CN103642045B - A kind of Efficient low molecule removal method for low viscosity silicone - Google Patents
A kind of Efficient low molecule removal method for low viscosity silicone Download PDFInfo
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- CN103642045B CN103642045B CN201310594477.2A CN201310594477A CN103642045B CN 103642045 B CN103642045 B CN 103642045B CN 201310594477 A CN201310594477 A CN 201310594477A CN 103642045 B CN103642045 B CN 103642045B
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Abstract
The invention discloses a kind of Efficient low molecule removal method for low viscosity silicone, low field is taken off for silicone oil, the present invention adopts the two-stage separation system comprising conventional vacuum separation system and high vacuum separation system, most of low molecule is removed in conventional vacuum separation system, high vacuum separation system removes low molecule further, makes product fugitive constituent below 0.2%.Two-stage separation system adopts two kinds of different vacuum systems, ensures the vacuum tightness of two-stage separation system, ensures product volatile content, thus ensures quality product, makes de-low inlet amount be greatly improved simultaneously, thus enhances productivity.In addition, in the present invention, silicone oil flows to cold zone by high-temperature zone, effective energy efficient, reduces cost of investment.
Description
Technical field
The present invention is used for silicone oil and takes off low field, particularly relates to a kind of Efficient low molecule removal method for low viscosity silicone.
Background technology
It is by volatile matter that silicone oil takes off low molecule, as ring body forwards gas phase to from liquid phase, and the process be separated.The feed composition of silicone oil is more, and its de-low molecule operation is more complicated.Along with standard of living improves constantly, the specification of quality of people to commodity improves constantly, and a lot of client requires that silicone oil product fugitive constituent is less than 0.5%, some high-end field now, as aerospace field, field of medicaments etc. require higher to silicone oil fugitive constituent.In silicone oil production process, the energy that de-low molecule 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 current silicone oil with low viscosity has two kinds of modes, and one is intermittent type: after silicone oil and end-capping reagent synthesize silicone oil under catalyst action, directly at reduced pressure conditions in reactor, removes low molecule.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, and take the product of this de-low mode, its fugitive constituent can only remain on about 1%; Two is continous ways: preheater is connected one or more thin-film evaporator, under same vacuum system, remove low molecule.Because silicone oil with low viscosity viscosity is less, be difficult to form liquid film in thin-film evaporator, adopt single thin-film evaporator, make equipment effectiveness low, and product volatile content can not be ensured, be not suitable for silicone oil with low viscosity and remove low molecule; Adopt the parallel connection of multiple thin-film evaporator or be together in series, although can to a certain degree ensure product volatile content, its equipment investment cost is high, energy consumption is large.
The half-finished low molecule content of general silicone oil is about 15%, and under single vacuum system, thin-film evaporator inlet amount is larger, then generate low molecule steam more, also larger to the pressure of vacuum system.Thus, under same operating, the inlet amount of thin-film evaporator and vacuum tightness are class inverse relation, in order to ensure system vacuum, having to reduce de-low inlet amount, making equipment effective rate of utilization low, affect product simultaneously and take off low effect.Therefore, develop in the urgent need to the efficiently de-low technique of a kind of silicone oil with low viscosity.
Summary of the invention
For solving the problem, the invention provides a kind of raising plant factor, improving product yield, reduce energy consumption, reduce the Efficient low molecule removal method for low viscosity silicone of cost of investment.
The technical solution adopted for the present invention to solve the technical problems is: a kind of Efficient low molecule removal method for low viscosity silicone, silicone oil work in-process to be delivered to from silicone oil surge tank in preheater after preheating by transferpump, enter falling-film evaporator evaporation, then conventional vacuum separation system is entered, and flash trapping stage is carried out in the separator of conventional vacuum separation system, liquid after separation enters high vacuum separation system, and the second-order separation is carried out in the thin-film evaporator of high vacuum separation system, after silicone oil finished product after separation overflows bottom thin-film evaporator, product storage tank is entered through supercooler cooling, 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.
Be 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 DEG C.
Be further used as the improvement of technical solution of the present invention, falling-film evaporator vaporization temperature is 130 ~ 170 DEG C.
Be further used as the improvement of technical solution of the present invention, separator Heating temperature is 160 ~ 180 DEG C.
Be further used as the improvement of technical solution of the present invention, thin-film evaporator vaporization temperature is 170 ~ 220 DEG C.
Beneficial effect of the present invention: the present invention adopts the two-stage separation system comprising conventional vacuum separation system and high vacuum separation system, most of low molecule is removed in conventional vacuum separation system, high vacuum separation system removes low molecule further, makes product fugitive constituent below 0.2%.Two-stage separation system adopts two kinds of different vacuum systems, ensures the vacuum tightness of two-stage separation system, ensures product volatile content, thus ensures quality product, makes de-low inlet amount be greatly improved simultaneously, thus enhances productivity.In addition, in the present invention, silicone oil flows to cold zone by high-temperature zone, effective 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 molecule system architecture schematic diagram of silicone oil with low viscosity of the present invention.
Embodiment
As shown in Figure 1, the efficiently de-low molecule 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 the separator 51 be located between falling-film evaporator 4 and high vacuum separation system 6 and first low molecule of being derived by separator 51 reclaims branch road, high vacuum separation system 6 comprises the thin-film evaporator 61 be located between separator 51 and water cooler 7 and second low molecule of being derived by thin-film evaporator 61 reclaims branch road.First low molecule reclaims branch road and comprises and the first low molecule container for storing liquid 52 of separator 51 top conducting and the first condenser 53 of being located between separator 51 and the first low molecule container for storing liquid 52.Second low molecule reclaims branch road and comprises and the second low molecule container for storing liquid 62 of thin-film evaporator 61 top conducting and the second condenser 63 of being located between thin-film evaporator 61 and the second low molecule container for storing liquid 62.
