CN102140170B - Preparation process of high-molecular-weight permethyl silicone oil - Google Patents
Preparation process of high-molecular-weight permethyl silicone oil Download PDFInfo
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Abstract
The invention relates to a preparation process of high-molecular-weight permethyl silicone oil. In the preparation process, a new formula is adopted, a composite catalyst is added, the product yield is high, high-molecular-weight product is obtained, and the molecular weight of the produced high-molecular-weight polydimethylsiloxane reaches 550,000 to 700,000 and has higher heat resistance, oxidization resistance, low-temperature resistance and shearing resistance than vinylsiloxane rubber. The high-molecular-weight permethyl silicone oil comprises the following chemical raw materials in part by mass: 10.2 parts of dimethyl cyclosiloxane (DMC) and 2.3 parts of polydimethylsiloxane; and a composite catalyst comprises 0.0263 part of tetramethylammonium hydroxide and 0.0025 part of hexamethylcyclotrisiloxane. The preparation process has the advantages that: the molecular weight and yield of the product are high; the loss in a low-boiling-point material removal process is small; the heat resistance, oxidization resistance, low-temperature resistance and shearing resistance are high; and the device is reasonable and compact, operates stably and can produce continuously.
Description
Technical field
The present invention relates to a kind of novel silicon oil technical field, the novel process of the full methyl-silicone oil of especially a kind of HMW.
Background technology
Generally the molecular weight of used dimethyl siloxane is the highest on the market generally has only 200,000; The present invention relates to the preparation of the full methyl-silicone oil of a kind of novel high polymer amount; Because of the polyreaction in its preparation technology's link has added composite catalyst: tetramethyl-oxyammonia and hexamethyl cyclotrisiloxane; Can make the molecular weight of YSR 3286 of the present invention reach 55-70 ten thousand, it is stronger to have better heat-resisting, antioxidant, lower temperature resistance and a shear resistant than vinylsiloxane rubber.
Summary of the invention
The object of the present invention is to provide the preparation technology of the full methyl-silicone oil of a kind of HMW.
The difficult problem that the present invention solves is that original methyl vinyl silicone rubber is converted to the full methyl-silicone oil of HMW and satisfies the client for high-molecular weight silicone oil demand.The present invention has changed new prescription; The composite catalyst that has added tetramethyl-oxyammonia and hexamethyl cyclotrisiloxane; The excellent results that can obtain is: the high yield of the HMW of product, product, take off that low operation loss amount is little, thermotolerance is high, antioxidant is good, lower temperature resistance is strong and shear resistant is stronger, the reasonable compactness of device; Stable, but continuous production.
The full methyl-silicone oil of the HMW that the present invention relates to, comprise the industrial chemicals of following quality proportioning: 100 parts of dimethyl silica alkylating mixtures (DMC), YSR 3286 are 23 parts; The amount of its composite catalyst is respectively: 0.26 part of tetramethyl-oxyammonia, 0.025 part of hexamethyl cyclotrisiloxane;
Wherein: be hexamethyl cyclotrisiloxane dimethyl silica alkylating mixture (DMC)), octamethylcyclotetrasiloxane, decamethylcyclopentaandoxane, ten diformazan basic rings, six siloxanes, any one in the tetradecamethylcycloheptasiloxane or several.
