CN104072773A - Device and method for preparing ultrahigh-viscosity ultrahigh-elasticity breast implant filler - Google Patents
Device and method for preparing ultrahigh-viscosity ultrahigh-elasticity breast implant filler Download PDFInfo
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- CN104072773A CN104072773A CN201310261783.4A CN201310261783A CN104072773A CN 104072773 A CN104072773 A CN 104072773A CN 201310261783 A CN201310261783 A CN 201310261783A CN 104072773 A CN104072773 A CN 104072773A
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Abstract
The invention discloses a device and method for preparing an ultrahigh-viscosity ultrahigh-elasticity breast implant filler. The device comprises a distillation room and a reaction kettle which are connected through a flange, wherein one path of a kettle bottom feed liquid outlet is connected to the top of the distillation room through a gear pump, and the other path of the kettle bottom feed liquid outlet is connected to the top of the reaction kettle; a top feed liquid inlet of the distillation room is communicated with a ring type porous liquid distributor; a disc shunt is arranged below the liquid distributor; a circle of gaps and a circle of baffles are arranged outside the disc of the shunt; a cylindrical liquid film evaporator is arranged in the distillation room; heating medium heating jackets are arranged on an outer wall of the liquid film evaporator and outside the distillation room and the reaction kettle; the top of the distillation room is sequentially connected with a tubular condenser, a recovery tank, a buffer tank, a spiral plate type condenser and a vacuum pump. The preparation method comprises the following steps: sucking raw materials into the reaction kettle, heating and raising the temperature to a polymerization temperature, and reacting for a period of time; further raising the temperature after polymerization is ended, performing circulating distillation, removing low-boiling-point substances in vacuum, and condensing and separating; and ending the operation when distillate is avoided. The evaporation efficiency is high, and the synthesized product is high in purity.
Description
Technical field
The invention belongs to silica gel preparing technical field, relate to preparation facilities and the preparation method of a kind of hyperviscosity, superelevation elastic breast prosthesis filler.
Background technology
Breast prosthesis is all based on a silicon rubber casings at present, and content is to concentrate high viscosity, elastomeric silicon gel on.For preventing the outflow that micro-low molecular weight volatile divides or oozing out, many enterprises have adopted new safer shell complete processing.But no matter how advanced shell-machining process is, to divide and can not effectively take off again lowly if weighting material itself contains a large amount of some low molecular weight volatiles that produce due to conventional polymerization equilibrium reaction, the viscosity of final weighting material and elasticity are just difficult to real raising, and feel is natural.
Therefore research and develop a kind of high viscosity, superelevation elasticity, has anthropoid fat, the natural breast prosthesis filler of realistic hand feeling is industry problem demanding prompt solution.
The basic technology of current conventional silicon gel thermopolymerization is low-molecular-weight D4(cyclic polysiloxanes), catalyzer and desired substance once put in reactor, is then warming up to temperature of reaction, starts reaction, cooling discharge after experience for some time.Due to polymerization equilibrium, in product, must there is some methyl ring siloxane mixtures (DMC), low molecule linear polydimethylsiloxane-, and the degradation production Trimethylamine 99 of catalyzer Tetramethylammonium hydroxide.The existence that these low molecular weight volatiles divide can cause synthetic polymer elasticity, reduced viscosity, and more than molecular diameter is difficult to reach nano level, prosthese breast feel nature not true to nature, cannot reach the effect of anthropoid fat.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, preparation facilities and the preparation method of a kind of hyperviscosity, superelevation elastic breast prosthesis filler is provided.
