CN115521461B - Continuous production process of low-viscosity vinyl silicone oil - Google Patents
Continuous production process of low-viscosity vinyl silicone oil Download PDFInfo
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- CN115521461B CN115521461B CN202211107049.8A CN202211107049A CN115521461B CN 115521461 B CN115521461 B CN 115521461B CN 202211107049 A CN202211107049 A CN 202211107049A CN 115521461 B CN115521461 B CN 115521461B
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- 238000000034 method Methods 0.000 title claims abstract description 44
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 title claims abstract description 40
- 229920002554 vinyl polymer Polymers 0.000 title claims abstract description 40
- 229920002545 silicone oil Polymers 0.000 title claims abstract description 36
- 238000010924 continuous production Methods 0.000 title claims abstract description 18
- 230000008569 process Effects 0.000 title claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 35
- 239000007788 liquid Substances 0.000 claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 12
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002861 polymer material Substances 0.000 claims abstract description 5
- 230000003068 static effect Effects 0.000 claims description 34
- -1 siloxane ring Chemical group 0.000 claims description 12
- BITPLIXHRASDQB-UHFFFAOYSA-N ethenyl-[ethenyl(dimethyl)silyl]oxy-dimethylsilane Chemical compound C=C[Si](C)(C)O[Si](C)(C)C=C BITPLIXHRASDQB-UHFFFAOYSA-N 0.000 claims description 7
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 2
- 229910052731 fluorine Inorganic materials 0.000 claims description 2
- 239000011737 fluorine Substances 0.000 claims description 2
- NOKUWSXLHXMAOM-UHFFFAOYSA-N hydroxy(phenyl)silicon Chemical group O[Si]C1=CC=CC=C1 NOKUWSXLHXMAOM-UHFFFAOYSA-N 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- 238000000889 atomisation Methods 0.000 abstract description 13
- 239000003054 catalyst Substances 0.000 abstract description 6
- 238000000926 separation method Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000000725 suspension Substances 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 3
- 238000004220 aggregation Methods 0.000 abstract description 2
- 230000002776 aggregation Effects 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 62
- 238000006116 polymerization reaction Methods 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 20
- 230000008878 coupling Effects 0.000 description 7
- 238000010168 coupling process Methods 0.000 description 7
- 238000005859 coupling reaction Methods 0.000 description 7
- 239000012467 final product Substances 0.000 description 6
- 238000003860 storage Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 5
- 239000003513 alkali Substances 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- OCKGFTQIICXDQW-ZEQRLZLVSA-N 5-[(1r)-1-hydroxy-2-[4-[(2r)-2-hydroxy-2-(4-methyl-1-oxo-3h-2-benzofuran-5-yl)ethyl]piperazin-1-yl]ethyl]-4-methyl-3h-2-benzofuran-1-one Chemical compound C1=C2C(=O)OCC2=C(C)C([C@@H](O)CN2CCN(CC2)C[C@H](O)C2=CC=C3C(=O)OCC3=C2C)=C1 OCKGFTQIICXDQW-ZEQRLZLVSA-N 0.000 description 3
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000003377 acid catalyst Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000003472 neutralizing effect Effects 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 239000004944 Liquid Silicone Rubber Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000001447 alkali salts Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 235000013601 eggs Nutrition 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000010409 ironing Methods 0.000 description 1
- IBIKHMZPHNKTHM-RDTXWAMCSA-N merck compound 25 Chemical compound C1C[C@@H](C(O)=O)[C@H](O)CN1C(C1=C(F)C=CC=C11)=NN1C(=O)C1=C(Cl)C=CC=C1C1CC1 IBIKHMZPHNKTHM-RDTXWAMCSA-N 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
- C08G77/08—Preparatory processes characterised by the catalysts used
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Silicon Polymers (AREA)
Abstract
The application relates to a continuous production process of low-viscosity vinyl silicone oil, which comprises the steps of preheating a siloxane mixture A, introducing the preheated mixture A into a reactor equipped with ultrasonic vibration to polymerize the mixture A to obtain a material B, introducing the material B into a high-speed atomization and devolatilization system to obtain a material C at a certain flow, and introducing the material C into a finished product tank after heat exchange and cooling to obtain a finished product D. The low-viscosity vinyl silicone oil production device and the continuous production process provided by the application have the advantages that firstly, the catalyst is in a micro-suspension state along with materials under ultrasonic vibration, the aggregation reaction and the separation function are integrated, the normal production period is improved, and the continuous production with a long period can be realized; secondly, the polymer material is processed into micron-sized or submicron-sized liquid drops through an atomizer, the dependence of temperature and vacuum degree is greatly reduced, the separation efficiency of low-boiling-point substances is improved, and vinyl silicone oil products with the total quantity of D3-D6 low-ring bodies less than 50ppm can be obtained.
