CN205774251U - A kind of detachable gum-free breast grain generator - Google Patents

A kind of detachable gum-free breast grain generator Download PDF

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Publication number
CN205774251U
CN205774251U CN201620420059.0U CN201620420059U CN205774251U CN 205774251 U CN205774251 U CN 205774251U CN 201620420059 U CN201620420059 U CN 201620420059U CN 205774251 U CN205774251 U CN 205774251U
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China
Prior art keywords
threeway
glass tube
nut
injection port
capillary
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Withdrawn - After Issue
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CN201620420059.0U
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Chinese (zh)
Inventor
刘杨
刘一杨
苏琳
李洁
刘梅芳
陈素芬
吴倩
李婧
黄勇
史瑞廷
初巧妹
张占文
冯建鸿
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Laser Fusion Research Center China Academy of Engineering Physics
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Laser Fusion Research Center China Academy of Engineering Physics
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Abstract

This utility model provides a kind of detachable gum-free breast grain generator, and described generator is a kind of newborn grain generating means possessing regulatory function easily, and based on three-port structure, glass pipe is auxiliary.Inner glass pipeline is in the middle of the protection of threeway and outer glass wall.Using silica gel sealing pad to coordinate conical seal ring to seal three-phase fluid, the injection port of each phase liquid is made up of sample feeding pipe and sealing structure matching.This utility model is applicable to high-quality Water-In-Oil (W/O) or the preparation of oil-in-water (O/W) type breast grain and prepared by polymeric hollow/solid microsphere, most of organic solvent can be used to be carried out device, and when preferably overcoming employing adhesive seal, organic solvent-resistant does not cleans and may introduce the drawback of impurity element in breast grain and microsphere.