Technical scheme of the present invention is as follows:
A preparation facilities for hyperviscosity, superelevation elastic breast prosthesis filler, it comprises the distillation reactor of circulation up and down that a top stilling chamber being connected by flange and bottom reactor form; Motor shaft is arranged at the axle center of stilling chamber, reactor, motor shaft and stilling chamber top cover mechanical connection; In reactor, be provided with the U-shaped framework being fixed on motor shaft and scrape wall agitator; The material liquid outlet of Polycondensation Reactor and Esterification Reactor is connected with toothed gear pump inlet duct, toothed gear pump outlet point two-way, and a road is communicated with the cocycle feed liquid entrance on stilling chamber top through cocycle pipeline, and another road is communicated with the lower circulation feed liquid entrance of reactor upper end through lower circulating line; In stilling chamber, cocycle feed liquid entrance is connected with circular ring type porous liquid sparger; Disc type splitter is established in liquid distributor below, splitter disk is provided with near the preglabellar field of motor shaft the interior side shield that feed liquid that a circle can prevent from flowing down from liquid distributor spills, splitter disk outer be provided with that feed liquid that a circle can prevent from flowing down from liquid distributor spills side shield, the outward flange junction of outer side shield and splitter disk is provided with a circle slot; The outward flange of outer side shield and splitter disk is fixed on stilling chamber inwall by horizontal strut; In stilling chamber, be provided with the cylindrical liquid thin-film evaporator on the flange that is fixed on stilling chamber lower end; Fluid film vaporizer outer wall is provided with heating medium for heating chuck; Between the outer wall of fluid film vaporizer and stilling chamber inner-wall surface, there is 2.5～3cm distance; The outer diameter of cylindrical liquid thin-film evaporator is than the large 1.5～2.5cm of the outer peripheral diameter of splitter disk; Stilling chamber and reactor outside are equipped with heating medium for heating chuck; Stilling chamber top is connected with the tubular(surface)condenser outside reactor by pipeline; Light constituent withdrawing can entrance and in, after the parallel connection of heavy constituent withdrawing can entrance, be connected with tubular(surface)condenser; Light constituent withdrawing can outlet and in, after heavy constituent withdrawing can outlet parallel connection, be linked in sequence with spiral sheet condenser, surge tank, vacuum pump.
The condensation area of described spiral sheet condenser is 2.5～3 times of condensation area of described tubular(surface)condenser.
Described vacuum distilling chamber outer wall is provided with toughened glass form, whether to observe feed liquid in circulation; Whether described low-boiling-point substance withdrawing can is provided with pipeline viewing mirror with the tank connected pipeline of buffering, also distillating to observe low-boiling-point substance phlegma.Bottom, vacuum distilling chamber is provided with thermometer insert port.
Utilize the preparation method of hyperviscosity that said apparatus carries out, superelevation elastic breast prosthesis filler as follows: the material vacuum preparing is in advance sucked to a reactor for circulation distillation reactor, heating, is warming up to polymerization temperature reaction for some time; Polymerization is complete, continues to heat up, and enters the circulation distillation stage, first removes G&W, then remove lighting end under vacuum, is condensed and isolates overhead product to tubular(surface)condenser, in finally removing, last running, is condensed and isolates overhead product to spiral sheet condenser; In the time that visor cylinder does not occur phlegma without overhead product, the vacuum tightness of equipment is the highest, and the intake pressure of vacuum pump approaches highest attainable vacuum, not exhaust of system, and vapor liquid equilibrium, now can end operation discharging.
Beneficial effect of the present invention:
Design cycle distillation reactor of the present invention, according to the requirement of separated material, evaporation area, condensation area all expand more than 3 times than traditional reactor; Under certain operational condition, volatile point from steaming the liquid level effusion of being heated, through 2 condensations; This process drag minimization, internal pressure is fallen very little, and therefore reactor can obtain very high vacuum tightness.
Advantage of the present invention: the one, improve vaporization efficiency.The 2nd, sintetics purity is high, and sintetics is waved part and reached 0.1%.The raising of vacuum tightness can make the boiling point of liquid sharply decline, and the raising that this means vacuum tightness makes originally not evaporable low-boiling-point substance in silicone oil, silicon rubber be evaporated completely, thereby has improved the purity of polymkeric substance.The 3rd, circulation distillation reactor is provided with circulation up and down, and cocycle can make low-boiling-point substance constantly circulate and steam, and lower circulation can guarantee that polyreaction raw material and catalyst mix are more evenly quicker.