Description
Technical Field
The application relates to a production technology of low-viscosity vinyl silicone oil, belonging to the technical field of chemical equipment and engineering technology.
Background
Vinyl silicone oil is short for vinyl polysiloxane, is one of the main raw materials of addition type liquid silicone rubber, and can be widely applied to the fields of food, medical treatment, electronics, electricity, electric power, aviation, aerospace, intelligent wearing and the like. The low-viscosity vinyl silicone oil is used as a product with lower viscosity of the vinyl silicone oil, and is mainly used as a base material of high-fluidity addition type silica gel and a modifier of other materials. The high-fluidity addition type adhesive is mainly applied to waterproof, packaging and heat conduction of integrated circuits, packaging and heat conduction of 5G base stations, encapsulation and vibration prevention of new energy battery components, wherein the low-viscosity vinyl silicone oil in the formula generally accounts for 10% -99%, and the low-viscosity vinyl quality is critical to the quality of the high-fluidity addition type adhesive.
CN106279697B is prepared by reacting dimethyl siloxane mixed ring with tetramethyl divinyl disiloxane under the action of inorganic liquid catalyst, and then removing the medium. CN112280039A is prepared by reacting dimethyl siloxane mixed ring with tetramethyl divinyl disiloxane under the action of an acid catalyst, neutralizing with liquid alkali or alkali salt, and performing suction filtration or plate-frame filter pressing after neutralizing to obtain low-viscosity vinyl silicone oil by conventional vacuum distillation. CN 111690138B heats methyl cyclosiloxane, methyl vinyl tetracyclic compound, acetic anhydride and acid catalyst concentrated sulfuric acid to 130-165 ℃ under stirring in a closed reaction kettle to react for 4-10 hours, and then removes low content to obtain hydroxyl silicone oil containing vinyl on a side chain. And preheating a mixed section of the CN 112940256B dimethyl cyclosiloxane mixture and hexamethyldisiloxane, polymerizing in an acidic resin fixed bed reactor, and removing by a multilayer thin film evaporator to obtain a methyl silicone oil product.
The above methods can produce low viscosity vinyl silicone oil and methyl silicone oil, but have the following problems: firstly, liquid acid or liquid alkali is adopted for catalysis, and liquid alkali or liquid acid is needed for neutralization, or Wen Pomei is high, the consumption of acid and alkali is large, and a large amount of impurities are left, or the odor of the rotten eggs is left; secondly, the fixed bed reactor has dead angles and dead areas commonly existing due to the limitations of the principle, the structure and the like, the local viscosity is larger, and the use efficiency is low; thirdly, the conventional reduced pressure distillation, the low removal of the thin film evaporator and the low removal efficiency and the effect are to be improved.
Disclosure of Invention
Aiming at the defects of polymerization reaction and catalyst separation of low-viscosity vinyl silicone oil and low efficiency of a conventional fixed bed reactor, the application provides a continuous production process of low-viscosity vinyl silicone oil, which is used for synchronously carrying out polymerization separation, avoiding the reaction dead zone and efficiently removing low components by a micro-suspension reactor, and the vinyl silicone oil with the total amount of D3-D6 low ring bodies of less than 50ppm is obtained.
The application adopts the following technical scheme:
a continuous production process of low-viscosity vinyl silicone oil comprises the following steps:
the siloxane mixture enters a static reactor for reaction at a certain flow after being preheated, enters an atomizer at a certain flow after the reaction is finished, and is subjected to atomization and de-ironing and heat exchange to obtain the low-viscosity vinyl silicone oil.
The device comprises a material A1 and a material A2;
a1 is one or more of methyl siloxane ring, vinyl siloxane ring, phenyl siloxane ring or fluorine-containing siloxane ring; a2 is tetramethyl divinyl disiloxane or alpha, omega-divinyl polydimethylsiloxane.
The mass ratio of the material A1 to the material A2 is 100:100-100:1.
Preheating the siloxane mixture to 40-110 ℃, and then pumping the mixture into a static reactor at a flow rate of 10-600L/h for reaction; an ultrasonic vibration rod is arranged in the static reactor, and the vibration frequency of the ultrasonic vibration rod is preferably 5KHZ-50KHZ.
