: the first, and each channel size that SCF and solution flow into should be enough tiny, to guarantee mixed process energy dissipation speed.For avoiding the Mixed Zone flow blind angle to occur, the Mixed Zone volume is also unsuitable big simultaneously.Therefore, relevant apparatus particularly the low discharge experimental provision processing very the difficulty, more be difficult to optimize troubled water; The second, each materials flow directly sprays into the partial crystallization container after mixing, and the time of staying skewness of materials flow in container influenced the size distribution of grain products.In addition, the energy dissipation speed of mixed process is limited in the coaxial nozzle, and the microcosmic mixed-scale is difficult to reduce, and also makes troubles for process design.

For improving mixed effect, (M.Hanna US6440337B1) has proposed to collide streamed nozzle to patent, to increase the energy dissipation speed of mixed process.Owing to still adopt coaxial multitube road design, this mixing arrangement is made of a trickle parts surplus ten, and processing and manufacturing is more difficult.

Summary of the invention:

The object of the present invention is to provide a kind of multiinjector collision stream mixing arrangement of being convenient to processing and manufacturing, and can make the substance solution of handling and supercritical fluid rapid mixing even, be used to prepare micro-nano granules.

The technical measures that the present invention mainly takes have two: article one is the number that increases the collision materials flow, can optimize troubled water under the different mixing proportion by adjusting the materials flow number, thereby reduce the requirement on machining accuracy to nozzle form; Second is to change common mixed liquor to flow to, solution with upwards spring up after supercritical fluid mixes, partial crystallization container below passage between top cover and distributing slot enters again, mixing nozzle combines the distributor that has formed mixture flow with container cap, can promote the quality transmission of nucleation process, and improve the time of staying distribution of mixed liquor in the partial crystallization container.

Multiinjector collision stream mixing arrangement of the present invention comprises nozzle core, the annular spread groove, fixed head and V-arrangement top cover four parts, nozzle core is by screw thread or be weldingly fixed in the middle of the annular spread groove, there is annular fluid passage between nozzle core and the annular spread groove, there is flared nozzle nozzle core bottom and side, the nozzle core center is a cup-shaped Mixed Zone, measuring few materials flow is entered by the bottom spout, the materials flow that amount is many is entered by the side spout, the side spout has angle of declination to strengthen mixed effect, side spout axis and horizontal line angle are 5-50 °, side spout number is 3-20, according to the volume ratio adjustment of supercritical fluid with the substance solution of handling, the volume of cup-shaped Mixed Zone is unsuitable big, and to reduce the composite character time, this volume is the 0.5-50 milliliter; The annular spread groove is fixed on the fixed head by screw; Fixed head then fastening on the V-arrangement top cover; Partial crystallization container below the V-arrangement top cover connects by flange.

Fixed head is made of support chip 12, reinforcing bar 13 and ring plate 14 welding.

The profile of annular spread groove is streamline or garden arc, dead angle area occurs to avoid mixing arrangement inside.

Material selection stainless steel, engineering plastics or the ceramic material of multiinjector collision stream mixing arrangement.

The simple in structure of mixing arrangement flowed in multiinjector collision of the present invention, is convenient to processing and manufacturing, good mixing property,

Reliable and stable work prepares micro-and nano-particles by supercritical fluid, and the particle diameter of gained micro-and nano-particles is little, and particle diameter is even.

The description of drawings and the specific embodiment

Fig. 1 is the structural representation of multiinjector collision stream mixing arrangement of the present invention.

Fig. 2 is fixed on the nozzle core of one and the vertical view of annular fluid distributing slot.

Fig. 3 is a fixed head shape schematic diagram.

Multiinjector collision stream mixing arrangement of the present invention as shown in Figure 1, comprise nozzle core 4, annular spread groove 2, fixed head 6 and V-arrangement top cover 1 four parts, there is annular fluid passage 8 between nozzle core and the annular spread groove, the annular spread groove is fixed on the fixed head by screw 5, fixed head is made of support chip 12, reinforcing bar 13 and ring plate 14 welding, ring plate 14 fastenings are on V-arrangement top cover inner surface during use, the next connection partial crystallization of V-arrangement top cover container;

The a plurality of spout distribution modes in nozzle core side as shown in Figure 2;

The specific constructive form of fixed head as shown in Figure 3.

Multiinjector collision stream mixing arrangement of the present invention in use, supercritical fluid at first passes the V-arrangement top cover sidewall, by the road 10 and connector 9 enter in the circular passage 8, by the flared nozzle 3 in some and aperture, mix with solution again in the Mixed Zone 11 of nozzle core central authorities.Solution passes the V-arrangement top cover sidewall equally, and 7 flared nozzles 3 from the nozzle core bottom enter Mixed Zone 11 by the road.

Use multiinjector collision stream mixing arrangement of the present invention to carry out the experiment of PLA superfine, device is prepared by stainless steel material, 4.2 milliliters of Mixed Zone volumes, the acetone soln of PLA sprays into from the nozzle core bottom, three nozzles spray into supercritical carbon dioxide fluid from the nozzle core side simultaneously, 20 ° at side nozzle inclination angle, the supercritical carbon dioxide fluid flow-control is about 30 times of liquid inventory, after the two mixes, enter in the partial crystallization container of 35 ℃ of pressure 10Mpa temperature, can obtain the micron-sized PLA particulate of particle diameter 0.5-1 rapidly, CO 2 fluid goes out through the sintered porous plate current of partial crystallization container bottom.

Use multiinjector collision stream mixing arrangement of the present invention to carry out the experiment of polystyrene superfine, device is prepared by stainless steel material, 6.6 milliliters of Mixed Zone volumes, the toluene solution of polystyrene sprays into from the nozzle core bottom, six nozzles spray into supercritical carbon dioxide fluid from the nozzle core side simultaneously, 30 ° at side nozzle inclination angle, the supercritical carbon dioxide fluid flow-control is about 50 times of liquid inventory, after the two mixes, enter in the partial crystallization container of 38 ℃ of pressure 10Mpa temperature, can obtain the micron-sized ps particle of particle diameter 0.5-1.5 rapidly, CO 2 fluid goes out through the sintered porous plate current of partial crystallization container bottom.

Claims

1, a kind of multiinjector collision stream mixing arrangement, it is characterized in that comprising nozzle core, the annular spread groove, fixed head and V-arrangement top cover four parts, nozzle core is by screw thread or be weldingly fixed in the middle of the annular spread groove, there is annular fluid passage between nozzle core and the annular spread groove, there is flared nozzle nozzle core bottom and side, the nozzle core center is a cup-shaped Mixed Zone, measuring few materials flow is entered by the bottom spout, the materials flow that amount is many is entered by the side spout, the side spout has angle of declination to strengthen mixed effect, side spout axis and horizontal line angle are 5-50 °, side spout number is 3-20, and according to the volume ratio adjustment of supercritical fluid with the substance solution of handling, the volume of cup-shaped Mixed Zone is unsuitable big, to reduce the composite character time, this volume is the 0.5-50 milliliter; The annular spread groove is fixed on the fixed head by screw; Fixed head then fastening on the V-arrangement top cover; Partial crystallization container below the V-arrangement top cover connects by flange.

2, a kind of multiinjector collision stream mixing arrangement according to claim 1 is characterized in that fixed head is made of support chip, reinforcing bar and ring plate welding.

3, a kind of multiinjector collision stream mixing arrangement according to claim 1, the profile that it is characterized in that the annular spread groove is streamlined or circular arc.