CN102120094A - Method for removing small molecules from silicone gel by molecular distillation - Google Patents
Method for removing small molecules from silicone gel by molecular distillation Download PDFInfo
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- CN102120094A CN102120094A CN2011100095258A CN201110009525A CN102120094A CN 102120094 A CN102120094 A CN 102120094A CN 2011100095258 A CN2011100095258 A CN 2011100095258A CN 201110009525 A CN201110009525 A CN 201110009525A CN 102120094 A CN102120094 A CN 102120094A
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Abstract
The invention discloses a method for removing small molecules from silicone gel by molecular distillation, which is characterized in that: a material is radically added into a molecular distiller from a place above a heating area and is distributed to a heating wall face by a distributor, the temperature, vacuum degree and rotation speed of scraper are controlled, and thus, the material is spread to form a liquid film with uniform thickness and is pushed downwards in a spiral manner; and after the material is heated, light molecules move upwards and condense into liquid when contacting a condenser in the molecular distiller, and heavy molecules move downwards along the wall of the distiller to be recovered. The method is used for removing small molecules (such as D3, D4, D5 and ketone, hydroxyl and phenyl compounds) from silicone gel in silicon rubber breast implanted products and can ensure the volatile matter of raw rubber is less than 0.1 percent.
Description
Technical field
The present invention relates to a kind of silicon rubber breast implant product silicon gel and remove micromolecular method, particularly a kind of employing molecular clock is removed micromolecular method in the silicon gel.
Background technology
The breast prosthesis divides two kinds of fundamental types, and promptly the silicon rubber shell of the silicone rubber seal housing apparatus of filling gel and expansive filled normal saline solution has comprised a check valve apparatus that can be used for filling.
The breast prosthesis of filling gel puts into biogel in the silicone rubber seal shell in advance, constant volume, the silicon rubber breast prosthesis of this filling gel has and tissue similar density and flexibility, implants that the rear udder attachment form is true to nature, feel is good, wherein with silicon gel typical case the most.Silicon gel silicone-gel is different with silicone oil silicone oil.Once adopting silicone oil (dimethicone) in early days is filler, and this liquid silicone oil in case silicone rubber seal shell (shell) breaks in vivo, will trickle along tissue space, because be oiliness, may remove clean hardly.Appear in the newspapers and the tissue disease that a large amount of silicone oil may cause clinically more.The silicon gel then is through over cure, the high polymer that is cross-linked to form, has certain viscoplasticity and macromolecular network structure, and gel can not trickle, be and freeze shape.Silicon rubber breast prosthesis with the silicon gel filling is the most general in clinical practice so far.
Although breast prosthesis's fundamental type and structure do not have much variations for many years, yet on, prescription synthetic and the manufacture craft bigger improvement (seeing the preparation of silicon gel) is arranged all, more to adapt to the requirement of clinical continuous development at material.The little molecule seepage discharge of filling breast prosthesis silicone oil of producing as the U.S. 60-70 age is 1 to 2 gram, and gel is higher to the swelling ratio of silicone rubber housings.
Rubber is that obtaining end group is the fluidised form polysiloxanes (silicone oil that is commonly called as) of vinyl by octamethylcy-clotetrasiloxane (D4) and the polymerization of closure agent tetramethyl divinyl two silicon ethers (MMVi) head and the tail.
Reaction equation:
D
4+ closure agent → CH
2=CH-Si-O (Si-O)
nCH=CH
2
The silicon gel be rubber under the effect of catalyst chloroplatinic acid, crosslinked make suitable with the crosslinking agent containing hydrogen silicone oil.Its medium and small molecule (lighter molecules) is common D
4, D
5, benzene class, ketone, heterocyclic, alkanes etc.
The little molecule of silicon gel is to be diffused into easily in the human body under the situation of outer casing rupture, and the U.S. has released the breast prosthesis of dual structure in the eighties to market, and internal layer is the silicon gel, and skin is a physiological saline.Clinical practice shows that in case the shell seepage or the shell that breaks will form fold, this fold not only influences breast shape, and very easily brings out the fibrous capsule contracture, and in fact clinical practice does not reach the effect of expected design, so seldom be used for clinical abroad.
