CN103642045A - Efficient low molecule removal method for low viscosity silicone oil - Google Patents
Efficient low molecule removal method for low viscosity silicone oil Download PDFInfo
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- CN103642045A CN103642045A CN201310594477.2A CN201310594477A CN103642045A CN 103642045 A CN103642045 A CN 103642045A CN 201310594477 A CN201310594477 A CN 201310594477A CN 103642045 A CN103642045 A CN 103642045A
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Abstract
The invention discloses an efficient low molecule removal method for low viscosity silicone oil, and the method can be used in the silicone oil low molecule removal field. The method provided by the invention adopts a two-stage separation system containing an ordinary vacuum separation system and a high vacuum separation system. Most low molecules are removed in the ordinary vacuum separation system, and low molecules are further removed in the high vacuum separation system so as to make the volatile content less than 0.2%. The two-stage separation system adopts two different vacuum systems, the vacuum degree of the two-stage separation system is ensured and the product volatile content is ensured, thus guaranteeing the product quality. At the same time, the low molecule removal feed amount is greatly improved, thereby enhancing the production efficiency. In addition, in the invention, silicone oil flows from a high temperature region to a low temperature region, thus effectively saving energy consumption and reducing the cost of investment.
Description
Technical field
The present invention, for the de-low field of silicone oil, particularly relates to the efficiently de-low molecular method of a kind of silicone oil with low viscosity.
Background technology
The de-low molecule of silicone oil is by volatile matter, as ring body forwards gas phase to from liquid phase, and separated process in addition.The feed composition of silicone oil is more, and its de-low molecule manipulation is more complicated.Along with standard of living improves constantly, people improve constantly the specification of quality of commodity, and now a lot of clients require silicone oil product fugitive constituent to be less than 0.5%, and some high-end field, as aerospace field, field of medicaments etc. require higher to silicone oil fugitive constituent.In silicone oil production process, the energy that de-low molecular process consumes accounts for 60%～70% of whole production process.Therefore, the quality of de-low molecule technique, directly affects silicone oil quality product and production cost.
The low molecule that removes of silicone oil with low viscosity has two kinds of modes at present, and the one, intermittent type: silicone oil and end-capping reagent after synthetic silicone oil, directly remove low molecule under catalyst action under reduced pressure in reactor.The shortcoming of this kind of mode: the de-low time is long, and efficiency is low, and energy consumption is high, batch fluctuation of product fugitive constituent is large, is not suitable for producing extension, takes the product of this de-low mode, and its fugitive constituent can only remain on 1% left and right; The 2nd, continous way: preheater one or more thin-film evaporators of connecting remove low molecule under same vacuum system.Because silicone oil with low viscosity viscosity is less, be difficult in thin-film evaporator, form liquid film, adopt single thin-film evaporator, make equipment effectiveness low, and can not guarantee product volatile content, be not suitable for silicone oil with low viscosity and remove low molecule; Adopt a plurality of thin-film evaporators parallel connections or be together in series, although can to a certain degree guarantee product volatile content, its equipment investment cost is high, energy consumption is large.
The general half-finished low molecule content of silicone oil is about 15%, and under single vacuum system, thin-film evaporator inlet amount is larger, generates low molecular vapors more, also just larger to the pressure of vacuum system.Thereby under same operating, the inlet amount of thin-film evaporator and vacuum tightness are class inverse relation, in order to guarantee system vacuum degree, have to reduce de-low inlet amount, make equipment effective rate of utilization low, affect the de-low effect of product simultaneously.Therefore, exploitation is in the urgent need to the efficiently de-low technique of a kind of silicone oil with low viscosity.
Summary of the invention
For addressing the above problem, the invention provides a kind of raising plant factor, improve product yield, reduce energy consumption, reduce the efficiently de-low molecular method of silicone oil with low viscosity of cost of investment.
The technical solution adopted for the present invention to solve the technical problems is: the efficiently de-low molecular method of a kind of silicone oil with low viscosity, by transferpump, silicone oil work in-process are delivered to from silicone oil surge tank in preheater after preheating, enter falling-film evaporator evaporation, then enter conventional vacuum separation system, and in the separator of conventional vacuum separation system, carry out flash trapping stage, liquid after separation enters high vacuum separation system, and in the thin-film evaporator of high vacuum separation system, carry out the second-order separation, silicone oil finished product after separation is from overflow thin-film evaporator bottom, through the cooling product storage tank that enters of supercooler, the low molecule of flash trapping stage and the second-order separation reclaims through condenser.