Description

A kind of detachable gum-free breast grain generator
Technical field
This utility model belongs to emulsion science and forming polymer field, is specifically related to a kind of detachable gum-free breast grain and sends out Raw device.
Background technology
Traditional method preparing hollow polymer microsphere mainly has emulsion polymerization, sol-gal process, emulsion micropackaging Method etc., but it is all diameter, the distribution of wall thickness width that its mode based on stirring solidification determines the tiny balloon prepared, and And its thickness is difficult to control.The birth of microflow control technique for preparing diameter, wall thickness narrow ditribution hollow polymer microsphere provides one Plant brand-new method, by designing the micro fluidic device of difference in functionality structure, it is possible to obtain high-quality emulsion and polymer are micro- Ball, is widely used in industries such as medicine, biomaterial, coating, thus is increasingly paid attention to by association area.
Breast grain generator technology is the one of microflow control technique, and this method is preparing single dispersing breast grain and polymeric hollow Microsphere aspect has original advantage.Its inner and outer diameter can be carried out by adjusting pipeline inner and outer diameter and three-phase flow rate of liquid Control.Newborn grain generator many employings mechanical vibration and the mode of jet of business forms drop at present, is mainly suitable for stability very Prepared by good newborn plastochondria system or solid core polymer microballoon, need to improve, and cost is higher in monodispersity.Domestic one Also there are the newborn grain generator using easy glass plate and pipeline collocation to use in a little research institutions, but cannot avoid making of binding agent With, organic solvent-resistant aggressivity is poor, and non-dismountable assembles again.Also have based on etching chip and glass pipe with the use of Newborn grain generator, binding agent to be used, and price comparison is expensive, is not suitable for being repeatedly used for a long.
Summary of the invention
A technical problem to be solved in the utility model is to provide a kind of detachable gum-free breast grain generator.
Detachable gum-free breast grain generator of the present utility model, is characterized in, including the sampling structure being linked in sequence, together Axle nesting pipeline configuration, adjustment structure;
Described sampling structure includes injection port I, injection port II, injection port III;
Described injection port includes nut, sample feeding pipe, conical seal ring, silica gel sealing pad;
Described injection port I is the first phase fluid inlet port, and sample feeding pipe sequentially passes through nut, conical seal ring withstands on silicon On glue sealing gasket, nut it is tightened on the right side of threeway A;
Described injection port II is the second phase fluid inlet port, and sample feeding pipe sequentially passes through nut, conical seal ring, silica gel It extend into after sealing gasket in the top through hole of threeway A, nut be tightened on the top of threeway A;
Described injection port III is third phase fluid inlet port, and structure is identical with injection port II, nut be tightened Top at threeway B;
Described coaxial nested pipeline configuration includes threeway, capillary glass tube, nut, conical seal ring, silica gel sealing pad And glass bushing;The right side nut of threeway A compresses silica gel sealing pad by conical seal ring and is tightened;The left side of threeway A, The left and right sides of threeway B is identical with the right side structure of threeway A, nut porch be provided with sealing ring, threeway A and threeway B and By stretching into the glass bushing connection of sealing ring between threeway B and straight molded cannula;Capillary glass tube A, capillary glass tube B and glass Capillary tube C is the most nested from inside to outside with glass bushing;Capillary glass tube A right-hand member stretches into through the silica gel sealing pad of injection port I In sample feeding pipe, capillary glass tube A left end is through threeway A and stretches into capillary glass tube B right-hand member, finally arrives in the middle part of glass bushing; Capillary glass tube B right-hand member enters threeway A after passing the nut on the left of threeway A, conical seal ring, silica gel sealing pad, arrives sample introduction The lower section of mouth II, capillary glass tube B left end stretches into capillary glass tube C right-hand member after threeway B, finally arrives threeway B and threeway C Between the middle part of glass bushing;After capillary glass tube C right-hand member passes the nut on the left of threeway B, conical seal ring, silica gel sealing pad Entering threeway B, arrive the lower section of injection port III, capillary glass tube C left end passes glass bushing and straight molded cannula.
Described adjustment structure includes adjusting screw, straight molded cannula, and straight molded cannula passes through glass bushing and coaxial embedding tube Connecting on the left of threeway B in road structure, four adjust screw omnidirectional distribution in straight molded cannula.
Detachable gum-free breast grain generator of the present utility model, often increases a set of injection port and capillary glass tube just can One layer of shell is increased at the newborn grain of preparation or the surface of tiny balloon.
Detachable gum-free breast grain generator of the present utility model is applicable to submillimeter and grade polymer hollow microsphere And breast grain preparation, the use cycle is longer and possesses certain pipeline with axial adjustment function, have simple in construction, convenient disassembly, Without the advantage of binding agent, being suitable to operation, practicality is good.