In early days, French PIP company adopts hydroxypropyl methylcellulose (HPMC), is used for the silicon rubber breast prosthesis through after the modification, and this gel is formulated by the aseptic deionized water of 3% hydroxypropyl methylcellulose and 97%.Therefore HPML degree of gelation after the modification is higher, has soft feel, but it is said also metabolism in vivo, but the clinical practice report is more rare.
The eighties middle and later periods, the hyposmosis type silicon gel breast prosthesis's who puts goods on the market infiltration capacity has been controlled in the very little scope, and degree of gelation improves, but gel is very soft, and overall flow situation is good.
McGhan company utilizes the earliest and applies the anti-penetration layer technology, plays the effect of Isolated Shield between sulphurated siliastic shell and silicon gel, thereby stops the medium and small molecule infiltration of silicon gel.Promptly reducing the fugitive constituent in the rubber, is the key of dealing with problems.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of employing molecular clock and remove micromolecular method in the silicon gel, reduce the fugitive constituent of silicon gel, thereby stop the medium and small molecule seepage of silicon gel, can reduce below the fugitive constituent to 0.1% of silicon gel.
The present invention realizes by following technical scheme:
A kind of employing molecular clock is removed micromolecular method in the silicon gel, material is radially added molecular still from top, the thermal treatment zone, be distributed to heating wall through distributing device, control temperature, vacuum, scraper plate rotating speed spread to the uniform liquid film of thickness with material and advance downwards with helical form; The material back lighter molecules of being heated forms the steam condenser of meeting molecular still inside that moves upward and condenses into fluid separation applications, and heavy molecules moves downward along wall and flows down recovery.
Described material can also add thin film evaporator before adding molecular still, be specially material is radially added thin film evaporator from top, the thermal treatment zone, be distributed to heating wall through distributing device, control temperature, vacuum, scraper plate rotating speed spread to the uniform liquid film of thickness with material and advance downwards with helical form; Lighter molecules formed the vapor stream rising after material was heated, and arrived the external condenser that thin film evaporator directly links to each other through gas-liquid separator, and heavy molecules is discharged bottom thin film evaporator.
The temperature of described molecular clock is 130-250 ℃, wherein is preferably 170-200 ℃.
The vacuum of described molecular clock is 0.02Mpa-0.05Mpa, wherein is preferably 0.025-0.032Mpa.
The scraper plate rotating speed of described molecular clock is 20-30rad/min.
The temperature of described thin film evaporation is 130-250 ℃, wherein is preferably 160-170 ℃.
The vacuum of described thin film evaporation is 0.02Mpa-0.05Mpa, wherein is preferably 0.03-0.035Mpa.
The scraper plate rotating speed of described thin film evaporation is 20-30rad/min.
Described material all remains on heating wall in thin film evaporator and in the molecular still spreading depth is 0.5-2mm, is preferably 0.5-1mm.
Concrete workflow is: get the rubber that preparation is finished, wherein contain D
3, D
4, D
5, micromolecular compound such as ketone, hydroxy kind, phenyl class, fugitive constituent is higher;
At first material is radially fed thin film evaporator from the top of the thermal treatment zone, be distributed to heating wall through distributing device, the control temperature is that 130-250 ℃, vacuum are 0.02Mpa-0.05Mpa, scraper plate rotating speed 20-30rad/min, Xuan Zhuan blade applicator spreads to the uniform liquid film of thickness continuously uniformly with material and advances downwards with helical form on heating surface then, THICKNESS CONTROL is between 0.5-2mm, in this process, continuous and the uniform liquid film of blade applicator assurance of rotation produces tells turbulent flow, and stop liquid film coking on heating surface, fouling, thereby improved mass tranfer coefficient; Lighter molecules formed the vapor stream rising after material was heated, and arrived the external condenser that thin film evaporator directly links to each other through gas-liquid separator, and heavy molecules is discharged collection bottom thin film evaporator.