Be further used as the improvement of technical solution of the present invention, the vacuum tightness of conventional vacuum separation system is-0.095～-0.098Mpa.
Being further used as the improvement of technical solution of the present invention, the vacuum tightness of high vacuum separation system is-more than 0.099Mpa.
Be further used as the improvement of technical solution of the present invention, the preheating temperature of preheater is 100～130 ℃.
Be further used as the improvement of technical solution of the present invention, falling-film evaporator vaporization temperature is 130～170 ℃.
Be further used as the improvement of technical solution of the present invention, separator Heating temperature is 160～180 ℃.
Be further used as the improvement of technical solution of the present invention, thin-film evaporator vaporization temperature is 170～220 ℃.
Beneficial effect of the present invention: the present invention adopts the two-stage separation system that comprises conventional vacuum separation system and high vacuum separation system, in conventional vacuum separation system, remove most of low molecule, high vacuum separation system further removes low molecule, makes product fugitive constituent below 0.2%.Two-stage separation system adopts two kinds of different vacuum systems, guarantees the vacuum tightness of two-stage separation system, guarantees product volatile content, thereby guarantees quality product, makes de-low inlet amount be greatly improved simultaneously, thereby enhances productivity.In addition, in the present invention, silicone oil flows to cold zone by high-temperature zone, and effectively energy efficient, reduces cost of investment.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the invention will be further described:
Fig. 1 is the efficiently de-low molecular system structural representation of silicone oil with low viscosity of the present invention.
Embodiment
As shown in Figure 1, the efficiently de-low molecular system of a kind of silicone oil with low viscosity, comprise successively by the silicone oil surge tank 1 of pipeline conducting, transferpump 2, preheater 3, falling-film evaporator 4, conventional vacuum separation system 5, high vacuum separation system 6, water cooler 7 and product storage tank 8, conventional vacuum separation system 5 comprises that the first low molecule that is located at the separator 51 of 6 of falling-film evaporator 4 and high vacuum separation systems and is derived by separator 51 reclaims branch road, high vacuum separation system 6 comprises that the second low molecule that is located at the thin-film evaporator 61 of 7, separator 51 and water cooler and is derived by thin-film evaporator 61 reclaims branch road.The first low molecule reclaims that branch road comprises and the first low molecule container for storing liquid 52 of separator 51 top conductings and be located at separator 51 and the first condenser 53 of 52 of the first low molecule container for storing liquids.The second low molecule reclaims that branch road comprises and the second low molecule container for storing liquid 62 of thin-film evaporator 61 top conductings and be located at thin-film evaporator 61 and the second condenser 63 of 62 of the second low molecule container for storing liquids.
In conjunction with said system, the invention provides the efficiently de-low molecular method of a kind of silicone oil with low viscosity, by transferpump 2, silicone oil work in-process are delivered to from silicone oil surge tank 1 in preheater 3 after preheating, enter falling-film evaporator 4 evaporations, then enter conventional vacuum separation system 5, and carry out flash trapping stage in the separator 51 of conventional vacuum separation system 5, liquid after separation enters high vacuum separation system 6, and carry out the second-order separation in the thin-film evaporator 61 of high vacuum separation system 6, silicone oil finished product after separation is from overflow thin-film evaporator 61 bottoms, through the cooling product storage tank 8 that enters of supercooler 7, the low molecule of flash trapping stage and the second-order separation reclaims through condenser.The present invention adopts the two-stage separation system that comprises conventional vacuum separation system 5 and high vacuum separation system 6, removes most of low molecule in conventional vacuum separation system 5, and high vacuum separation system 6 further removes low molecule, makes product fugitive constituent below 0.2%.Two-stage separation system adopts two kinds of different vacuum systems, guarantees the vacuum tightness of two-stage separation system, guarantees product volatile content, thereby guarantees quality product, makes de-low inlet amount be greatly improved simultaneously, thereby enhances productivity.In addition, in the present invention, silicone oil flows to cold zone by high-temperature zone, and effectively energy efficient, reduces cost of investment.