Brief description of the drawings
Fig. 1 is the structural representation of a kind of hyperviscosity of the present invention, superelevation elastic breast prosthesis filler production equipment;
Fig. 2 is the structural representation of facing of splitter 6 in the present invention and outer part thereof;
Fig. 3 is splitter 6 in the present invention and the plan structure schematic diagram of outer part thereof.
In figure: 1, reactor 2, toothed gear pump 3, U-shaped framework are scraped wall agitator
4, stilling chamber 5, liquid distributor 6, splitter 7, motor shaft
8, top cover 9, fluid film vaporizer 10, tubular(surface)condenser 11, light constituent withdrawing can
12, in, heavy constituent withdrawing can 13, spiral sheet condenser 14, surge tank 15, vacuum pump
16, heating agent enters 17, heating agent goes out 18, heating agent enters 19, heating agent goes out
20, heating agent enters 21, heating agent goes out 22, cocycle feed liquid entrance 23, material liquid outlet
24, pipeline viewing mirror 25, pipeline viewing mirror 26, Heat-transfer Oil Pump 27, heat conduction oil groove
28, lower circulation feed liquid entrance 29, cocycle pipeline valve 30, lower circulating line valve
31, flange 61, outer side shield 62, gap 63, horizontal strut 64, interior side shield
Embodiment
Below in conjunction with drawings and Examples, the present invention is further illustrated.
Embodiment 1
As shown in Figure 1, the preparation facilities of a kind of hyperviscosity of the present invention, superelevation elastic breast prosthesis filler, it comprises the distillation reactor of circulation up and down that a top stilling chamber 4 being connected by flange 31 and bottom reactor 1 form; Motor shaft 7 is arranged at the axle center of stilling chamber, reactor, motor shaft and stilling chamber top cover 8 mechanical connections; In reactor, be provided with the U-shaped framework being fixed on motor shaft and scrape wall agitator 3; The material liquid outlet 23 of Polycondensation Reactor and Esterification Reactor is connected with toothed gear pump 2 inlet ducts, toothed gear pump exports through three reduction of fractions to a common denominator two-way, one tunnel is communicated with the cocycle feed liquid entrance 22 on stilling chamber top through cocycle pipeline, and another road is communicated with the lower circulation feed liquid entrance 28 of reactor upper end through lower circulating line; In stilling chamber, cocycle feed liquid entrance is connected with the circular ring type porous liquid sparger 5 of horizontal positioned; Disc type splitter 6 is established in liquid distributor below, splitter disk is provided with near the preglabellar field of motor shaft 7 the interior side shield 64 that feed liquid that a circle can prevent from flowing down from liquid distributor spills, splitter disk outer be provided with that feed liquid that a circle can prevent from flowing down from liquid distributor spills side shield 61, the slot 62(that outer side shield 61 and the outward flange junction of splitter disk are provided with a circle 1mm is referring to Fig. 2, Fig. 3), can make to accumulate in feed liquid on splitter 6 by this ring shape slot and be membranaceous equably along the outer side of fluid film vaporizer to dirty; The outward flange of outer side shield 61 and splitter disk is fixed on stilling chamber inwall by four horizontal struts 63 that are distributed on same circumference; In stilling chamber, be provided with cylindrical liquid thin-film evaporator 9(on the flange 31 that is fixed on stilling chamber lower end hollow); Fluid film vaporizer outer wall is provided with heating medium for heating chuck (heating agent enters 16, heating agent go out 17); Between the outer wall (being the outside of fluid film vaporizer heating medium for heating chuck) of fluid film vaporizer and stilling chamber inner-wall surface, there is 2.7cm distance; The outer diameter of cylindrical liquid thin-film evaporator is than the large 2cm of the outer peripheral diameter of splitter disk; Stilling chamber outside is provided with heating medium for heating chuck (heating agent enters 18, heating agent go out 19), and reactor outside is provided with heating medium for heating chuck (heating agent enters 20, heating agent go out 21); Stilling chamber top is connected with the tubular(surface)condenser 10 outside reactor by pipeline; Light constituent withdrawing can 11 entrances and in, after the 12 entrance parallel connections of heavy constituent withdrawing can, contact with tubular(surface)condenser 10; Light constituent withdrawing can outlet and in, after heavy constituent withdrawing can outlet parallel connection, with spiral sheet condenser 13, surge tank 14, vacuum pump 15(Roots vacuum system) be linked in sequence.