The static reactor with the ultrasonic vibration rod can be one-stage or multistage static reactors which are connected in series or in parallel.
The polymer material reacted in the static reactor enters an atomizer at the speed of 10L-500L/h, and is stirred at high speed in the atomizer and sheared to atomized liquid drops to 1-100 mu m.
The pressure in the atomizer is controlled to be 0-10KPa, and the temperature is 150-200 ℃. Preferably, the pressure is 5Pa to 3kPa, and the temperature is 170 ℃ to 180 ℃. The atomizer can be a primary atomizer, or can be obtained by connecting a plurality of atomizers in series or in parallel, and when the atomizer is a plurality of atomizers, the pressure of each stage of atomizer is 0-10kPa, preferably 5-3 kPa during operation.
Through the technical scheme, the application has the following technical effects:
1. the catalyst in the static reactor equipped with the ultrasonic vibration moving rod is in a micro-suspension state, so that the scale formation in the reactor is greatly reduced, the service life of the catalyst is prolonged, the material is catalyzed and polymerized by the catalyst in the micro-suspension state, the reaction material is pushed by the feeding power to filter out the polymer material at the top of the reactor, the aggregation reaction and the separation function are integrated, and the long-period continuous production can be realized.
2. The low-viscosity vinyl silicone oil polymer material is processed into micron-sized or submicron-sized liquid drops through an atomizer, the dependence of temperature and vacuum degree is greatly reduced, the separation efficiency of low-boiling substances is improved, and the low-viscosity vinyl silicone oil product with the total amount of D3-D6 low ring bodies less than 50ppm can be obtained.
Drawings
FIG. 1 is a schematic diagram of an apparatus for producing low viscosity vinyl silicone oil, wherein 1 is a raw material tank A,2 is a raw material tank B,3 is a material pump, 4 is a coupling heat exchanger, 5 is a static reactor, 6 is an ultrasonic vibration rod, 7 is a polymerization buffer tank, 8 is an atomizer, 9 is a buffer tank, 10 is a finished product tank, 11 is a low molecular tank, and 12 is a vacuum unit.
Detailed Description
Example 1
The low-viscosity vinyl silicone oil production device is characterized in that a raw material storage tank A1 and a raw material storage tank B2 are respectively connected with a material pump 3 through pipelines, the material pump 3 is connected with a coupling heat exchanger 4, and the coupling heat exchanger 4 is connected with a static reactor 5;
the static reactor 5 is connected with a polymerization buffer tank 7, and the polymerization buffer tank 7 is connected with an atomizer 8;
the atomizer 8 is connected with a buffer tank 9, and the buffer tank 9 is connected with a finished product tank 10.
An ultrasonic vibration bar 6 is arranged on the static reactor 5. The atomizer 8 is connected with a low-molecular storage tank 11, and the low-molecular storage tank 11 is connected with a vacuum unit 12. The buffer tank 9 is connected with the finished product tank 10 through the coupling heat exchanger 4.
Atomizer, LPG series of Woldster rotary atomizing technology Co., ltd.
Static reactor, cangzhou Songchuang plumbing Co.
Example 2
A continuous production process of low-viscosity vinyl silicone oil comprises the following steps of 2m 3 A storage tank 12, wherein the mixed material comprises a siloxane mixed material of 40kg of tetramethyl divinyl disiloxane and 1600kg of octamethyl cyclotetrasiloxane, the mixture is heated to 90 ℃ by a material pump through a preheater, and then enters a static reactor for reaction at a flow rate of 100L/h, an ultrasonic vibration rod is arranged in the static reactor, the vibration frequency of the ultrasonic vibration rod is 20KHZ, and a polymerization sample B-23 is obtained and enters a polymer buffer tank;
and (3) enabling the polymer reacted in the static reactor to enter an atomizer at a flow rate of 90L/h, atomizing and devolatilizing under the conditions that the temperature in the atomizer is 170 ℃ and the pressure is 3KPa, and when the fog drops are stabilized at a size of 70-80 mu m, discharging at a flow rate of 80L/h, and carrying out heat exchange on the material by a buffer tank and a coupling heat exchanger to obtain a low-viscosity vinyl silicone oil finished product D-2.
The atomizer, the commercial products are more, and the example is tried on LPG series of tin-free Wobbe rotary atomization technology Co., ltd.
Example 3
The procedure was as in example 2, except that the flow rate into the static reactor was adjusted to 120L/h, and into the finishing tank to give the finished product D-3.