The above-mentioned material of collecting of discharging from the thin film evaporator bottom is proceeded molecular clock, the condensing unit of molecular still is mounted in its inside, material is radially added molecular still from top, the thermal treatment zone, be distributed to heating wall through distributing device, the control temperature is that 130-250 ℃, vacuum are that 0.02Mpa-0.05Mpa, scraper plate rotating speed are 20-30rad/min, material is spread to the uniform liquid film of thickness advance downwards, keep thickness between 0.5-2mm with helical form; The material back lighter molecules of being heated forms the steam condenser of meeting molecular still inside that moves upward and condenses into fluid separation applications, and heavy molecules moves downward along wall and flows down recovery.Wherein, make that vacuum pump-down is very little, can keep the device interior higher vacuum because the lighter molecules gas phase is condensed in molecular still inside.By molecular motion mean free path principle as can be known, the operating temperature of molecular still does not need boiling far below the boiling point of material; The short-path distillation heated time is short, only is tens seconds.
Promptly slough boiling point little molecule from low to high respectively by thin film evaporation and molecular clock, thereby reduce the fugitive constituent of rubber, material can be repeatedly by the processing of thin film evaporation and molecular clock, constantly regulate temperature, pressure removes different little molecules with the scraper plate rotating speed, finally can reach the rubber fugitive constituent that makes after the processing less than 0.1%.
Beneficial effect of the present invention is:
(1) material is short by the molecular clock processing time, only is tens seconds at every turn, can repeatedly handle repeatedly, does not influence manufacturing schedule;
(2) fugitive constituent that can make rubber makes the synthetic silicon gel of rubber have better biocompatibility less than 0.1%, nontoxic, aseptic, suitable long-term the implantation;
(3) after removing little molecule, make its surface clean transparent, free from admixture, modest viscosity, the phenomenon of seepage can not appear in the silicon gel of production.
The specific embodiment
Below in conjunction with embodiment, the present invention will be further described.
D
4+ closure agent → CH
2=CH-Si-O (Si-O)
nCH=CH
2
By the synthetic rubber of above-mentioned reaction, and molecular weight to be controlled at n value be 200-400, the fugitive constituent that records sample is about 1.10-1.56%, gets four samples respectively and carries out the present invention and remove micromolecular processing.
Embodiment 1
Get four identical samples of fugitive constituent, keeping thickness of liquid film is 1.2mm, and the scraper plate rotating speed is to carry out processing of the present invention under the condition of 20rad/mi n, begins to have lighter molecules to ooze from condenser in the time of 130 ℃, handles as table 1.
Table 1
| Treatment conditions | Fugitive constituent 1/% | Fugitive constituent 2/% | Fugitive constituent 3/% | Fugitive constituent 4/% |
| 150 ℃ of thin film evaporation+molecular clock 28Pa | 0.12 | 0.23 | 0.20 | 0.18 |
| 150 ℃ of molecular clocks, 32Pa | 0.19 | 0.23 | 0.20 | 0.20 |
| 170 ℃ of molecular clocks, 31Pa | 0.07 | 0.07 | 0.12 | 0.086 |
| 190 ℃ of molecular clocks, 30pa | 0.07 | 0.05 | 0.06 | 0.06 |
| 150 ℃ of molecular clock secondaries, 26Pa | 0.08 | 0.09 | 0.09 | 0.086 |
| 170 ℃ of molecular clock secondaries, 25Pa | 0.05 | 0.02 | 0.02 | 0.03 |
It is good more to draw the high more distilling effect of temperature by table 1; It is good to handle twice ratio processing effect once under the identical temperature.
Embodiment 2
Get four different samples of fugitive constituent, wherein sample 1 and 2 fugitive constituent are 1.25%, sample 3 and 4 fugitive constituent are 1.55%, keeping thickness of liquid film is 0.8mm, the scraper plate rotating speed is to carry out processing of the present invention under the condition of 30rad/min, in the time of 130 ℃, begin to have lighter molecules to ooze, handle as table 2 from condenser.