Technical scheme of the present invention is:
The preparation technology of the full methyl-silicone oil of HMW, processed by the industrial chemicals of following quality proportioning: 100 parts of dimethyl silica alkylating mixtures (DMC), YSR 3286 are 23 parts; The amount of its composite catalyst is respectively: 0.26 part of tetramethyl-oxyammonia, 0.025 part of hexamethyl cyclotrisiloxane;
Wherein: dimethyl silica alkylating mixture (DMC) is a hexamethyl cyclotrisiloxane, octamethylcyclotetrasiloxane, decamethylcyclopentaandoxane, ten diformazan basic rings, six siloxanes, any one in the tetradecamethylcycloheptasiloxane or several;
Wherein technical process: get the raw materials ready, filter, binder is switched in dehydration, polymerization, and the matchmaker is broken in slaking, takes off low discharging; Specific as follows:
1. get the raw materials ready
The open vacuum pump cuts out the scale tank blow-off valve, slowly opens the scale tank vacuum valve, makes to form vacuum in the scale tank, opens the feed valve of material-pumping tube then, in qualified dimethyl silica alkylating mixture (DMC) suction raw material test tank.When treating that raw material reaches the scale tank calibration value, close the scale tank vacuum valve, open blow-off valve, at this moment, unnecessary material will return in the bucket through syphonic effect.The raw material and the small amount of moisture that do not exhaust at the bottom of the Raw material pail to be got in the settling bath, re-used after making the moisture content sedimentation.
2. filter
Remove mechanical impurity and the moisture content in the material in the material.
3. dehydration
After filtering completion, close dehydration still feed valve,, vacuumize and use N in steam heating
2Dewater under the condition of bubbling.The dehydration normal discharge must ensure that certain effluent is arranged on the groove visor, simultaneously liquid with even trickling for well.
4. binder is prepared burden polymerization
4.1 when dehydration finishes, close dehydration groove vacuum valve, open blow-off valve, continue material in the still is heated to 103 ℃, the binder temperature is controlled at 105 ℃.Before the polymeric kettle charging, its system's thermal oil temperature must reach 170 ℃.
4.2 switch binder
4.2.1 the N of two reaction kettles
2After the balance, close original reactor discharging dish valve, open another reaction kettle bleeder valve, open reaction kettle groove vacuum valve, often open reaction kettle stirrer cooling water valve, water temperature＜40 ℃.Open empty reaction kettle mixer motor, and the casual position of being transferred to 50r/n slowly.When hearing that emptying finishes, then open dehydration still bleeder valve.
4.2.2 at first open N
2The bubbling valve carries out nitrogen equilibrium again, opens two reaction kettle N
2Feed valve is turned off when the both sides pointer is motionless.Empty still carries out emptying, after emptying is intact, opens vacuum valve and vacuumizes, and waits to be extracted into-close vacuum during 0.098MPa, opens the material feed valve and begins charging, 105 ℃ of material temperature.During binder, dehydration still pressure remains on about 0. 1MPa, must not be higher than 0.2MPa, batching, and polymerization when binder finishes, is closed dehydration still feed valve.When (2) binder finishes, close feed valve, prepare to add alkali glue then and carry out polyreaction.Temperature of charge maintains about 105 ℃.With dilution material dilution alkali glue, rock plastic tank, make alkali glue even, from suction pipe, add in the reaction kettle then.When adding alkali glue, viscosity fast rise in the still will suitably be used N
2Advertise.Use N Deng adding continued
2Tympanites blows, so that alkali glue is evenly distributed.Again vacuum tightness is extracted into-closes during 0.098MPa vacuum valve, stir, continue reaction.
4.3 polyreaction
When input dimethyl silica alkylating mixture (DMC) and YSR 3286 carry out polyreaction in reaction kettle; Add composite catalyst; The entire reaction time was controlled at 3 hours, and in first hour of entire reaction, the temperature of reaction of polymeric kettle is controlled at 108 ℃; The temperature of reaction of polymeric kettle is controlled at 115 ℃ in two hours after entire reaction, and the heating steam pressure of polymeric kettle is controlled at 0.2MPa.
5. slaking, broken matchmaker, take off low
After the polyreaction reaction is accomplished, switch, material in reactor is used N through the dish valve
2Be pressed into and carry out slaking in the slaking tube, N in the still
2Pressure-controlling is at 0.40MPa; The heating steam of slaking tube is opened, control its vapor pressure, make temperature of charge maintain 125 ℃ at 0.35MPa; After treating that material entering oil adds the hot tearing pipe; Catalyzer decomposes under 150 ℃ of high temperature, loses activity, and material removes low molecular impurity by flash distillation in taking off low device when card is dispersed into filament.
