High-pressure electrostatic electronics shuttle nano-spun silk device
Technical field
The invention belongs to the electrostatic spinning technique field, be specifically related to a kind of high-pressure electrostatic electronics shuttle nano-spun silk device.
Background technology
Electrostatic spinning technique is that non-newtonian fluid produces jet after the match at high-pressure electrostatic, forms a kind of technology of micron and even nanofiber, and it is the direct method that can be used for preparing organic and inorganic and composite nano fiber.Because electro spinning nano fiber all has good prospects for application at numerous areas such as filtrations, medicine, environment, organizational project, electronics, catalysis, sound-absorbing and military affairs, thus about the research of electrospinning silk equipment at one of hot subject that becomes global many scholars and engineers and technicians recently.
At present, the electrospinning silk equipment of prepared in laboratory nanofiber mainly contains following several form: single spray nozzle type, many spray nozzle types, porous type, roll-type, slit electrical spinning method.Wherein modal is single spray nozzle type, and it builds simple, cheap, but spinning speed is extremely slow, in 0.001-0.01 g/h scope; Many spray nozzle types are that tens even thousands of single spinning needle points are made up, ejection efficiency can be increased to 0.1 ~ 1.0 g/h, but electrostatic interference often occurs, shower nozzle easily stops up, and causes that spinning is discontinuous, the nanofiber diameter homogeneity is difficult to the appearance of shortcomings such as keeping.Porous type has problems such as spinning efficiency is low equally.The representative of roll-type electrostatic spinning is Czech " nanometer spider " technology, and its spinning efficiency is 1 ~ 5g/min, and area density is 0.1 ~ 5g/m
2, nanofiber diameter is in 50 ~ 300 nm scopes, and fabric width has two kinds of 300 and 500 mm.Recently, we have invented high-pressure electrostatic shuttle nano-spun silk device, adopt the slit method to carry out the preparation of nanofiber, slit length (fabric width) is adjustable, its spinning efficiency and nanometer spider are similar, but but continuous feeding, have easy cleaning, low energy consumption, safe and reliable, easy and simple to handle, advantages of environment protection, be suitable for laboratory and industrial amplification production.
Yet we know that what people often needed in basic scientific research is that the raising spinning efficiency prepares sample fast, learns test result as early as possible.Therefore, we attempt single shower nozzle spinning time of each sample of preparation was shortened in a few minutes from several hours even one day, ultrahigh speed is finished the preparation of laboratory spinning sample, for quickening the basic scientific research process, further improving industrialization macroblock quantization preparation efficiency and lay the first stone.For this reason, we have invented this patent.
Summary of the invention
The purpose of this invention is to provide a kind of high-pressure electrostatic electronics shuttle nano-spun silk device, it has installed the electric liquid pump in the liquid storage cylinder bottom on the basis of static shuttle.The electric liquid pump is adding under the action of alternating magnetic field, spinning solution is produced shaking force and the boosting power that makes progress, make several Taylor's vertebras of electrospinning silk liquid level in the liquid storage cylinder under the acting in conjunction of these two power and high-pressure electrostatic field force, be equivalent on unit are, have the spinning at the same time of a plurality of shower nozzles, thereby make electrospinning silk nanofiber number roll up, and then the spinning efficiency in the unit interval also improve thereupon greatly.This device has that emissivity is stronger, nanofiber diameter is adjustable (by adjusting emitter stage and receiving pole relative distance), energy consumption be low, be not subjected to advantages such as environment (temperature/humidity) influence, easy cleaning.
