CN105032333B - A kind of method for the device and making for preparing heterogeneous particles filled-type bar polymers material - Google Patents
A kind of method for the device and making for preparing heterogeneous particles filled-type bar polymers material Download PDFInfo
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- CN105032333B CN105032333B CN201510168981.5A CN201510168981A CN105032333B CN 105032333 B CN105032333 B CN 105032333B CN 201510168981 A CN201510168981 A CN 201510168981A CN 105032333 B CN105032333 B CN 105032333B
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Abstract
The present invention relates to a kind of method for the device and making for preparing heterogeneous particles filled-type bar polymers material.A kind of device for preparing heterogeneous particles filled-type bar polymers material, the device includes stepper motor, reaction vessel, stationary platen and thermostat water bath, stationary platen is set in described thermostat water bath, the upper end of described stationary platen sets gear train, one end of described gear train sets connection quarter butt to be connected with described reaction vessel, the other end of described gear train sets connection stock to be connected with described stepper motor, and described stepper motor is by setting the upper end that fixed support is fixed on described thermostat water bath.Reaction unit of the present invention, passes through the effect of gear train and connecting rod, it is possible to achieve reaction is carried out under condition of water bath heating, can be used in the generation of most polymerisations.Have a extensive future.
Description
Technical field
The present invention relates to a kind of device reacted for heteropolymerization and preparation method, more particularly to one kind prepares out-phase
The device of particle-filled type bar polymers material and the method for making.
Background technology
Polymeric material is obtained a wide range of applications in the every field such as industry, agricultural, medical science.With its application neck
The continuous goods station in domain, requirement to polymer performance also more and more higher, exploitation high performance polymer material is increasingly becoming material
The focus of scientific circles.Blending polymerization is reacted as a kind of effective polymeric material method of modifying, receives more and more researchers
Concern.A kind of important kind of blending polymerization reaction is exactly particle filled composite and polymer solution or melt blended, in this process
In, particle and polymer are always out-phase structure, and reactor has strong influence to out-phase reaction.Therefore, design optimization is filled out
The polymerization technique of particle is filled, the final polymeric filling material for obtaining function admirable has become the important topic of Material Field.
In recent years, new construction, the bar polymers of new capability be constantly synthesized, development and application, filled out with heterogeneous particles
Fill that to prepare polymer be focus.Researchers modify particle surface by complicated reaction or selection dispersiveness is preferably molten
Agent, it is intended to improve the dispersiveness in reaction solution of heterogeneous particles.But in polymerization process, heterogeneous particles often because
Reactor bottom is deposited in for Action of Gravity Field, and the means such as stirring or vibration can destroy the club shaped structure of polymer.Therefore need badly
The new reaction unit of exploitation, to prepare the bar polymers of heterogeneous particles filling.
The content of the invention
In order to solve above-mentioned technical problem, an object of the present disclosure provides one kind, and to prepare heterogeneous particles filled-type bar-shaped poly-
The device of compound material, to overcome in polymerization process, heterogeneous particles can be deposited in reactor bottom because of Action of Gravity Field,
And the means such as stirring or vibration can destroy the club shaped structure of polymer.
In order to realize above-mentioned purpose, present invention employs following technical scheme：
A kind of device for preparing heterogeneous particles filled-type bar polymers material, the device includes stepper motor, reaction and held
Stationary platen is set in device, stationary platen and thermostat water bath, described thermostat water bath, the upper end of described stationary platen is set
Put gear train, one end of described gear train sets connection quarter butt to be connected with described reaction vessel, described gear train it is another
One end sets connection stock to be connected with described stepper motor, and described stepper motor is by setting fixed support to be fixed on institute
The upper end for the thermostat water bath stated.
As a further improvement, described connection quarter butt is by setting fixed sleeving to be connected with described reaction vessel, institute
The connection stock stated is by setting connection sleeve pipe to be connected with stepper motor.
As a further improvement, setting controller on described stepper motor.
As a further improvement, described controller is Arduino chips, two main parts are included：Hardware components
It is for doing circuit connection and Arduino circuit boards；Software section is software code Arduino IDE, by the journey in computer
Sequence development environment.
As a further improvement, the material of described reaction vessel is respectively stainless steel, plastics or resin, and it is shaped as post
Shape.
As a further improvement, described reaction vessel includes cylindric blank pipe, sealing-plug and gasket seal, described sky
Pipe upper and lower ends are threaded respectively, and set described gasket seal and sealing-plug to seal respectively by screw thread upper and lower ends.
Second purpose of the invention prepares heterogeneous particles filled-type bar polymers material fabrication process there is provided one kind.