After material takes off and hangs down, fall into and take off low device feed basin, see packing through spiral discharging machine off through the water cooler material again.
Taking off when low, the thermal oil temperature of electrically heated case is controlled at 173 ℃, takes off low molecule device card temperature upper strata and is controlled at 161 ℃, and card temperature lower floor is controlled at 164 ℃; Take off low device top pressure and be controlled at 0.0025 MPa, the card pressure-controlling is at 0.20 MPa, and the vapor pressure control pressure table displayed value that takes off low molecule device heating is 0.58MPa; After material takes off and hangs down, fall into and take off low device feed basin, see packing through spiral discharging machine off through the water cooler material again.
6. discharging, packing
When taking off, material runs up to 1/2 in the low device basin when above, the discharging of unlatching spiral discharging machine.Whether be water white transparency do not have mechanical impurity, will in time handle in case pinpoint the problems if will often observe the material outward appearance during discharging.When filling with substance also will be noted avoiding impurity to sneak into.To pave wholely at the bottom of the plastics bag, wear at the end to prevent to melt.
The present invention relates to the preparation of the full methyl-silicone oil of a kind of novel high polymer amount; Because of the polyreaction in its preparation technology's link has added composite catalyst: tetramethyl-oxyammonia and hexamethyl cyclotrisiloxane; Can make the molecular weight of YSR 3286 of the present invention reach 55-70 ten thousand, it is stronger to have better heat-resisting, antioxidant, lower temperature resistance and a shear resistant than vinylsiloxane rubber.
The viscosity of the YSR 3286 that the present invention relates to is that 5000-8000S is proper.In general the extensive 5S-250000S of the viscosity profile of YSR 3286.
Embodiment
The preparation technology of embodiment 1, the full methyl-silicone oil of HMW, processed by the industrial chemicals of following quality proportioning: 100 parts of dimethyl silica alkylating mixtures (DMC), YSR 3286 are 23 parts; The amount of its composite catalyst is respectively: 0.26 part of tetramethyl-oxyammonia, 0.025 part of hexamethyl cyclotrisiloxane;
Dimethyl silica alkylating mixture (DMC) wherein is 5 parts of hexamethyl cyclotrisiloxanes, 30 parts of octamethylcyclotetrasiloxanes, 60 parts of decamethylcyclopentaandoxane, 4 parts of ten diformazan basic rings, six siloxanes, the mixture that tetradecamethylcycloheptasiloxane is 1 part;
Wherein technical process: get the raw materials ready, filter, binder is switched in dehydration, polymerization, and the matchmaker is broken in slaking, takes off low discharging; Specific as follows:
1. get the raw materials ready
The open vacuum pump cuts out the scale tank blow-off valve, slowly opens the scale tank vacuum valve, makes to form vacuum in the scale tank, opens the feed valve of material-pumping tube then, in qualified dimethyl silica alkylating mixture (DMC) suction raw material test tank.When treating that raw material reaches the scale tank calibration value, close the scale tank vacuum valve, open blow-off valve, at this moment, unnecessary material will return in the bucket through syphonic effect.The raw material and the small amount of moisture that do not exhaust at the bottom of the Raw material pail to be got in the settling bath, re-used after making the moisture content sedimentation.
2. filter
Remove mechanical impurity and the moisture content in the material in the material.
3. dehydration
After filtering completion, close dehydration still feed valve,, vacuumize and use N in steam heating
2Dewater under the condition of bubbling.The dehydration normal discharge must ensure that certain effluent is arranged on the groove visor, simultaneously liquid with even trickling for well.
4. binder is prepared burden polymerization
4.1 when dehydration finishes, close dehydration groove vacuum valve, open blow-off valve, continue material in the still is heated to 103 ℃, the binder temperature is controlled at 105 ℃.Before the polymeric kettle charging, its system's thermal oil temperature must reach 170 ℃.