Example 4
The procedure was as in example 2, except that the flow rate into the static reactor was adjusted to 160L/h, and into the finishing tank to give finished product D-4.
Example 5
The procedure was as in example 2, except that the flow rate into the static reactor was adjusted to 200L/h, and into the finishing tank to give finished product D-5.
Comparative example 2A
The procedure was as in example 2, except that the flow rate into the static reactor was adjusted to 50L/h, and into the finishing tank to give finished product D-2A.
Examples 2 to 5 and comparative example 2A, the results are shown in Table 1.
Table 1 results list of examples 1 to 5 and comparative example 2A
Note that: x1 and Y1 are respectively 2 or 3 or 4 or 5 or 2A polymerization sample and finished product.
Example 6
A continuous production process of low-viscosity vinyl silicone oil comprises the following steps that a siloxane mixture of 23kg of tetramethyl divinyl disiloxane and 1600kg of octamethyl cyclotetrasiloxane is preheated to 90 ℃ and then enters a static reactor for reaction at a flow rate of 140L/h, and an ultrasonic vibration rod is arranged in the static reactor, wherein the vibration frequency of the ultrasonic vibration rod is 20KHZ.
And (3) enabling the polymer reacted in the static reactor to enter an atomizer at a flow rate of 120L/h, atomizing and devolatilizing under the conditions that the temperature in the atomizer is 170 ℃ and the pressure is 3KPa, and stably discharging at a flow rate of 100L/h when the fog drops are stabilized at a size of 70-80 mu m, and obtaining a low-viscosity vinyl silicone oil finished product D-6 after the material is subjected to heat exchange through a buffer tank and a coupling heat exchanger.
Wherein the atomizer is a high-speed pneumatic atomizer of a disc coating machine of taiwan brightness, and the air source is 99.999 nitrogen.
Example 7
The procedure was as in example 6, except that the flow rate into the static reactor was adjusted to 180L/h, and into the finishing tank to give finished product D-7.
Example 8
The procedure was as in example 6, except that the flow rate into the static reactor was adjusted to 240L/h, and into the finishing tank to give finished product D-8.
Example 9
The procedure was as in example 6, except that the flow rate into the static reactor was adjusted to 280L/h, and into the finishing tank to give finished product D-9.
Comparative example 6B
The procedure was as in example 6, except that the flow rate into the static reactor was adjusted to 100L/h, and into the finishing tank to give finished product D-6B.
Example 6C
The procedure was as in example 6, except that the flow rate into the static reactor was adjusted to 60L/h, and into the finishing tank to give the finished product D-6C.
Examples 6 to 9, comparative examples 6B and 6C, and the results are shown in table 2.
Table 2 results list of examples 6-9, comparative examples 6B and 6C
Note that: x2 and Y2 are respectively 6 or 7 or 8 or 9 or 6B or 6C polymerization samples and finished products.
Example 10
The operation procedure is the same as in example 2, the frequency of the ultrasonic vibration rod is only adjusted to be 30KW and 30KHZ respectively, the polymerization sample is B-10, and the finished product is D-10 after entering the finished product tank.
Example 11
The operation procedure is the same as in example 2, and the frequency of the ultrasonic vibration rod is only adjusted to 40KW and 40KHZ respectively, the polymerization sample is B-11, and the obtained product enters a finished product tank to obtain a finished product D-11.
Example 12
The operation procedure is the same as in example 6, the frequency of the ultrasonic vibration rod is only adjusted to 25KW and 35KHZ respectively, the polymerization sample is B-12, and the finished product is D-12 after entering the finished product tank.
Example 13
The operation procedure is the same as in example 6, and the frequency of the ultrasonic vibration rod is only adjusted to 45KW and 65KHZ respectively, the polymerization sample is B-13, and the polymerization sample enters a finished product tank to be a finished product D-13.
Comparative example 10D
The operation procedure is the same as in example 2, and the frequency of the ultrasonic vibration rod is only adjusted to 10KW and 10KHZ respectively, the polymerization sample is B-10D, and the polymerization sample enters a finished product tank to be a finished product D-10D.
Comparative example 12E
The operation procedure is the same as in example 6, and the frequency of the ultrasonic vibration rod is only adjusted to 10KW and 10KHZ respectively, the polymerization sample is B-10D, and the polymerization sample enters a finished product tank to be a finished product D-10D.
The results of examples 10 to 13 and comparative examples 10D and 12E are shown in Table 3.
Table 3 results list of examples 10-13, comparative examples 10D and 12E
Note that: x3 and Y3 are respectively 10 or 11 or 12 or 13 or 10D or 12E polymerization samples and finished products.