Accompanying drawing explanation
Fig. 1 is detachable gum-free breast grain generator architecture figure of the present utility model;
Fig. 2 is threeway and sealing structure broken away view in detachable gum-free breast grain generator of the present utility model;
Fig. 3 is threeway and sealing structure assembling figure in detachable gum-free breast grain generator of the present utility model;
In figure, 1. sample feeding pipe 2. nut 3. capillary glass tube A 4. threeway A 5. conical seal ring 6. silica gel sealing pad 7. the straight molded cannula 11. of sealing ring 8. glass bushing 9. capillary glass tube B 10. adjusts screw 12. capillary glass tube C 13. Threeway B.
Detailed description of the invention
Embodiment 1
A kind of water-in-oil type breast grain of the present embodiment preparation, method is as follows:
As shown in Figure 1-Figure 3, detachable gum-free breast grain generator of the present utility model, it is characterised in that include order The sampling structure connected, coaxial nested pipeline configuration, adjustment structure;
Described sampling structure includes injection port I, injection port II, injection port III;
Described injection port includes nut, sample feeding pipe, conical seal ring, silica gel sealing pad;
Described injection port I is the first phase fluid inlet port, and sample feeding pipe 1 sequentially passes through nut 2, conical seal ring 5 pushes up On silica gel sealing pad 6, nut 2 it is tightened on the right side of threeway A4;
Described injection port II is the second phase fluid inlet port, and sample feeding pipe sequentially passes through nut, conical seal ring, silica gel It extend into after sealing gasket in the top through hole of threeway A4, nut be tightened on the top of threeway A4;
Described injection port III is third phase fluid inlet port, and structure is identical with injection port II, nut be tightened Top at threeway B13;
Described coaxial nested pipeline configuration includes threeway, capillary glass tube, nut, conical seal ring, silica gel sealing pad And glass bushing;The right side nut 2 of threeway A4 compresses silica gel sealing pad 6 by conical seal ring 5 and is tightened;Threeway A4's Left side, threeway B13 the left and right sides identical with the right side structure of threeway A4, nut porch is provided with sealing ring, threeway A4 with Connect by stretching into the glass bushing 8 of sealing ring between threeway B13 and threeway B13 and straight molded cannula 10;Capillary glass tube A3, Capillary glass tube B9 and capillary glass tube C12 is the most nested from inside to outside with glass bushing 8;Capillary glass tube A3 right-hand member pass into The silica gel sealing pad 6 of sample mouth I stretches in sample feeding pipe 1, and capillary glass tube A3 left end is through threeway A4 and stretches into capillary glass tube B9 Right-hand member, finally arrives in the middle part of glass bushing 8;Capillary glass tube B9 right-hand member passes the nut on the left of threeway A4, conical seal ring, silicon Entering threeway A4 after glue sealing gasket, arrive the lower section of injection port II, capillary glass tube B9 left end stretches into glass after threeway B13 Capillary tube C12 right-hand member, finally arrives the middle part of glass bushing between threeway B and threeway C;Capillary glass tube C12 right-hand member passes three Enter threeway B13 after leading to the nut on the left of B13, conical seal ring, silica gel sealing pad, arrive the lower section of injection port III, glass fiber Tubule C12 left end passes glass bushing 8 and straight molded cannula 10.
Described adjustment structure includes adjusting screw 11, straight molded cannula 10, and straight molded cannula 10 passes through glass bushing 8 with coaxial Connecting on the left of threeway B13 in nested pipeline configuration, four adjust screw 11 omnidirectional distribution in straight molded cannula 10.
The realization that closely cooperates relying primarily on silica gel sealing pad, conical seal ring and nut owing to sealing structure seals work With, therefore it is required that the diameter of through hole is slightly less than the extracapillary diameter passed through on glue sealing ring, conical seal ring through-hole diameter is slightly More than stainless steel capillary overall diameter, the length of capillary tube A and capillary tube B controls to reach to be preferred in the middle part of glass bushing with end, It is easy to observe drop in capillary tube by sleeve pipe and shapes situation with breast grain.
The present embodiment before assembling, first carries out the hydrophobic treatment of capillary glass tube, prepares 1%(volume ratio) octadecane Pending capillary tube, as AL, is soaked 24 little in 10%HNO3 solution by base trimethoxy silane/toluene solvant Time, clean with deionized water after taking-up, supersound process 5min in ethanol solution, the alkylating reagent of preparation before then using Process at 75 DEG C about 3 hours, be dried after cleaning with EtOH Sonicate after taking-up.