High-pressure electrostatic electronics shuttle nano-spun silk device of the present invention is made up of non-metal frame, metal receiving system, reception substrate, nanofiber, HV generator, electro-thermostat, the casing in electric liquid pump driver, electric liquid pump, liquid storage cylinder, spinning solution chamber;
Wherein, the electric liquid pump is installed in the liquid storage cylinder bottom, by top electrode and bottom electrode, be positioned at upper and lower interelectrode piezoelectric ceramic piece and form, and and drive circuit form electric liquid pump driver; Electric liquid pump driver is installed in the below of electrode, links to each other with bottom electrode with the top electrode of electric liquid pump with another plain conductor by plain conductor;
The outside of liquid storage cylinder, electric liquid pump and electric liquid pump driver is equipped with non-metal frame, and they are constituted one, becomes static electronics shed open;
HV generator connects lead by metal and links to each other with electric liquid pump driver, and links to each other with the electric liquid pump through another plain conductor, and it and static electronics shed open are formed static electronics shuttle jointly;
Another output of HV generator connects lead through another metal and links to each other with the metal receiving system, and the lower end of metal receiving system is loaded with the reception substrate, is used to receive nanofiber, thereby forms the high-voltage electrostatic spinning electric field; The shape of metal receiving system can be dull and stereotyped or netted, and its receiving area is more than 10 times of liquid storage cylinder emission area, and the metal receiving system can be wire netting or metallic plate; Receive the substrate appendix on the metal receiving system, it can be various macromolecule nonwoven fabric, paper, metallic plate;
Electric liquid pump driver provides driving voltage for the electric liquid pump, the electric liquid pump is produced continuously and the mechanical thrust of fluctuation liquid, thereby make the surface of electric spinning solution in the liquid storage cylinder produce Taylor's vertebra, emission liquid stream under the high-voltage electrostatic spinning effect of electric field, form nanofiber, thereby obtain nano fiber non-woven fabric at the reception substrate;
The present invention carries out the electrospinning silk with high-pressure electrostatic electronics shuttle nano-spun silk device transposition in a rectangular box body, and be provided with electro-thermostat in the bottom of rectangular box body, it make temperature in the casing 10 ~ 50 ° of C scopes in, humidity continuous variation 10 ~ 60 RH scopes in.
The electric liquid pump is a piezoelectric, under signal of telecommunication effect, spinning solution is produced boosting power upwards, this boosting power can make its liquid level produce a large amount of Taylor's vertebras, the quantity of taylor cone is by the voltage decision of high voltage source generator, and voltage changes continuously at 0-80 kV.The material of liquid storage cylinder is glass, plastics or pottery, the multiple geometry of spherical in shape, cylinder, and the bottom of cavity is a little less than the electric liquid pump electrode, so that install; Cavity top is higher than about electrode 10 mm, and it is the end with the top electrode; Liquid storage cylinder, electric liquid pump and electric liquid pump driver are mounted to integrative-structure by non-conductive support, wherein, liquid storage cylinder and electric liquid pump are installed in the top of electric liquid pump driver, non-conductive support is a polytetrafluoroethylplastic plastic, its upper end open also has female thread structure, the sidewall of liquid storage cylinder has external thread structure, and then is installed on the non-conductive support.
The metal receiving system is wire netting or metallic plate.
Receiving substrate is macromolecule nonwoven fabric, paper or metal etc.
High-pressure electrostatic electronics shuttle nano-spun silk device of the present invention can carry out the electrospinning silk at unlimited system (no casing), also can carry out the electrospinning silk in an airtight casing, and the volume of casing is greater than 0.3 m
3Simultaneously be provided with electro-thermostat in the bottom of rectangular box body, electro-thermostat make temperature in the casing 10 ~ 50 ° of C scopes in, humidity continuous variation 10 ~ 60 RH% scopes in.Have automaticity height, easy cleaning, safe and reliable, easy and simple to handle, advantage such as environment is good.
Description of drawings
Fig. 1 is a static electronics shuttle nano-spun silk device structural representation of the present invention.
Fig. 2 is PAN nano fibrous membrane of the present invention (left side) and SEM photo (right side).
Fig. 3 is PVP nano fibrous membrane of the present invention (left side) and SEM photo (right side).