The condensation area of above-mentioned tubular(surface)condenser 10 is 2 square metres, and the condensation area of above-mentioned spiral sheet condenser 13 is 5 square metres.
Vacuum distilling chamber outer wall is provided with toughened glass form, whether to observe feed liquid in circulation; Whether the pipeline that tubular(surface)condenser 10 is connected with light constituent withdrawing can 11 is provided with pipeline viewing mirror 24, also distillating to observe low-boiling-point substance (light constituent) phlegma; Tubular(surface)condenser 10 with in, the pipeline that is connected of heavy constituent withdrawing can 12 is provided with pipeline viewing mirror 25, whether also distillating to observe the middle and high thing that boils (in, heavy constituent) phlegma.Bottom, vacuum distilling chamber is provided with thermometer insert port, can survey vacuum distilling temperature.
The heating agent using in said apparatus is thermal oil, by Heat-transfer Oil Pump 26, thermal oil is transported to respectively to the heating medium for heating chuck of fluid film vaporizer outside and the heating medium for heating chuck of stilling chamber and reactor outside from heat conduction oil groove 27Fen tri-tunnels.
The principle of work of circulation distillation reactor is as follows: first, toothed gear pump 2 sucks the material liquid outlet 23 of feed liquid autoreaction still bottom, get to the feed liquid entrance 22 on stilling chamber top, feed liquid enters vacuum distilling chamber 4, by liquid distributor 5 be dispersed into liquid film, fluid column becomes droplet-like to fall, then on splitter 6, distribute again, make feed liquid be membranaceous equably along the outer side of fluid film vaporizer to dirty.Because the outside at fluid film vaporizer, stilling chamber outer wall are equipped with heating medium for heating chuck, the feed liquid therefore flowing down is heated evaporation very soon between the outer side of fluid film vaporizer and stilling chamber inner-wall surface.Under vacuum condition, the low-boiling-point substance in the feed liquid of heating can be pumped at 4 tops, vacuum distilling chamber, is condensed and isolates overhead product to tubular(surface)condenser 10; The middle and high thing that boils in the feed liquid of heating can be pumped at 4 tops, vacuum distilling chamber, the cut can not separating to tubular(surface)condenser 10 can deliver to spiral sheet condenser 13 be condensed isolate overhead product (because of the condensation area of tubular(surface)condenser 10 limited, and the condensation area of spiral sheet condenser 13 is 2.5 times of tubular(surface)condenser).Feed liquid after de-low declines towards bottom, again delivers to vacuum distilling chamber, reactor top 4 by toothed gear pump 2 de-low.So iterative cycles, till obtaining qualified product.
Utilize preparation method's (de-low flow process of the distillation reactor that circulates) of hyperviscosity that said apparatus carries out, superelevation elastic breast prosthesis filler as follows: the reactor 1 that the material vacuum preparing is in advance sucked to circulation distillation reactor, heating, is warming up to polymerization temperature reaction for some time; Polymerization is complete, continues to heat up, and enters the circulation distillation stage, first removes G&W, then remove lighting end under vacuum, is condensed and isolates overhead product to tubular(surface)condenser 10, in finally removing, last running, is condensed and isolates overhead product to spiral sheet condenser 13.In the time that visor cylinder does not occur phlegma without overhead product, the vacuum tightness of equipment is the highest, and the intake pressure of vacuum pump 15 approaches highest attainable vacuum, not exhaust of system, and vapor liquid equilibrium, now can end operation, and discharging.