Embodiment 1
By transferpump 2, silicone oil work in-process are delivered to from silicone oil surge tank 1 to preheating in preheater 3, controlling preheating temperature is 100 ℃, then enter falling-film evaporator 4 evaporations, controlling vaporization temperature is 130 ℃, then enter separator 51 separation, controlling separator 51 Heating temperatures is 160 ℃, the vacuum tightness of controlling conventional vacuum separation system 5 is-0.095Mpa, liquid after separation enters thin-film evaporator 61 and carries out the second-order separation, the temperature of controlling thin-film evaporator 61 is 170 ℃, the vacuum tightness of controlling high vacuum separation system 6 is-0.099Mpa, silicone oil finished product is from overflow thin-film evaporator 61 bottoms, through the cooling product storage tank 8 that enters of supercooler 7, separated low molecule reclaims branch road through the first low molecule and the second low molecule reclaims branch road recovery.
Embodiment 2
By transferpump 2, silicone oil work in-process are delivered to from silicone oil surge tank 1 to preheating in preheater 3, controlling preheating temperature is 130 ℃, then enter falling-film evaporator 4 evaporations, controlling vaporization temperature is 170 ℃, then enter separator 51 separation, controlling separator 51 Heating temperatures is 180 ℃, the vacuum tightness of controlling conventional vacuum separation system 5 is-0.098Mpa, liquid after separation enters thin-film evaporator 61 and carries out the second-order separation, the temperature of controlling thin-film evaporator 61 is 220 ℃, the vacuum tightness of controlling high vacuum separation system 6 is-0.101Mpa, silicone oil finished product is from overflow thin-film evaporator 61 bottoms, through the cooling product storage tank 8 that enters of supercooler 7, separated low molecule reclaims branch road through the first low molecule and the second low molecule reclaims branch road recovery.
Comparative example
By transferpump 2, silicone oil work in-process are delivered to from silicone oil surge tank 1 to preheating in preheater 3, controlling preheating temperature is 170 ℃, then thin-film evaporator 61, the temperature of controlling thin-film evaporator 61 is 200 ℃, the vacuum tightness of Controlling System is-0.099Mpa, silicone oil finished product is from overflow thin-film evaporator 61 bottoms, and through the cooling product storage tank 8 that enters of supercooler 7, separated low molecule reclaims branch road through the second low molecule and reclaims.
Table 1 embodiment and comparative example result synopsis
Note: product yield, reduction specific consumption and raising charging dose rate are to take comparative example as radix.
Certainly, the invention is not limited to above-mentioned embodiment, those of ordinary skill in the art also can make equivalent variations or replacement under the prerequisite without prejudice to spirit of the present invention, and the modification that these are equal to or replacement are all included in the application's claim limited range.
Claims (7)
1. a silicone oil with low viscosity efficiently takes off low molecular method, it is characterized in that: by transferpump, silicone oil work in-process are delivered to from silicone oil surge tank in preheater after preheating, enter falling-film evaporator evaporation, then enter conventional vacuum separation system, and in the separator of described conventional vacuum separation system, carry out flash trapping stage, liquid after separation enters high vacuum separation system, and in the thin-film evaporator of described high vacuum separation system, carry out the second-order separation, silicone oil finished product after separation is from overflow described thin-film evaporator bottom, through the cooling product storage tank that enters of supercooler, the low molecule of flash trapping stage and the second-order separation reclaims through condenser.
2. the efficiently de-low molecular method of silicone oil with low viscosity according to claim 1, is characterized in that: the vacuum tightness of described conventional vacuum separation system is-0.095～-0.098Mpa.
3. the efficiently de-low molecular method of silicone oil with low viscosity according to claim 1 and 2, is characterized in that: the vacuum tightness of described high vacuum separation system for-more than 0.099Mpa.
4. the efficiently de-low molecular method of silicone oil with low viscosity according to claim 3, is characterized in that: the preheating temperature of described preheater is 100～130 ℃.
5. the efficiently de-low molecular method of silicone oil with low viscosity according to claim 3, is characterized in that: described falling-film evaporator vaporization temperature is 130～170 ℃.