Example 14
The operation procedure is the same as in example 2, the size of atomized liquid drops of the atomizer is adjusted from 70-80 μm to 50-60 μm, and the atomized liquid drops enter a finished product tank to obtain a finished product D-14.
Example 15
The operation procedure is the same as in example 2, the size of atomized liquid drops of the atomizer is adjusted from 70-80 μm to 30-40 μm, and the atomized liquid drops enter a finished product tank to obtain a finished product D-15.
Example 16
The operation procedure is the same as in example 2, the size of atomized liquid drops of the atomizer is adjusted from 70 to 80 mu m to 15 to 20 mu m, and the atomized liquid drops enter a finished product tank to be a finished product D-16.
Example 17
The operation procedure is the same as in example 2, the size of atomized liquid drops of the atomizer is adjusted from 70-80 μm to 1-8 μm, and the atomized liquid drops enter a finished product tank to obtain a finished product D-17.
Comparative example 14F
The operation procedure is the same as in example 2, the size of atomized liquid drops of the atomizer is adjusted from 70 to 80 μm by 200 to 500 μm, and the atomized liquid drops enter a finished product tank to be a finished product D to 14F.
The results of examples 14 to 17 and comparative example 14F are shown in Table 4.
Table 4 results list of examples 14 to 17 and comparative example 14F
Note that: y4 is 14 or 15 or 16 or 17 or 18 or 14F, respectively.
Example 18
The operation procedure is the same as in example 2, only the primary atomization stripping is increased to the secondary atomization stripping, and the secondary atomization stripping is carried out to obtain a finished product D-18 in a finished product tank.
Example 19
The operation procedure is the same as in example 2, only the primary atomization stripping is increased to the tertiary atomization stripping, and the primary atomization stripping is carried out in a finished product tank to obtain a finished product D-19.
Example 20
The procedure was as in example 18, with only 3kpa set to 5kpa for the vacuum unit 53 (1), and the product was fed into the product tank as the product D-20.
Example 21
The procedure was as in example 18, except that the pressure setting of the vacuum unit 53 (1) was adjusted to 500Pa, and the product was fed into the final tank as the final product D-21.
Example 22
The procedure was as in example 18, with only 3kpa set to 100pa for the vacuum unit 53 (1), and the product was fed into the product tank as product D-18.
Comparative example 18G
The procedure was as in example 14, except that the primary atomization stripping was increased to the quaternary atomization stripping, and the product was fed into the product tank as the product D-14F.
Comparative example 22H
The operation procedure was the same as in example 14, except that the primary atomization dropping was increased to the tertiary atomization dropping, the pressure setting of the vacuum unit 53 (1) was adjusted to 15kpa at 3kpa, and the resultant was fed into the final tank as the final product D-18G.
The results of examples 14 to 18 and comparative examples 18G and 22H are shown in Table 5.
Table 5 results list of examples 18-22, comparative examples 18G and 22H
Note that: y5 is a polymerization sample and a finished product of 18 or 19 or 20 or 21 or 22 or 18G or 22H, respectively.
Example 23
2m 3 A storage tank 12, wherein the mixed material A-23 comprises 32L of tetramethyl divinyl disiloxane and 1600L of octamethyl cyclotetrasiloxane, and enters a static reactor through a preheater 31 by a material pump 21 at a flow rate of 180L/h, and enters a polymer buffer tank to obtain a polymerization sample B-23; starting the vacuum unit in advance, setting the pressure to be 500Pa, feeding the material B-23 into a primary atomizer at 170 ℃ at 160L/h, continuously feeding into a secondary atomizer at 170 ℃,starting a vacuum unit in advance, adjusting parameters of the primary atomizer and the secondary atomizer to keep the droplet size to be about 15-20 mu m, enabling the droplets to flow out at a flow rate of 135L/h after the system is stable, and enabling the droplets to enter a buffer tank to obtain a material C-23; and the material C-23 is subjected to coupling heat exchange with a preheater through a heat exchanger 61 and enters a finished product tank to obtain a finished product material D-23.
The atomizing apparatus and the gas source were as in example 6.
Example 24
The atomizer temperature was adjusted from 170 ℃ to 150 ℃ and the other operating steps were the same as in example 23 to obtain the final product material D-24.
Example 25
The atomizer temperature was adjusted from 170 ℃ to 130 ℃ and the other operating steps were the same as in example 23 to obtain the final product material D-25.