After device assembles, aqueous phase in preparing, oil phase and outer aqueous phase solution.The present embodiment is interior water with deionized water Phase, the fluorobenzene solution of polystyrene is oil phase, and polyvinyl alcohol water solution is outer aqueous phase.Three capillaries need to be seen under the microscope Examining, inside and outside wall is without substantially polluting, and port is without obvious defect, and capillary glass tube B need to be through hydrophobic treatment.According to group shown in Fig. 1-3 Installing generator, capillary glass tube C12 outlet is positioned at bottom and generator vertically downward.Use flexible pipe by sample feeding pipe and conjunction Suitable syringe connects, and respectively filled with interior aqueous phase, oil phase and outer aqueous phase solution in syringe, this example uses medical injection pump automatic Control the flow of liquid in syringe.Generator assemble after when using first, need to be passed through in three sample feeding pipes of generator from Sub-water is hunted leak.
When starting to prepare breast grain, it is passed through in the sample feeding pipe of injection port I successively in the sample feeding pipe of deionized water, injection port III It is passed through polyvinyl alcohol water solution, treats that deionized water is full of capillary glass tube B9, poly-vinyl alcohol solution is full of capillary glass tube C12 After, start in the sample feeding pipe of injection port II, be passed through polystyrene/fluorobenzene solution.Observe glass between threeway A4 and threeway B13 The port of capillary glass tube A3 in sleeve pipe, from the beginning of capillary glass tube A3 port, will form continuous print in capillary glass tube B9 Interior aqueous phase droplets.Generate as do not observed aqueous phase droplets in continuous print, interior aqueous phase and Oil phase flow rate need to be adjusted, as in glass capillary When can only see the two phase flow along glass wall flowing in pipe B9, then it is owing to the hydrophobic treatment of middle capillary tube is incomplete, solves Method is off fluid input, the capillary glass tube B9 that replacing processed.Formed aqueous phase droplets together with oil phase from glass Glass capillary tube B9 flows to capillary glass tube C12, forms independent water in oil breast grain at capillary glass tube B9 port.By observing Glass bushing between threeway B13 and straight molded cannula is it can be seen that the newborn grain formational situation of capillary glass tube B9 port, such as breast grain Breakdown of emulsion occurs when going out the port of capillary glass tube B9, then the port of capillary glass tube B9 there may be burr or hydrophobic treatment is lost Effect, the capillary tube that need to more renew, as breast grain sticks in the inwall of capillary glass tube C12 continuing downward output procedure, then be due to Capillary glass tube C12 inwall is contaminated, same replacing capillary glass tube C12.
By adjust suitable three-phase flow rate of liquid, till generator exports independent newborn grain continuously, breast grain interior External diameter is relevant with the fluid properties of capillary size, three-phase flow velocity and each phase liquid, needs to investigate according to specific experiment to confirm, three Phase liquid can select suitable liquid according to breast grain composition requirements.
Having prepared rear generator needs and cleaned in case next time uses, cleanout fluid uses very good dissolving to polystyrene The oxolane of property.First three-phase fluid input is stopped, the syringe note being full of oxolane oil phase input used Emitter is replaced, and the syringe input of outer aqueous phase used is replaced with the syringe being full of deionized water.Open three-phase liquid Driving syringe pump, to flexible pipe, oil phase is purged completely, more repeatedly cleans 2 times.Close injection port II, continue to inject interior aqueous phase Device also uses the syringe of full oxolane to replace, and repeatedly cleans oil phase solvent remaining in can washing generator for 2 times, Generator can reuse after drying.
Embodiment 2
A kind of oil-in-water type breast grain of the present embodiment preparation, method is substantially the same manner as Example 1, and difference is to need to dredge The capillary tube that water processes is changed into capillary glass tube A3 and capillary glass tube C12 by capillary glass tube B9, and it is molten that injection port I enters interior oil phase Liquid, injection port II enter aqueous phase solution, injection port III enters outer oil-phase solution.Each phase liquid is also according to the emulsion feature needing preparation Carry out selecting preparation.
Embodiment 3
A kind of hollow polymer microsphere of the present embodiment preparation, method is substantially the same manner as Example 1, and difference is breast grain Use flask to receive breast grain after generation, be placed in rotary evaporator, after rotating the elevated cure regular hour, obtain internal containing The polystyrene microsphere of water, more hollow polystyrene microsphere can be formed after 50 DEG C of oven dryings.Obtain as required Polymer microballoon component requirements, selects corresponding suitably polymer oil-phase solution.The mode of microsphere solidification can be according to polymerization Thing characteristic is specifically chosen, and as the modes such as emulsion polymerization or photocuring all can use, initiator can be introduced by inside and outside aqueous phase.
Embodiment 4
A kind of solid polymeric microspheres of the present embodiment preparation, method is substantially the same manner as Example 3, and difference is reality Injection port III in example 3 is closed or is passed through the solution as injection port II and serves as wash fluid, passes through similar solidification and does Solid polystyrene microsphere is obtained after dry.
This utility model is not limited to above-mentioned detailed description of the invention, and person of ordinary skill in the field visualizes from above-mentioned Sending out, without performing creative labour, done all conversion, within all falling within protection domain of the present utility model.