4.2 switch binder
4.2.1 the N of two reaction kettles
2After the balance, close original reactor discharging dish valve, open another reaction kettle bleeder valve, open reaction kettle groove vacuum valve, often open reaction kettle stirrer cooling water valve, water temperature＜40 ℃.Open empty reaction kettle mixer motor, and the casual position of being transferred to 50r/n slowly.When hearing that emptying finishes, then open dehydration still bleeder valve.
4.2.2 at first open N
2The bubbling valve carries out nitrogen equilibrium again, opens two reaction kettle N
2Feed valve is turned off when the both sides pointer is motionless.Empty still carries out emptying, after emptying is intact, opens vacuum valve and vacuumizes, and waits to be extracted into-close vacuum during 0.098MPa, opens the material feed valve and begins charging, 105 ℃ of material temperature.During binder, dehydration still pressure remains on about 0. 1MPa, must not be higher than 0.2MPa, batching, and polymerization when binder finishes, is closed dehydration still feed valve.When (2) binder finishes, close feed valve, prepare to add alkali glue then and carry out polyreaction.Temperature of charge maintains about 105 ℃.With dilution material dilution alkali glue, rock plastic tank, make alkali glue even, from suction pipe, add in the reaction kettle then.When adding alkali glue, viscosity fast rise in the still will suitably be used N
2Advertise.Use N Deng adding continued
2Tympanites blows, so that alkali glue is evenly distributed.Again vacuum tightness is extracted into-closes during 0.098MPa vacuum valve, stir, continue reaction.
4.3 polyreaction
When input dimethyl silica alkylating mixture (DMC) and YSR 3286 carry out polyreaction in reaction kettle; Add composite catalyst; The entire reaction time was controlled at 3 hours, and in first hour of entire reaction, the temperature of reaction of polymeric kettle is controlled at 108 ℃; The temperature of reaction of polymeric kettle is controlled at 115 ℃ in two hours after entire reaction, and the heating steam pressure of polymeric kettle is controlled at 0.2MPa.
5. slaking, broken matchmaker, take off low
After the polyreaction reaction is accomplished, switch, material in reactor is used N through the dish valve
2Be pressed into and carry out slaking in the slaking tube, N in the still
2Pressure-controlling is at 0.40MPa; The heating steam of slaking tube is opened, control its vapor pressure, make temperature of charge maintain 125 ℃ at 0.35MPa; After treating that material entering oil adds the hot tearing pipe; Catalyzer decomposes under 150 ℃ of high temperature, loses activity, and material removes low molecular impurity by flash distillation in taking off low device when card is dispersed into filament.
After material takes off and hangs down, fall into and take off low device feed basin, see packing through spiral discharging machine off through the water cooler material again.
Taking off when low, the thermal oil temperature of electrically heated case is controlled at 173 ℃, takes off low molecule device card temperature upper strata and is controlled at 161 ℃, and card temperature lower floor is controlled at 164 ℃; Take off low device top pressure and be controlled at 0.0025 MPa, the card pressure-controlling is at 0.20 MPa, and the vapor pressure control pressure table displayed value that takes off low molecule device heating is 0.58MPa; After material takes off and hangs down, fall into and take off low device feed basin, see packing through spiral discharging machine off through the water cooler material again.
6. discharging, packing
When taking off, material runs up to 1/2 in the low device basin when above, the discharging of unlatching spiral discharging machine.Whether be water white transparency do not have mechanical impurity, will in time handle in case pinpoint the problems if will often observe the material outward appearance during discharging.When filling with substance also will be noted avoiding impurity to sneak into.To pave wholely at the bottom of the plastics bag, wear at the end to prevent to melt.
Embodiment 2, the full methyl-silicone oil of HMW, comprise the industrial chemicals of following quality proportioning: 100 parts of dimethyl silica alkylating mixtures (DMC), YSR 3286 are 25 parts; The amount of its composite catalyst is respectively: 0.263 part of tetramethyl-oxyammonia, 0.025 part of hexamethyl cyclotrisiloxane;
All the other are with embodiment 1.