In order to realize above-mentioned purpose, present invention employs following technical scheme：
One kind prepares heterogeneous particles filled-type bar polymers material fabrication process, and this method comprises the following steps：
（1）Thermostat water bath is opened, 40-100 DEG C is adjusted the temperature to；
（2）The lower end of the sealing-plug and gasket seal of lower end and threaded cylindric blank pipe is tightened, with disposable note
Emitter injects rapidly the reaction raw materials mixed liquor containing heterogeneous particles CNT rapidly from the upper end of cylindric blank pipe, extremely adds
Untill full reaction vessel, the gasket seal and sealing-plug of upper end are tightened, that is, adds and finishes；
（3）Reaction vessel is connected on fixed sleeving, is put into thermostat water bath；
（4）Stepper motor is opened, the rotation for adjusting stepper motor by controller is：It is forward and reverse in 1 minute to rotate each 5
Circle, stepper motor is connected by connection sleeve pipe with being connected stock, then connects quarter butt by gear set drive, then passes through fixed cover
Pipe drives reaction vessel to carry out forward and reverse rotate；
（5）After reaction terminates, stepper motor is closed, reaction vessel is removed；Open the sealing of the upper and lower ends of reaction vessel
Plug and gasket seal, the polymeric material in column jecket are touched with sticking plaster, you can obtain heterogeneous particles filled-type bar polymers.
As a further improvement, described reaction raw materials mixed liquor include reaction monomers, crosslinking agent, initiator, pore-foaming agent,
Modifier.
As a further improvement, the preparation method of described reaction raw materials mixed liquor comprises the following steps：
1）2-4mL GMAs, 0.5-1.5 mL glycol dinitrates are measured in 50 mL small beakers
Base acrylate and 5-15 mg CNTs, utilize ultrasonic instrument mixing 4-6min；
2）Mixed liquor adds 0.03-0.07g initiator azodiisobutyronitriles, dissolving after fully mixing；
3）The polymerization inhibitor oxygen in nitrogen 4-6min removal solution is filled with, that is, obtains the reaction raw materials mixed liquor.
As a further improvement, the program arrange parameter of described controller is as follows：Turn to：Rotate forward 1 time to invert 1 time, hand over
Carried out for circulation；When often returning：500 milliseconds；Step angle during four beat runnings：θ=360 degree；Step angle during eight beat runnings：θ=360
Degree；Positioning motor：8-11 pins.
Reaction unit of the present invention, passes through the effect of gear train and connecting rod, it is possible to achieve reaction is in heating water bath
Under the conditions of carry out, can be used in the generation of most polymerisations.Have a extensive future.
Polymer prepared by the present invention, with porous and good permeability, and can be changed by heterogeneous particles
Property after have property, such as can as chromatographic isolation stationary phase, sample extraction scavenging material be applied to analytical chemistry
Field, can also be used as the environmental sciences such as pollutant absorbent.
Brief description of the drawings
Fig. 1 is reaction unit structural representation of the invention.
Fig. 2 is the motor circuit figure of the reaction unit of the present invention.
Fig. 3 is the structural representation of the reaction vessel of the present invention.
Fig. 4 is the organic polymer material structural characterization figure of the invention containing CNT heterogeneous particles.1- contains carbon and received
The scanning electron microscope (SEM) photograph of the organic polymer material of mitron heterogeneous particles；2- contains the organic polymer material of CNT heterogeneous particles
The Raman spectrogram of material；The Raman spectrogram of 3- CNT heterogeneous particles.
Embodiment
The embodiment to the present invention is described in further detail below in conjunction with the accompanying drawings.
A kind of device for preparing heterogeneous particles filled-type bar polymers material as shown in Figure 1, the device includes stepping electricity
Stationary platen 10, institute are set in machine 1, reaction vessel 9, stationary platen 10 and thermostat water bath 11, described thermostat water bath 11
The upper end for the stationary platen 10 stated sets gear train 6, and one end of described gear train 6 sets connection quarter butt 7, and described connection is short
Bar 7 is by setting fixed sleeving 8 to be connected with described reaction vessel 9, and the other end of described gear train 6 sets connection stock 5,
Described connection stock 5 is by setting connection sleeve pipe 3 to be connected with stepper motor 1, and described stepper motor 1 is by setting fixed branch
Frame 4, which is fixed on the upper end of described thermostat water bath 11, described stepper motor 1, sets controller 2.
Shown controller 2 is Arduino chips, includes two main parts：Hardware components are for doing circuit company
Connect and Arduino circuit boards；Software section is software code Arduino IDE, by the programming development environment in computer.
The material of described reaction vessel 9 is respectively stainless steel, and is shaped as column.