A kind of Efficient low molecule removal method for low viscosity silicone is the invention provides in conjunction with said system, silicone oil work in-process to be delivered to from silicone oil surge tank 1 in preheater 3 after preheating by transferpump 2, enter falling-film evaporator 4 to evaporate, then conventional vacuum separation system 5 is entered, and flash trapping stage is carried out in the separator 51 of conventional vacuum separation system 5, liquid after separation enters high vacuum separation system 6, and the second-order separation is carried out in the thin-film evaporator 61 of high vacuum separation system 6, after silicone oil finished product after separation overflows bottom thin-film evaporator 61, product storage tank 8 is entered through supercooler 7 cooling, the low molecule of flash trapping stage and the second-order separation reclaims through condenser.The present invention adopts the two-stage separation system comprising conventional vacuum separation system 5 and high vacuum separation system 6, and in conventional vacuum separation system 5, remove most of low molecule, high vacuum separation system 6 removes low molecule further, makes product fugitive constituent below 0.2%.Two-stage separation system adopts two kinds of different vacuum systems, ensures the vacuum tightness of two-stage separation system, ensures product volatile content, thus ensures quality product, makes de-low inlet amount be greatly improved simultaneously, thus enhances productivity.In addition, in the present invention, silicone oil flows to cold zone by high-temperature zone, effective energy efficient, reduces cost of investment.
Embodiment 1
By transferpump 2, silicone oil work in-process are delivered to preheating in preheater 3 from silicone oil surge tank 1, controlling preheating temperature is 100 DEG C, then enter falling-film evaporator 4 to evaporate, controlling vaporization temperature is 130 DEG C, then enter separator 51 to be separated, controlling separator 51 Heating temperature is 160 DEG C, the vacuum tightness 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 controlling thin-film evaporator 61 is 170 DEG C, the vacuum tightness controlling high vacuum separation system 6 is-0.099Mpa, after silicone oil finished product overflows bottom thin-film evaporator 61, product storage tank 8 is entered through supercooler 7 cooling, the low molecule be separated reclaims branch road and the recovery of the second low molecule recovery branch road through the first low molecule.
Embodiment 2
By transferpump 2, silicone oil work in-process are delivered to preheating in preheater 3 from silicone oil surge tank 1, controlling preheating temperature is 130 DEG C, then enter falling-film evaporator 4 to evaporate, controlling vaporization temperature is 170 DEG C, then enter separator 51 to be separated, controlling separator 51 Heating temperature is 180 DEG C, the vacuum tightness 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 controlling thin-film evaporator 61 is 220 DEG C, the vacuum tightness controlling high vacuum separation system 6 is-0.101Mpa, after silicone oil finished product overflows bottom thin-film evaporator 61, product storage tank 8 is entered through supercooler 7 cooling, the low molecule be separated reclaims branch road and the recovery of the second low molecule recovery branch road through the first low molecule.
Comparative example
By transferpump 2, silicone oil work in-process are delivered to preheating in preheater 3 from silicone oil surge tank 1, controlling preheating temperature is 170 DEG C, then thin-film evaporator 61, the temperature controlling thin-film evaporator 61 is 200 DEG C, the vacuum tightness of Controlling System is-0.099Mpa, after silicone oil finished product overflows bottom thin-film evaporator 61, enter product storage tank 8 through supercooler 7 cooling, the low molecule of separation 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 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 these equivalent modification or replacement are all included in the application's claim limited range.
Claims (7)
1. an Efficient low molecule removal method for low viscosity silicone, it is characterized in that: silicone oil work in-process to be delivered to from silicone oil surge tank in preheater after preheating by transferpump, enter falling-film evaporator evaporation, then conventional vacuum separation system is entered, and flash trapping stage is carried out in the separator of described conventional vacuum separation system, liquid after separation enters high vacuum separation system, and the second-order separation is carried out in the thin-film evaporator of described high vacuum separation system, after silicone oil finished product after separation overflows bottom described thin-film evaporator, product storage tank is entered through supercooler cooling, the low molecule of flash trapping stage and the second-order separation reclaims through condenser.
2. Efficient low molecule removal method for low viscosity silicone according to claim 1, is characterized in that: the vacuum tightness of described conventional vacuum separation system is-0.095 ~-0.098Mpa.
3. Efficient low molecule removal method for low viscosity silicone according to claim 1 and 2, is characterized in that: the vacuum tightness of described high vacuum separation system is more than-0.099Mpa.
4. Efficient low molecule removal method for low viscosity silicone according to claim 3, is characterized in that: the preheating temperature of described preheater is 100 ~ 130 DEG C.
5. Efficient low molecule removal method for low viscosity silicone according to claim 3, is characterized in that: described falling-film evaporator vaporization temperature is 130 ~ 170 DEG C.
6. Efficient low molecule removal method for low viscosity silicone according to claim 3, is characterized in that: described separator Heating temperature is 160 ~ 180 DEG C.
7. Efficient low molecule removal method for low viscosity silicone according to claim 3, is characterized in that: described thin-film evaporator vaporization temperature is 170 ~ 220 DEG C.
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| 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 |
| 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 |
| CN114015052B (en) * | 2021-11-03 | 2023-05-23 | 佛山市金银河智能装备股份有限公司 | Silicone oil stripping process |
| CN114213663B (en) * | 2021-12-30 | 2022-11-01 | 杭州崇耀科技发展有限公司 | Acrylate modified silicone oil and preparation method thereof |
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 |
| 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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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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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. |