Embodiment 3, the full methyl-silicone oil of HMW, comprise the industrial chemicals of following quality proportioning: 100 parts of dimethyl silica alkylating mixtures (DMC), YSR 3286 are 28 parts; The amount of its composite catalyst is respectively: 0.263 part of tetramethyl-oxyammonia, 0.025 part of hexamethyl cyclotrisiloxane;
All the other are with embodiment 1.
Embodiment 4, the full methyl-silicone oil of HMW, comprise the industrial chemicals of following quality proportioning: 100 parts of dimethyl silica alkylating mixtures (DMC), YSR 3286 are 23 parts; The amount of its composite catalyst is respectively: 0.263 part of tetramethyl-oxyammonia, 0.025 part of hexamethyl cyclotrisiloxane.
Taking off when low, the thermal oil temperature of electrically heated case is controlled at 180 ℃, takes off low molecule device card temperature upper strata and is controlled at 165 ℃, and card temperature lower floor is controlled at 167 ℃.Take off low device top pressure and be controlled at 0.28MPa, the card pressure-controlling is at 0.22 Mpa, and the vapor pressure that takes off low molecule device heating is controlled at 0.59Mpa;
Wherein: dimethyl silica alkylating mixture (DMC) is a hexamethyl cyclotrisiloxane, octamethylcyclotetrasiloxane, decamethylcyclopentaandoxane, ten diformazan basic rings, six siloxanes, any one in the tetradecamethylcycloheptasiloxane or several; All the other technical process are with embodiment 1.
Embodiment 5, the full methyl-silicone oil of HMW, comprise the industrial chemicals of following quality proportioning: 100 parts of dimethyl silica alkylating mixtures (DMC), YSR 3286 are 23 parts; The amount of its composite catalyst is respectively: 0.263 part of tetramethyl-oxyammonia, 0.025 part of hexamethyl cyclotrisiloxane;
Taking off when low, the thermal oil temperature of electrically heated case is controlled at 170 ℃, takes off low molecule device card temperature upper strata and is controlled at 158 ℃, and card temperature lower floor is controlled at 155 ℃.Take off low device top pressure and be controlled at 0.22MPa, the card pressure-controlling is at 0.18MPa.The vapor pressure that takes off low molecule device heating is controlled at 0.52Mpa;
Wherein: dimethyl silica alkylating mixture (DMC) is a hexamethyl cyclotrisiloxane, octamethylcyclotetrasiloxane, decamethylcyclopentaandoxane, ten diformazan basic rings, six siloxanes, any one in the tetradecamethylcycloheptasiloxane or several; All the other technical process are with embodiment 1.
Embodiment 6, the full methyl-silicone oil of HMW, comprise the industrial chemicals of following quality proportioning: 100 parts of dimethyl silica alkylating mixtures (DMC), YSR 3286 are 23 parts; The amount of its composite catalyst is respectively: 0.263 part of tetramethyl-oxyammonia, 0.025 part of hexamethyl cyclotrisiloxane;
Taking off when low, the thermal oil temperature of electrically heated case is controlled at 160 ℃, takes off low molecule device card temperature upper strata and is controlled at 152 ℃, and card temperature lower floor is controlled at 155 ℃.Take off low device top pressure and be controlled at 0.22MPa, the card pressure-controlling is at 0.18MPa.The vapor pressure that takes off low molecule device heating is controlled at 0.52Mpa;
Wherein: dimethyl silica alkylating mixture (DMC) is a hexamethyl cyclotrisiloxane, octamethylcyclotetrasiloxane, decamethylcyclopentaandoxane, ten diformazan basic rings, six siloxanes, any one in the tetradecamethylcycloheptasiloxane or several; All the other technical process are with embodiment 1.
Embodiment 7, the full methyl-silicone oil of HMW comprise the industrial chemicals of following quality proportioning: 100 parts of dimethyl silica alkylating mixtures (DMC), 2 parts of vinyl ring bodies, 1 part of vinyl silicone oil;
Wherein: dimethyl silica alkylating mixture (DMC) is a hexamethyl cyclotrisiloxane, octamethylcyclotetrasiloxane, decamethylcyclopentaandoxane, ten diformazan basic rings, six siloxanes, any one in the tetradecamethylcycloheptasiloxane or several;
The common process production of vinylsiloxane rubber is pressed in its technical process.