As shown in figure 3, described reaction vessel 9 includes blank pipe 13, sealing-plug 14 and gasket seal 12, described blank pipe 13
Upper and lower ends port is sealed by the gasket seal 12 and sealing-plug 14 described in setting respectively.Described blank pipe 13 is cylindric sky
Pipe, the length of cylindric blank pipe is 3.0 cm, a diameter of 4.6 mm, and upper and lower ends are threaded respectively.
One kind prepares heterogeneous particles filled-type bar polymers material fabrication process, and this method comprises the following steps：
1）Thermostat water bath 11 is opened, 60 DEG C are adjusted the temperature to；
2）The lower end of the sealing-plug 14 and gasket seal 12 and threaded cylindric blank pipe of lower end is tightened, with disposable
Syringe injects rapidly the reaction raw materials mixed liquor containing heterogeneous particles CNT rapidly from the upper end of cylindric blank pipe, extremely
Untill filling it up with reaction vessel 9, the gasket seal 12 and sealing-plug 14 of upper end are tightened, that is, adds and finishes；
3）Reaction vessel 9 is connected on fixed sleeving 8, is put into thermostat water bath 8；
4）Stepper motor 1 is opened, the rotation for adjusting stepper motor 1 by controller 2 is：It is forward and reverse in 1 minute to rotate each 5
Circle, stepper motor 1 is connected by connection sleeve pipe 3 with being connected stock 5, then drives connection quarter butt 7 by gear train 6, is then passed through
Fixed sleeving 8 drives reaction vessel 9 to carry out forward and reverse rotation；
5）After reaction terminates, stepper motor 1 is closed, reaction vessel 9 is removed；Open reaction vessel 9 upper and lower ends it is close
Blocking 14 and gasket seal 12, the polymeric material in column jecket is touched with sticking plaster, you can obtain heterogeneous particles filled-type bar-shaped
Polymer.
Described reaction raw materials mixed liquor includes reaction monomers, crosslinking agent, initiator, pore-foaming agent, modifier.
The preparation method of described reaction raw materials mixed liquor comprises the following steps：
1）3mL GMAs, 1 mL ethylene glycol dimethacrylates are measured in 50 mL small beakers
With 10 mg CNTs, ultrasonic instrument mixing 5min is utilized；
2）Mixed liquor adds 0.05g initiator azodiisobutyronitriles, dissolving after fully mixing；
3）The polymerization inhibitor oxygen in nitrogen 5min removal solution is filled with, that is, obtains the reaction raw materials mixed liquor.
The program arrange parameter of described controller 2 is as follows：Turn to：Rotate forward 1 time to invert 1 time, alternate cycles are carried out；Every turn
Delay：500 milliseconds；Step angle during four beat runnings：θ=360 degree；Step angle during eight beat runnings：θ=360 degree；Positioning motor：8-11
Pin.
Claims (4)
1. a kind of method for preparing heterogeneous particles filled-type bar polymers material, it is characterised in that the device that this method is used
Including stepper motor (1), reaction vessel (9), stationary platen (10) and thermostat water bath (11), described thermostat water bath (11)
Interior setting stationary platen (10), the upper end of described stationary platen (10) sets gear train（6）, described gear train（6）One
End sets connection quarter butt（7）It is connected with described reaction vessel (9), described gear train（6）The other end set connection stock
（5）It is connected with described stepper motor (1), described stepper motor (1) is by setting fixed support (4) to be fixed on described perseverance
Controller (2) is set on the upper end of warm water bath (11), described stepper motor (1)；Described reaction vessel (9) includes cylinder
Shape blank pipe（13）, sealing-plug（14）And gasket seal（12）, described blank pipe（13）Upper and lower ends are threaded respectively, and are passed through
Screw thread upper and lower ends set described gasket seal respectively（12）And sealing-plug（14）Sealing；Described method includes following step
Suddenly：
1）Open thermostat water bath（11）, adjust the temperature to 40-100 DEG C；
2）By the sealing-plug of lower end（14）And gasket seal（12）Tightened with the lower end of threaded cylindric blank pipe, with disposable
Syringe injects the rapid upper end from cylindric blank pipe of the reaction raw materials mixed liquor containing heterogeneous particles CNT, to filling it up with
Reaction vessel（9）Untill, tighten the gasket seal of upper end（12）And sealing-plug（14）, that is, add and finish；
Described reaction raw materials mixed liquor includes reaction monomers, crosslinking agent, initiator, pore-foaming agent, modifier；Described reaction is former
The preparation method of material mixed liquor comprises the following steps：Measured in 50 mL small beakers 2-4mL GMAs,