In polymerization stage, close cocycle pipeline valve 29, open lower circulating line valve 30, feed liquid is moved in lower circulating line, circulates by this feed liquid, can guarantee that polyreaction raw material and catalyst mix are more evenly quicker.
Claims (7)
1. a preparation facilities for hyperviscosity, superelevation elastic breast prosthesis filler, is characterized in that, it comprises the distillation reactor of circulation up and down that a top stilling chamber being connected by flange and bottom reactor form; Motor shaft is arranged at the axle center of stilling chamber, reactor, motor shaft and stilling chamber top cover mechanical connection; In reactor, be provided with the U-shaped framework being fixed on motor shaft and scrape wall agitator; The material liquid outlet of Polycondensation Reactor and Esterification Reactor is connected with toothed gear pump inlet duct, toothed gear pump outlet point two-way, and a road is communicated with the cocycle feed liquid entrance on stilling chamber top through cocycle pipeline, and another road is communicated with the lower circulation feed liquid entrance of reactor upper end through lower circulating line; In stilling chamber, cocycle feed liquid entrance is connected with circular ring type porous liquid sparger; Disc type splitter is established in liquid distributor below, splitter disk is provided with near the preglabellar field of motor shaft the interior side shield that feed liquid that a circle can prevent from flowing down from liquid distributor spills, splitter disk outer be provided with that feed liquid that a circle can prevent from flowing down from liquid distributor spills side shield, the outward flange junction of outer side shield and splitter disk is provided with a circle slot; The outward flange of outer side shield and splitter disk is fixed on stilling chamber inwall by horizontal strut; In stilling chamber, be provided with the cylindrical liquid thin-film evaporator on the flange that is fixed on stilling chamber lower end; Fluid film vaporizer outer wall is provided with heating medium for heating chuck; Between the outer wall of fluid film vaporizer and stilling chamber inner-wall surface, there is 2.5～3cm distance; The outer diameter of cylindrical liquid thin-film evaporator is than the large 1.5～2.5cm of the outer peripheral diameter of splitter disk; Stilling chamber and reactor outside are equipped with heating medium for heating chuck; Stilling chamber top is connected with the tubular(surface)condenser outside reactor by pipeline; Light constituent withdrawing can entrance and in, after the parallel connection of heavy constituent withdrawing can entrance, be connected with tubular(surface)condenser; Light constituent withdrawing can outlet and in, after heavy constituent withdrawing can outlet parallel connection, be linked in sequence with spiral sheet condenser, surge tank, vacuum pump.
2. the preparation facilities of hyperviscosity as claimed in claim 1, superelevation elastic breast prosthesis filler, is characterized in that, the condensation area of described spiral sheet condenser is 2.5～3 times of condensation area of described tubular(surface)condenser.
3. the preparation facilities of hyperviscosity as claimed in claim 1 or 2, superelevation elastic breast prosthesis filler, is characterized in that, described vacuum distilling chamber outer wall is provided with toughened glass form.
4. the preparation facilities of hyperviscosity as claimed in claim 3, superelevation elastic breast prosthesis filler, is characterized in that, described low-boiling-point substance withdrawing can is provided with pipeline viewing mirror with the tank connected pipeline of buffering.
5. the preparation facilities of hyperviscosity as claimed in claim 4, superelevation elastic breast prosthesis filler, is characterized in that, bottom, described vacuum distilling chamber is provided with thermometer insert port.