Embodiment 8, the full methyl-silicone oil of HMW; Wherein: dimethyl silica alkylating mixture (DMC) is 5 parts of hexamethyl cyclotrisiloxanes, 30 parts of octamethylcyclotetrasiloxanes, 60 parts of decamethylcyclopentaandoxane; 4 parts of ten diformazan basic rings, six siloxanes, 1 part of tetradecamethylcycloheptasiloxane.All the other are with embodiment 1.
Embodiment 9, the full methyl-silicone oil of HMW; Wherein: dimethyl silica alkylating mixture (DMC) is 3 parts of hexamethyl cyclotrisiloxanes, 80 parts of octamethylcyclotetrasiloxanes, 15 parts of decamethylcyclopentaandoxane; 2 parts of ten diformazan basic rings, six siloxanes, 0 part of tetradecamethylcycloheptasiloxane.All the other are with embodiment 2.
Embodiment 10, the full methyl-silicone oil of HMW, wherein: dimethyl silica alkylating mixture (DMC) is 100 parts of octamethylcyclotetrasiloxanes.All the other are with embodiment 3.
Embodiment 11, the full methyl-silicone oil of HMW; Wherein: dimethyl silica alkylating mixture (DMC) is 0 part of a hexamethyl cyclotrisiloxane, 5 parts of octamethylcyclotetrasiloxanes, 30 parts of decamethylcyclopentaandoxane; 60 parts of ten diformazan basic rings, six siloxanes, 5 parts of tetradecamethylcycloheptasiloxanes.All the other are with embodiment 4.
Embodiment 12, the full methyl-silicone oil of HMW, wherein: dimethyl silica alkylating mixture (DMC) is 100 parts of tetradecamethylcycloheptasiloxanes.All the other are with embodiment 3.
Embodiment 13, the full methyl-silicone oil of HMW, wherein: YSR 3286 adopts viscosity: 5000-8000S the most suitable.All the other are with above-mentioned each embodiment.
Test Example 1
Test materials: will be divided into six groups of A, B, C, D, E, F by the Zylox that embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5, embodiment 6 make.
(1) relatively obtains the molecular weight of product
Test Example 2
Test materials: will be divided into six groups of A, B, C, D, E, F by the Zylox that embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5, embodiment 6 make; Other is provided with blank group the 7th component, and wherein the 7th group of sample that provides made by embodiment 1.
TP
(2) high-and low-temperature resistance test
To make Zylox by the foregoing description and all heat 30min, take out with the baking oven of putting into 280 ℃, observe phenomena, other is provided with blank group the 7th component, and wherein the 7th group of sample that provides made by embodiment 1.To make Zylox by the foregoing description in addition then and put into-100 ℃ refrigerator, refrigeration 30min takes out, observe phenomena, and other is provided with blank group the 7th component, and wherein the 7th group of sample that provides made by embodiment 1.
Test Example 3
Test materials: will be divided into six groups of A, B, C, D, E, F by the Zylox that embodiment 1, embodiment 2, embodiment 3, embodiment 4, embodiment 5, embodiment 6 make; Other is provided with blank group the 7th component, and wherein the 7th group of sample that provides made by embodiment 1.
TP
(3) antioxidant test
To make Zylox by the foregoing description puts into K is housed
2In the reaction vessels of O, take out observe phenomena.
Above-mentioned test shows technical scheme the best that embodiment 1 provides.