Table 2
| Treatment conditions | Fugitive constituent 1/% | Fugitive constituent 2/% | Fugitive constituent 3/% | Fugitive constituent 4/% |
| 180 ℃ of thin film evaporation+molecular clock 25Pa | 0.10 | 0.08 | 0.15 | 0.18 |
| 170 ℃ of molecular clocks, 28Pa | 0.15 | 0.13 | 0.18 | 0.16 |
| 180 ℃ of molecular clocks, 27Pa | 0.12 | 0.10 | 0.13 | 0.15 |
| 190 ℃ of molecular clock 26pa | 0.07 | 0.05 | 0.06 | 0.06 |
| 180 ℃ of molecular clock secondaries, 26Pa | 0.05 | 0.02 | 0.05 | 0.07 |
| 190 ℃ of molecular clock secondaries, 25Pa | 0.03 | 0.02 | 0.06 | 0.05 |
By table 2 can draw the rubber sample be untreated before little molecule content few more, vacuum is good more in the processing procedure, treatment effect can promote.
Embodiment 3
Get four identical samples of fugitive constituent, keeping thickness of liquid film is 1mm, and the scraper plate rotating speed is to carry out processing of the present invention under the condition of 25rad/min, begins to have lighter molecules to ooze from condenser in the time of 130 ℃, handles as table 3.
Table 3
| Treatment conditions | Fugitive constituent 1/% | Fugitive constituent 2/% | Fugitive constituent 3/% | Fugitive constituent 4/% |
| 190 ℃ of thin film evaporation+molecular clock 25Pa | 0.03 | 0.05 | 0.05 | 0.04 |
| 180 ℃ of molecular clocks, 26Pa | 0.10 | 0.09 | 0.08 | 0.06 |
| 190 ℃ of molecular clocks, 25Pa | 0.05 | 0.03 | 0.03 | 0.03 |
| 200 ℃ of molecular clock 25pa | 0.05 | 0.05 | 0.03 | 0.02 |
| 180 ℃ of molecular clock secondaries, 26Pa | 0.05 | 0.02 | 0.05 | 0.02 |
| 190 ℃ of molecular clock secondaries, 25Pa | 0.03 | 0.02 | 0.06 | 0.05 |
Can be drawn by table 3, the preferred treatment temperature of the present invention is 170-200 ℃, and preferred vacuum is 0.025-0.032Mpa.
Single molecular clock, thin film evaporation and the molecular clock selected except the foregoing description use simultaneously; And under the condition of different thickness of liquid films, temperature, vacuum, scraper plate rotating speed, can also in scope disclosed by the invention, select different experiment conditions once more, all can reach effect of the present invention.
Prove that by the above embodiments the fugitive constituent that method of the present invention can make rubber (is generally carried out according to U.S. ASTM F703-96 standard) within industrial standard, for fugitive constituent less than 1%.And optimum condition method of the present invention can also make fugitive constituent between 0.1-0.3%, when selecting appropriate condition, can also reach below 0.1%.
Get by the arbitrary rubber sample after the present invention's processing and carry out the technical indicator test, the result is as follows:
| Pilot project | Technical indicator | Experimental technique |
| Outward appearance | Clear ﹠ Transparent, do not have visible impurity | Range estimation |
| The volatility thing (150 ℃, 4hr) | ≤0.5％ | Oven Method |
| Viscosity (cp) | 1200-1600 | Rotation viscometer |
Above-mentioned rubber product meets U.S. ASTM F703-96 standard, and safe by the silicon gel products of above-mentioned rubber preparation, good biocompatibility.According to the YY0647-2008 requirement, housing and above-mentioned silicon gel are done biocompatibility test respectively.
Project has:
1. cell toxicity test 8. long-term Implantation Tests
2. whole body acute toxicity test 9. genetoxics
3. hemolytic test 10. chronic general toxicities
4. sensitization test (STT) 11. genotoxicities
5. pyrogen testing 12. immunotoxicities
6. intracutaneous irritant test
7. aseptic
All reach the safety standard level, and on average be higher than the safety standard level more than 30%, repeat no more Safety shell herein and above-mentioned silicon gel is done biocompatibility test respectively.
Processing method of the present invention makes pure higher of follow-up silicon gel, is ad eundem silica gel material product the best in quality.