6. the preparation facilities of hyperviscosity as claimed in claim 5, superelevation elastic breast prosthesis filler, it is characterized in that, the heating agent using in described device is thermal oil, by Heat-transfer Oil Pump, thermal oil is transported to respectively to the heating medium for heating chuck of fluid film vaporizer outer wall and the heating medium for heating chuck of stilling chamber and reactor from heat conduction oil groove Fen San road.
A utilization as arbitrary in claim 1-6 as described in the hyperviscosity that carries out of device, the preparation method of superelevation elastic breast prosthesis filler, it is characterized in that: the reactor that the material vacuum preparing is in advance sucked to circulation distiller, heating, is warming up to polymerization temperature reaction for some time; Polymerization is complete, continues to heat up, and enters the circulation distillation stage, first removes G&W, then remove lighting end under vacuum, is condensed and isolates overhead product to tubular(surface)condenser, in finally removing, last running, is condensed and isolates overhead product to spiral sheet condenser; In the time that visor cylinder does not occur phlegma without overhead product, the vacuum tightness of equipment is the highest, and the intake pressure of vacuum pump approaches highest attainable vacuum, not exhaust of system, and vapor liquid equilibrium, now can end operation discharging.
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| CN201310261783.4A CN104072773B (en) | 2013-06-27 | 2013-06-27 | A kind of hyperviscosity, the preparation facilities of super-elastic breast prosthesis filler and preparation method |
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| CN201310261783.4A CN104072773B (en) | 2013-06-27 | 2013-06-27 | A kind of hyperviscosity, the preparation facilities of super-elastic breast prosthesis filler and preparation method |
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| CN104072773A true CN104072773A (en) | 2014-10-01 |
| CN104072773B CN104072773B (en) | 2016-06-29 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107663274A (en) * | 2017-09-27 | 2018-02-06 | 航天材料及工艺研究所 | A kind of silicon rubber purification system, method of purification, purifying silicon rubber and application |
| CN108658155A (en) * | 2018-07-06 | 2018-10-16 | 陈建君 | A kind of physical processing apparatus and method of industry strong acid and strong base high-salt wastewater |
| CN116440803A (en) * | 2023-06-16 | 2023-07-18 | 北京湃普莱恩尼龙新材料技术有限公司 | Preparation process and preparation device of polyamide |
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| CN1154974A (en) * | 1996-09-12 | 1997-07-23 | 化学工业部晨光化工研究院(成都) | Raw-silastic continuously polymerizing apparatus and technology thereof |
| CN101565506A (en) * | 2009-05-25 | 2009-10-28 | 威海赛奥新材料科技有限公司 | Method for preparing medical high-activity silicon oil |
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2013
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1154974A (en) * | 1996-09-12 | 1997-07-23 | 化学工业部晨光化工研究院(成都) | Raw-silastic continuously polymerizing apparatus and technology thereof |
| CN101565506A (en) * | 2009-05-25 | 2009-10-28 | 威海赛奥新材料科技有限公司 | Method for preparing medical high-activity silicon oil |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107663274A (en) * | 2017-09-27 | 2018-02-06 | 航天材料及工艺研究所 | A kind of silicon rubber purification system, method of purification, purifying silicon rubber and application |
| CN107663274B (en) * | 2017-09-27 | 2021-03-26 | 航天材料及工艺研究所 | Silicon rubber purification system, purification method, purified silicon rubber and application |
| CN108658155A (en) * | 2018-07-06 | 2018-10-16 | 陈建君 | A kind of physical processing apparatus and method of industry strong acid and strong base high-salt wastewater |
| CN116440803A (en) * | 2023-06-16 | 2023-07-18 | 北京湃普莱恩尼龙新材料技术有限公司 | Preparation process and preparation device of polyamide |
| CN116440803B (en) * | 2023-06-16 | 2023-09-05 | 北京湃普莱恩尼龙新材料技术有限公司 | Preparation process and preparation device of polyamide |
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