Fig. 4 is U nano fibrous membrane of the present invention (left side) and SEM photo (right side).
Fig. 5 is PVA nano fibrous membrane of the present invention (left side) and SEM photo (right side).
Wherein the name of accompanying drawing 1 each parts is called: 1. electric liquid pump driver, 11. plain conductors, 12. another plain conductors, 2. electric liquid pump, 21. top electrodes, 22. bottom electrodes, 23. piezoelectric ceramic pieces, 3. HV generator, 31. metals connect lead, 41. another metals connect leads, 4. the metal receiving system, 5. liquid storage cylinder, 6. electro-thermostat, 7. non-metal frame, 8. nanofiber, 9. receive substrate, 10. casing.
The specific embodiment
The present invention is before carrying out high-voltage electrostatic spinning, with HV generator 3, spinning voltage is adjustable continuously in 0 ~ 80 kV scope, (model that U.S. GAMMA company produces: output ES30P-5W/DDPM) connects lead 31 by metal and is connected to the top electrode 21 of while as the electric liquid pump 2 at 5 ends of liquid storage cylinder, another output of HV generator 3 connects lead 41 by another metal and is connected to metal receiving system 4, forms the high-pressure electrostatic electric field at 5 ends of liquid storage cylinder and 4 of metal receiving systems;
An output of electric liquid pump driver 1 is connected to the top electrode 21 of electric liquid pump 2 by another plain conductor 12, another output of electric liquid pump driver 1 is connected to the bottom electrode 22 of electric liquid pump 2 by plain conductor 11, thereby for electric liquid pump 2 provides driving voltage, make piezoelectric ceramic piece 23(driving voltage 0V---48V, frequency is 0Hz---2.5MHz) alternating magnetic field of generation in liquid storage cylinder 5, electrospinning liquid is under the effect of alternating magnetic field in the liquid storage cylinder 5, having a boosting power and a vibration force to metal receiving system 4 directions produces, these can make its liquid level produce several Taylor's vertebras, further under the high-voltage electrostatic spinning effect of electric field, form jet, splitting becomes nanofiber, obtains nano fiber non-woven fabric on reception substrate 9.
Further, static electronics shuttle nano-spun silk device of the present invention can be placed an airtight casing 10, in casing 10, be provided with electro-thermostat 6, when carrying out the electrospinning silk, open electro-thermostat 6, the model that Shandong universal love company produces is HWJR-B), thus make the temperature and humidity in the whole box body 10 reach the setting requirement, improve the quality and the effect of spinning.
Liquid storage cylinder 5 is a cylinder, and the lower end of its sidewall is a little less than the upper end of the top electrode 21 of electric liquid pump 2, thereby makes the upper end of top electrode 21 become the end of liquid storage cylinder 5; The sidewall of liquid storage cylinder 5 is higher than about upper end 10 mm of top electrode 21, and the capacity of liquid storage cylinder 5 is used to load electric spinning solution in 1 ~ 5 mL scope; The sidewall of liquid storage cylinder 5 is high dielectric materials such as plastics, pottery or glass.
Liquid storage cylinder 5, electric liquid pump 2, electric liquid pump driver 1 are inlayed the inside that is installed in non-metal frame 7 jointly, constitute the structure of a monolithic stability.
Embodiment 1:
With 0. 4g polyacrylonitrile (PAN, molecular weight: 1,40,000) join in the 9.6 g dimethyl formamides (DMF), utilized the magnetic stirring and dissolving at normal temperatures 2 hours, obtain electric spinning solution; Electric spinning solution 10 ml that obtain are joined in the liquid storage cylinder 5 in the casing 10.Regulate the automatically controlled thermostat in the casing, temperature and humidity reaches 25 ℃ and 30RH% respectively, and level 33.5 cm on dash receiver and the reservoir stablized 2 minutes.