0.5-1.5 mL ethylene glycol dimethacrylates and 5-15 mg CNTs, utilize ultrasonic instrument mixing 4-6min；Mixing
Liquid adds 0.03-0.07g initiator azodiisobutyronitriles, dissolving after fully mixing；Nitrogen 4-6min is filled with to remove in solution
Polymerization inhibitor oxygen, that is, obtain the reaction raw materials mixed liquor；
3）By reaction vessel（9）It is connected in fixed sleeving（8）On, it is put into thermostat water bath（11）It is interior；
4）Open stepper motor（1）, pass through controller（2）Adjust stepper motor（1）Rotation be：It is forward and reverse in 1 minute to rotate
Each 5 circle, stepper motor（1）Pass through connection sleeve pipe（3）With being connected stock（5）It is connected, then passes through gear train（6）Drive connection quarter butt
（7）, then pass through fixed sleeving（8）Drive reaction vessel（9）Carry out forward and reverse rotate；
Controller（2）Program arrange parameter it is as follows：Turn to：Rotate forward 1 time to invert 1 time, alternate cycles are carried out；When often returning：500
Millisecond；Step angle during four beat runnings：θ=360 degree；Step angle during eight beat runnings：θ=360 degree；Positioning motor：8-11 pins；
5）After reaction terminates, stepper motor is closed（1）, remove reaction vessel（9）；Open reaction vessel（9）Upper and lower ends
Sealing-plug（14）And gasket seal（12）, the polymeric material in column jecket is touched with sticking plaster, you can obtain heterogeneous particles filling
Type bar polymers.
2. according to the method described in claim 1, it is characterised in that：Described connection quarter butt（7）By setting fixed sleeving（8）
It is connected with described reaction vessel (9), described connection stock（5）By setting connection sleeve pipe（3）With stepper motor (1) phase
Even.
3. according to the method described in claim 1, it is characterised in that：Shown controller (2) is Arduino chips, includes two
Individual main part：Hardware components are for doing circuit connection and Arduino circuit boards；Software section is software code
Arduino IDE, by the programming development environment in computer.
4. according to the method described in claim 1, it is characterised in that：Described reaction vessel（9）Material be stainless steel, plastics
Or resin, and it is shaped as column.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510168981.5A CN105032333B (en) | 2015-04-10 | 2015-04-10 | A kind of method for the device and making for preparing heterogeneous particles filled-type bar polymers material |
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|---|---|---|---|
| CN201510168981.5A CN105032333B (en) | 2015-04-10 | 2015-04-10 | A kind of method for the device and making for preparing heterogeneous particles filled-type bar polymers material |
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| Publication Number | Publication Date |
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| CN105032333A CN105032333A (en) | 2015-11-11 |
| CN105032333B true CN105032333B (en) | 2017-08-25 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1410455A (en) * | 2002-03-14 | 2003-04-16 | 四川大学 | Preparation method of polymer/carbon nano pipe composite emulsion and its in situ emulsion polymerization |
| US8084544B2 (en) * | 2005-07-04 | 2011-12-27 | Sumitomo Seika Chemicals Co., Ltd. | Process for production of water-absorbing resin |
| CN104195042A (en) * | 2014-07-27 | 2014-12-10 | 北京化工大学 | Preparation method and application of nano material monolithic column immobilized enzyme biological micro-reactor |
| CN104307497A (en) * | 2014-10-12 | 2015-01-28 | 北京工业大学 | Rotating device for ultraviolet polymerization preparation of capillary micro/nano particle copolymerization monolithic column |
| CN204620002U (en) * | 2015-04-10 | 2015-09-09 | 浙江省中医药研究院 | A kind of device preparing heterogeneous particles filled-type bar polymers material |
-
2015
- 2015-04-10 CN CN201510168981.5A patent/CN105032333B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1410455A (en) * | 2002-03-14 | 2003-04-16 | 四川大学 | Preparation method of polymer/carbon nano pipe composite emulsion and its in situ emulsion polymerization |
| US8084544B2 (en) * | 2005-07-04 | 2011-12-27 | Sumitomo Seika Chemicals Co., Ltd. | Process for production of water-absorbing resin |
| CN104195042A (en) * | 2014-07-27 | 2014-12-10 | 北京化工大学 | Preparation method and application of nano material monolithic column immobilized enzyme biological micro-reactor |
| CN104307497A (en) * | 2014-10-12 | 2015-01-28 | 北京工业大学 | Rotating device for ultraviolet polymerization preparation of capillary micro/nano particle copolymerization monolithic column |
| CN204620002U (en) * | 2015-04-10 | 2015-09-09 | 浙江省中医药研究院 | A kind of device preparing heterogeneous particles filled-type bar polymers material |
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