Claims (9)
1. one kind is adopted molecular clock to remove micromolecular method in the silicon gel, it is characterized in that material is radially added molecular still from top, the thermal treatment zone, be distributed to heating wall through distributing device, control temperature, vacuum, scraper plate rotating speed spread to the uniform liquid film of thickness with material and advance downwards with helical form; The material back lighter molecules of being heated forms the steam condenser of meeting molecular still inside that moves upward and condenses into fluid separation applications, and heavy molecules moves downward along wall and flows down recovery.
2. employing molecular clock as claimed in claim 1 is removed micromolecular method in the silicon gel, it is characterized in that described material can also add thin film evaporator before adding molecular still, be specially material is radially added thin film evaporator from top, the thermal treatment zone, be distributed to heating wall through distributing device, control temperature, vacuum, scraper plate rotating speed spread to the uniform liquid film of thickness with material and advance downwards with helical form; Lighter molecules formed the vapor stream rising after material was heated, and arrived the external condenser that thin film evaporator directly links to each other through gas-liquid separator, and heavy molecules is discharged bottom thin film evaporator.
3. employing molecular clock as claimed in claim 1 is removed micromolecular method in the silicon gel, and the temperature that it is characterized in that described molecular clock is 130-250 ℃, wherein is preferably 170-200 ℃.
4. employing molecular clock as claimed in claim 1 is removed micromolecular method in the silicon gel, and the vacuum that it is characterized in that described molecular clock is 0.02Mpa-0.05Mpa, wherein is preferably 0.025-0.032Mpa.
5. employing molecular clock as claimed in claim 1 is removed micromolecular method in the silicon gel, and the scraper plate rotating speed that it is characterized in that described molecular clock is 20-30rad/min.
6. employing molecular clock as claimed in claim 1 or 2 is removed micromolecular method in the silicon gel, and the temperature that it is characterized in that described thin film evaporation is 130-250 ℃, wherein is preferably 160-170 ℃.
7. employing molecular clock as claimed in claim 1 or 2 is removed micromolecular method in the silicon gel, and the vacuum that it is characterized in that described thin film evaporation is 0.02Mpa-0.05Mpa, wherein is preferably 0.03-0.035Mpa.
8. employing molecular clock as claimed in claim 1 or 2 is removed micromolecular method in the silicon gel, and the scraper plate rotating speed that it is characterized in that described thin film evaporation is 20-30rad/min.
9. employing molecular clock as claimed in claim 1 or 2 is removed micromolecular method in the silicon gel, it is characterized in that described material all remains on heating wall in thin film evaporator and in the molecular still spreading depth is 0.5-2mm, is preferably 0.5-1mm.
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Cited By (5)
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| CN103349845A (en) * | 2013-07-27 | 2013-10-16 | 上海泰坦科技股份有限公司 | Molecular rectification and purification technology of heterocyclic compound |
| 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 |
| CN112023429A (en) * | 2020-08-11 | 2020-12-04 | 中天东方氟硅材料有限公司 | Method for removing low molecules of low-viscosity silicone oil |
| CN112867726A (en) * | 2021-01-25 | 2021-05-28 | 安徽金禾实业股份有限公司 | Production equipment and production method of sucrose-6-ester |
| CN113698605A (en) * | 2021-09-27 | 2021-11-26 | 矽时代材料科技股份有限公司 | Preparation method of high-purity polysiloxane |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103349845A (en) * | 2013-07-27 | 2013-10-16 | 上海泰坦科技股份有限公司 | Molecular rectification and purification technology of heterocyclic compound |
| 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 |
| CN112023429A (en) * | 2020-08-11 | 2020-12-04 | 中天东方氟硅材料有限公司 | Method for removing low molecules of low-viscosity silicone oil |
| CN112867726A (en) * | 2021-01-25 | 2021-05-28 | 安徽金禾实业股份有限公司 | Production equipment and production method of sucrose-6-ester |
| CN113698605A (en) * | 2021-09-27 | 2021-11-26 | 矽时代材料科技股份有限公司 | Preparation method of high-purity polysiloxane |
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