Example 26
The atomizer temperature was adjusted from 170 ℃ to 110 ℃ and the other operating steps were the same as in example 23 to obtain the final product material D-26.
Comparative example 23K
The atomizer temperature was adjusted from 170 ℃ to 190 ℃ and the other operating steps were the same as in example 23 to obtain the final product material D-23K.
The results of examples 23 to 26 and comparative example 23K are shown in Table 6.
Table 6 results of examples 23 to 26 and comparative example 23K Table
Note that: y6 is a polymerization sample and a finished product of 23 or 24 or 25 or 26 or 23K respectively.
The above embodiments are merely preferred embodiments of the present application, and should not be construed as limiting the present application, and the embodiments and features of the embodiments of the present application may be arbitrarily combined with each other without collision. The protection scope of the present application is defined by the claims, and the protection scope includes equivalent alternatives to the technical features of the claims. I.e., equivalent replacement modifications within the scope of this application are also within the scope of the application.
Claims (8)
1. The continuous production process of the low-viscosity vinyl silicone oil is characterized by comprising the following steps of:
the siloxane mixture enters a static reactor for reaction at a certain flow after being preheated, enters an atomizer at a certain flow after the reaction is finished, is atomized and reduced, and then undergoes heat exchange to obtain low-viscosity vinyl silicone oil, wherein the low-viscosity vinyl silicone oil comprises a material A1 and a material A2; preheating the siloxane mixture to 40-110 ℃, and then pumping the siloxane mixture into a static reactor for reaction at a flow rate of 100-200L/h;
a1 is one or more of methyl siloxane ring, vinyl siloxane ring, phenyl siloxane ring or fluorine-containing siloxane ring; a2 is one or two of tetramethyl divinyl disiloxane or alpha, omega-divinyl polydimethylsiloxane; an ultrasonic vibration rod is arranged in the static reactor, the vibration frequency of the ultrasonic vibration rod is 20KHZ-50KHZ, and the ultrasonic vibration rod is stirred at a high speed in an atomizer and sheared until atomized liquid drops reach 1-100 mu m.
2. The continuous production process of low-viscosity vinyl silicone oil according to claim 1, wherein the mass ratio of the material A1 to the material A2 is 100:100-100:1.
3. The continuous production process of low-viscosity vinyl silicone oil according to claim 1, wherein the static reactor is a static reactor realized by one or more stages connected in series or in parallel.
4. The continuous production process of low-viscosity vinyl silicone oil according to claim 1, wherein the polymer material after the reaction in the static reactor is fed into the atomizer at 10L to 500L/h.
5. The continuous production process of low-viscosity vinyl silicone oil according to claim 4, wherein the pressure in the atomizer is controlled to be 0-10KPa, and the temperature is controlled to be 150-200 ℃.
6. The continuous production process of low-viscosity vinyl silicone oil according to claim 5, wherein the pressure in the atomizer is controlled to be 5 Pa-3 kPa, and the temperature is 170-180 ℃.
7. The continuous production process of low-viscosity vinyl silicone oil according to claim 4, wherein the atomizer is a primary atomizer, and can be obtained by connecting a plurality of atomizers in series or in parallel, and when the atomizer is a plurality of atomizers, the pressure of each primary atomizer is 0-10kPa during operation.
8. The continuous production process of low-viscosity vinyl silicone oil according to claim 7, wherein the pressure of each stage of atomizer is 5Pa to 3kPa during operation.
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| US4250290A (en) * | 1979-06-18 | 1981-02-10 | General Electric Company | Process for the continuous manufacture of siloxane polymers |
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| CN102924721A (en) * | 2012-11-22 | 2013-02-13 | 深圳市森日有机硅材料有限公司 | Method for continuously preparing vinyl silicone oil |
| CN204973853U (en) * | 2015-09-29 | 2016-01-20 | 成都博达爱福科技有限公司 | Organosilicon takes off low device |
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| US4250290A (en) * | 1979-06-18 | 1981-02-10 | General Electric Company | Process for the continuous manufacture of siloxane polymers |
| CN1334274A (en) * | 2000-07-26 | 2002-02-06 | 陶氏康宁有限公司 | Polymerization reactor and method |
| CN102924721A (en) * | 2012-11-22 | 2013-02-13 | 深圳市森日有机硅材料有限公司 | Method for continuously preparing vinyl silicone oil |
| CN204973853U (en) * | 2015-09-29 | 2016-01-20 | 成都博达爱福科技有限公司 | Organosilicon takes off low device |
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