Open HV generator 3 then, slowly transfer to 70 kV; Dash receiver height 33.5 cm.At this moment, the surface of liquid storage cylinder 5 has jet to occur, and splitting takes place, and has the PAN nano fiber non-woven fabric to form on the reception substrate, and spinning finishes in 5 minutes, spinning efficiency 0.08g/min, and average diameter is 200 nm, 20 g/m
2, the photo of PAN nano fibrous membrane and SEM image shows are in accompanying drawing 2[parameter: 4 wt%, U=80 kV, d=33.5 cm, substrate: PP nonwoven fabric] in.
Embodiment 2:
With 0.35g polyvinyl pyrrole Lopa Nationality alkane ketone (PVP, molecular weight: 1,50,000) join in the 9.65 g ethanol, utilize the magnetic stirring and dissolving to obtain electric spinning solution in 2 hours at normal temperatures; Electric spinning solution 10 ml that obtain are joined in the liquid storage cylinder 5 in the casing 10.Regulate the automatically controlled thermostat in the casing, temperature and humidity reaches 25 ℃ and 30RH% respectively, and level 33.5 cm on dash receiver and the reservoir stablized 2 minutes.
Open HV generator 3 then, slowly transfer to 70 kV.At this moment, the surface of liquid storage cylinder 5 has jet to occur, and splitting takes place, and has the PVP nano fiber non-woven fabric to form on the reception substrate, and spinning finishes in 8 minutes, the about 0.043g/min of spinning efficiency, and average diameter is 300 nm, 21 g/m
2, the photo of PVP nano fibrous membrane and SEM image shows are in accompanying drawing 3[parameter: 3.5 wt%, U=70 kV, d=33.5 cm, substrate: PP nonwoven fabric] in.
Embodiment 3:
With 1.0g polyurethane (PU, molecular weight: 1,50,000) join in the mixed solution of 9.0 g oxolane/dimethyl formamides (mol ratio 3:4), utilize the magnetic stirring and dissolving to obtain electric spinning solution in 4 hours at normal temperatures; Electric spinning solution 10 ml that obtain are joined in the liquid storage cylinder 5 in the casing 10.Regulate the automatically controlled thermostat in the casing, temperature and humidity reaches 25 ℃ and 30RH% respectively, and level 19.5 cm on dash receiver and the reservoir stablized 2 minutes.
Open HV generator 3 then, slowly transfer to 80 kV.At this moment, the surface of storage cavity 5 has jet to occur, and splitting takes place, and has the PU nano fiber non-woven fabric to form on the reception substrate, and spinning finishes in 10 minutes, the about 0.1g/ branch of spinning efficiency, and average diameter is 500 nm, 50 g/m
2, the photo of PVP nano fibrous membrane and SEM image shows are in accompanying drawing 4[parameter: 10 wt%, U=80 kV, d=19.5 cm, substrate: PP nonwoven fabric] in.
Embodiment 4:
With 0.6g polyvinyl alcohol (PVA, molecular weight: 90,000) join in the 9.4 g aqueous solution, utilize the magnetic stirring and dissolving to obtain electric spinning solution in 4 hours at normal temperatures; Electric spinning solution 10 ml that obtain are joined in the liquid storage cylinder 5 in the casing 10.Regulate the automatically controlled thermostat in the casing, temperature and humidity reaches 25 ℃ and 30RH% respectively, and level 19.5 cm on dash receiver and the reservoir stablized 2 minutes.
Open HV generator 3 then, slowly transfer to 80 kV.At this moment, the surface of storage cavity 5 has jet to occur, and splitting takes place, and has the PVA nano fiber non-woven fabric to form on the reception substrate, and spinning finishes in 12 minutes, the about 0.05g/ branch of spinning efficiency, and average diameter is 500 nm, 25 g/m
2, the photo of PVP nano fibrous membrane and SEM image shows are in accompanying drawing 5[parameter: 6 wt%, U=80 kV, d=19.5 cm, substrate: PP nonwoven fabric] in.