Claims (1)
1. the preparation technology of the full methyl-silicone oil of HMW, processed by the industrial chemicals of following quality proportioning: 10.2 parts of dimethyl silica alkylating mixtures, YSR 3286 are 2.3 parts; The amount of its composite catalyst is respectively: 0.0263 part of tetramethyl-oxyammonia, 0.0025 part of hexamethyl cyclotrisiloxane;
Dimethyl silica alkylating mixture wherein is 5 parts of hexamethyl cyclotrisiloxanes, 30 parts of octamethylcyclotetrasiloxanes, 60 parts of decamethylcyclopentaandoxane, 4 parts of ten diformazan basic rings, six siloxanes, the mixture that tetradecamethylcycloheptasiloxane is 1 part;
It is characterized in that: technical process: get the raw materials ready, filter, binder is switched in dehydration, polymerization, and the matchmaker is broken in slaking, takes off low discharging;
Wherein polymerization procedure is following: when input dimethyl silica alkylating mixture and YSR 3286 carry out polyreaction in reaction kettle; Add composite catalyst; The entire reaction time was controlled at 3 hours, and in first hour of entire reaction, the temperature of reaction of polymeric kettle is controlled at 108 ℃; The temperature of reaction of polymeric kettle is controlled at 115 ℃ in two hours after entire reaction, and the heating steam pressure of polymeric kettle is controlled at 0.2MPa;
The broken matchmaker's step of its matured is following: after the polyreaction reaction is accomplished, switch through the dish valve, material in reactor is used N
2Be pressed into and carry out slaking in the slaking tube, N in the still
2Pressure-controlling is at 0.40MPa; The heating steam of slaking tube is opened, control its vapor pressure, make temperature of charge maintain 125 ℃ at 0.35MPa; After treating that material entering oil adds the hot tearing pipe; Catalyzer decomposes under 150 ℃ of high temperature, loses activity, and material removes low molecular impurity by flash distillation in taking off low device when card is dispersed into filament;
It is following wherein to take off low discharging step: taking off when low, the thermal oil temperature of electrically heated case is controlled at 173 ℃, takes off low molecule device card temperature upper strata and is controlled at 161 ℃, and card temperature lower floor is controlled at 164 ℃; Take off low device top pressure and be controlled at 0.0025 MPa, the card pressure-controlling is at 0.20 MPa, and the vapor pressure control pressure table displayed value that takes off low molecule device heating is 0.58MPa; After material takes off and hangs down, fall into and take off low device feed basin, see packing through spiral discharging machine off through the water cooler material again.
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| CN102617858A (en) * | 2012-04-11 | 2012-08-01 | 唐山三友硅业有限责任公司 | Preparation method for low-volatility 110 methyl vinyl silicone rubber |
| CN102643427B (en) * | 2012-05-09 | 2013-07-03 | 山东轻工业学院 | Method for producing high-purity dimethyl silicon oil by using anhydrous strong alkali as catalyst |
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| CN104672454B (en) * | 2015-03-13 | 2017-11-14 | 扬州宏远化工新材料有限公司 | Waste silicone rubber produces the synthetic method of 201 methyl-silicone oils |
| WO2017084036A1 (en) * | 2015-11-18 | 2017-05-26 | 广州道林合成材料有限公司 | Continuous preparation process of polydimethylsiloxane having high purity and low viscosity |
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| GB803288A (en) * | 1954-05-11 | 1958-10-22 | Gen Electric | Polymerization of organopolysiloxanes |
| CN1105036A (en) * | 1992-12-23 | 1995-07-12 | 国际壳牌研究有限公司 | Star-shaped polydimethylsiloxane block copolymers and process for the preparation thereof |
| CN1837262A (en) * | 2006-04-24 | 2006-09-27 | 广州吉必时科技实业有限公司 | Process for synthesis of polysiloxane |
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Address after: 330300 Yangjialing, Yongxiu County, Jiujiang City, Jiangxi Province Patentee after: JIANGXI BLUESTAR XINGHUO ORGANIC SILICONE Co.,Ltd. Address before: 330319 Spark Industrial Park, Yongxiu County, Jiujiang City, Jiangxi Province Patentee before: Jiangxi Star-Fire Silicone Factory of Bluestar New Chemical Materials Co.,Ltd. |