Claims (4)

1. a detachable gum-free breast grain generator, it is characterised in that sampling structure that described generator includes being linked in sequence, Coaxial nested pipeline configuration, adjustment structure;
Described sampling structure includes injection port I, injection port II, injection port III;
Described injection port includes nut, sample feeding pipe, conical seal ring, silica gel sealing pad;
Described injection port I is the first phase fluid inlet port, and sample feeding pipe (1) sequentially passes through nut (2), conical seal ring (5) Withstand on silica gel sealing pad (6), nut (2) be tightened at threeway A(4) right side;
Described injection port II is the second phase fluid inlet port, and sample feeding pipe sequentially passes through nut, conical seal ring, silica gel sealing Extend into threeway A(4 after pad) top through hole in, nut be tightened at threeway A(4) top;
Described injection port III is third phase fluid inlet port, and structure is identical with injection port II, nut be tightened three Logical B(13) top;
Described coaxial nested pipeline configuration includes threeway, capillary glass tube, nut, conical seal ring, silica gel sealing pad and glass Glass sleeve pipe;Threeway A(4) right side nut (2) by conical seal ring (5) compress silica gel sealing pad (6) be tightened;Threeway A(4) left side, threeway B(13) the left and right sides and threeway A(4) right side structure identical, nut porch is provided with sealing Circle, threeway A(4) and threeway B(13) and threeway B(13) and straight molded cannula (10) between by stretching into the glass bushing of sealing ring (8) connect;Capillary glass tube A(3), capillary glass tube B(9) and capillary glass tube C(12) and glass bushing (8) from inside to outside with Axle is nested;Capillary glass tube A(3) right-hand member stretches in sample feeding pipe (1) through the silica gel sealing pad (6) of injection port I, capillary glass tube A(3) left end passes threeway A(4) and stretch into capillary glass tube B(9) right-hand member, finally arrive glass bushing (8) middle part;Glass capillary Pipe B(9) right-hand member is through threeway A(4) nut in left side, conical seal ring, enter threeway A(4 after silica gel sealing pad), arrive sample introduction The lower section of mouthful II, capillary glass tube B(9) left end stretches into capillary glass tube C(12 after threeway B (13)) right-hand member, finally arrive The middle part of glass bushing between threeway B and threeway C;Capillary glass tube C(12) right-hand member is through threeway B(13) nut in left side, cone Threeway B(13 is entered after shape sealing ring, silica gel sealing pad), arrive the lower section of injection port III, capillary glass tube C(12) left end passes Glass bushing (8) and straight molded cannula (10);
Described adjustment structure include adjust screw (11), straight molded cannula (10), straight molded cannula (10) by glass bushing (8) with Threeway B(13 in coaxial nested pipeline configuration) left side connection, four adjust screw (11) omnidirectional distribution in straight molded cannula (10) On.
Detachable gum-free breast grain generator the most according to claim 1, it is characterised in that described nut, threeway Material is rustless steel or ETFE, PEEK base polymer of solvent resistant corrosion, and cone seal loop material is ETFE;Sample feeding pipe is stainless Steel.
Detachable gum-free breast grain generator the most according to claim 1, it is characterised in that described detachable gum-free Breast grain generator is when being used for preparing w/o type breast grain and hollow polymer microsphere, described capillary glass tube B(9) need to carry out hydrophobic Surface is modified;When described detachable gum-free breast grain generator is used for preparing O/W type breast grain and solid polymeric microspheres, described Capillary glass tube A(3) and capillary glass tube C(12) hydrophobic surface modification need to be carried out.
Detachable gum-free breast grain generator the most according to claim 3, it is characterised in that described capillary tube hydrophobic Surface is modified and is used octadecyl trimethoxysilane and the mixed solution of toluene 1:100 by volume preparation, alkylated reaction Rear cleanout fluid is ethanol.
CN201620420059.0U 2016-05-11 2016-05-11 A kind of detachable gum-free breast grain generator Withdrawn - After Issue CN205774251U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105754116A (en) * 2016-05-11 2016-07-13 中国工程物理研究院激光聚变研究中心 Detachable no-adhesive type emulsion granule generator
CN113145038A (en) * 2021-04-21 2021-07-23 西安交通大学 Method and device for preparing oil emulsion adjuvant based on microfluidics

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105754116A (en) * 2016-05-11 2016-07-13 中国工程物理研究院激光聚变研究中心 Detachable no-adhesive type emulsion granule generator
CN105754116B (en) * 2016-05-11 2018-03-02 中国工程物理研究院激光聚变研究中心 A kind of detachable gum-free milk particle generator
CN113145038A (en) * 2021-04-21 2021-07-23 西安交通大学 Method and device for preparing oil emulsion adjuvant based on microfluidics

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Granted publication date: 20161207

Effective date of abandoning: 20180302