6. the efficiently de-low molecular method of silicone oil with low viscosity according to claim 3, is characterized in that: described separator Heating temperature is 160～180 ℃.
7. the efficiently de-low molecular method of silicone oil with low viscosity according to claim 3, is characterized in that: described thin-film evaporator vaporization temperature is 170～220 ℃.
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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 |
| CN108102100A (en) * | 2017-12-27 | 2018-06-01 | 浙江福斯特新材料研究院有限公司 | A kind of production method and production system of low volatilization vinyl silicone oil |
| CN111454453A (en) * | 2020-04-27 | 2020-07-28 | 辽宁新邦新材料有限公司 | Production process for preparing room temperature vulcanized phenyl silicone rubber crude rubber |
| CN114015052A (en) * | 2021-11-03 | 2022-02-08 | 佛山市金银河智能装备股份有限公司 | Silicon oil low-removing process method |
| CN114213663A (en) * | 2021-12-30 | 2022-03-22 | 杭州崇耀科技发展有限公司 | Acrylate modified silicone oil and preparation method thereof |
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| EP0183793B1 (en) * | 1984-05-24 | 1989-04-12 | Chen-Yen Cheng | Wet and dry distillative freezing process for separating mixtures and apparatuses for use therein |
| CN102206349A (en) * | 2011-04-23 | 2011-10-05 | 茂名市信翼化工有限公司 | Method for purifying alpha,omega-dihydroxy-polydimethylsiloxane |
| CN102206348A (en) * | 2011-01-19 | 2011-10-05 | 颜建平 | Secondary flash evaporation low molecular weight removing process and equipment |
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2013
- 2013-11-21 CN CN201310594477.2A patent/CN103642045B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| EP0183793B1 (en) * | 1984-05-24 | 1989-04-12 | Chen-Yen Cheng | Wet and dry distillative freezing process for separating mixtures and apparatuses for use therein |
| CN102206348A (en) * | 2011-01-19 | 2011-10-05 | 颜建平 | Secondary flash evaporation low molecular weight removing process and equipment |
| CN102206349A (en) * | 2011-04-23 | 2011-10-05 | 茂名市信翼化工有限公司 | Method for purifying alpha,omega-dihydroxy-polydimethylsiloxane |
Cited By (7)
| 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 |
| CN108102100A (en) * | 2017-12-27 | 2018-06-01 | 浙江福斯特新材料研究院有限公司 | A kind of production method and production system of low volatilization vinyl silicone oil |
| CN108102100B (en) * | 2017-12-27 | 2020-11-10 | 浙江福斯特新材料研究院有限公司 | Production method and production system of low-volatility vinyl silicone oil |
| CN111454453A (en) * | 2020-04-27 | 2020-07-28 | 辽宁新邦新材料有限公司 | Production process for preparing room temperature vulcanized phenyl silicone rubber crude rubber |
| CN114015052A (en) * | 2021-11-03 | 2022-02-08 | 佛山市金银河智能装备股份有限公司 | Silicon oil low-removing process method |
| CN114213663A (en) * | 2021-12-30 | 2022-03-22 | 杭州崇耀科技发展有限公司 | Acrylate modified silicone oil and preparation method thereof |
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Effective date of registration: 20160315 Address after: 510663 901A, four street, 10 science Avenue, Guangzhou, Guangdong, Luogang District Applicant after: GUANGZHOU DAOLIN SYNTHETIC MATERIAL CO., LTD. Applicant after: YICHANG KELIN SILICON MATERIALS CO., LTD. Address before: Industrial Park in Hubei province Yichang city 443711 Xiakou town of Xingshan County Applicant before: YICHANG KELIN SILICON MATERIALS CO., LTD. |
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Effective date of registration: 20190920 Address after: 443700 Economic Development Zone of Xingshan County, Yichang City, Hubei Province Patentee after: YICHANG KELIN SILICON MATERIALS CO., LTD. Address before: 510663 901A, four street, 10 science Avenue, Guangzhou, Guangdong, Luogang District Co-patentee before: YICHANG KELIN SILICON MATERIALS CO., LTD. Patentee before: GUANGZHOU DAOLIN SYNTHETIC MATERIAL CO., LTD. |
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