CN116003797A - High-boiling silicone oil production process and production system - Google Patents
High-boiling silicone oil production process and production system Download PDFInfo
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- CN116003797A CN116003797A CN202211570974.4A CN202211570974A CN116003797A CN 116003797 A CN116003797 A CN 116003797A CN 202211570974 A CN202211570974 A CN 202211570974A CN 116003797 A CN116003797 A CN 116003797A
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- 238000009835 boiling Methods 0.000 title claims abstract description 147
- 229920002545 silicone oil Polymers 0.000 title claims abstract description 120
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 38
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 94
- 238000005406 washing Methods 0.000 claims abstract description 78
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 60
- 230000007062 hydrolysis Effects 0.000 claims abstract description 55
- 238000011282 treatment Methods 0.000 claims abstract description 39
- 239000003513 alkali Substances 0.000 claims abstract description 35
- 239000002253 acid Substances 0.000 claims abstract description 33
- 230000002378 acidificating effect Effects 0.000 claims abstract description 30
- 239000000178 monomer Substances 0.000 claims abstract description 30
- 238000001035 drying Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000001914 filtration Methods 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 16
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 14
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000010703 silicon Substances 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 230000007935 neutral effect Effects 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 239000007788 liquid Substances 0.000 claims description 26
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 22
- 239000000872 buffer Substances 0.000 claims description 18
- 239000003921 oil Substances 0.000 claims description 18
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 16
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 11
- 239000007787 solid Substances 0.000 claims description 11
- 238000003860 storage Methods 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 9
- 239000002274 desiccant Substances 0.000 claims description 8
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 8
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 8
- 230000032798 delamination Effects 0.000 claims 1
- 238000002156 mixing Methods 0.000 abstract description 12
- 230000003301 hydrolyzing effect Effects 0.000 abstract 1
- 239000011368 organic material Substances 0.000 description 7
- 239000012535 impurity Substances 0.000 description 6
- 239000007853 buffer solution Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- -1 polytetrafluoroethylene Polymers 0.000 description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 description 3
- 206010024769 Local reaction Diseases 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000005046 Chlorosilane Substances 0.000 description 1
- 229910008045 Si-Si Inorganic materials 0.000 description 1
- 229910006411 Si—Si Inorganic materials 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 238000006136 alcoholysis reaction Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- YGZSVWMBUCGDCV-UHFFFAOYSA-N chloro(methyl)silane Chemical compound C[SiH2]Cl YGZSVWMBUCGDCV-UHFFFAOYSA-N 0.000 description 1
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- ZHPNWZCWUUJAJC-UHFFFAOYSA-N fluorosilicon Chemical compound [Si]F ZHPNWZCWUUJAJC-UHFFFAOYSA-N 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
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Abstract
The invention provides a high-boiling silicone oil production process and a production system, and relates to the technical field of silicone oil production. The method comprises the following steps: s1, mixing and hydrolyzing the organic silicon high-boiling monomer and the first dilute hydrochloric acid to obtain a hydrolysis mixture. S2, layering the hydrolysis mixture at constant temperature to obtain the first acidic high-boiling silicone oil and raw material concentrated hydrochloric acid. S3, separating the raw material concentrated hydrochloric acid to obtain second acidic high-boiling silicone oil and first concentrated hydrochloric acid. S4, separating the first acidic high-boiling silicone oil from the second acidic high-boiling silicone oil to obtain second concentrated hydrochloric acid and pretreated high-boiling silicone oil. S5, washing the pretreated high-boiling silicone oil to obtain second dilute hydrochloric acid and weak acid high-boiling silicone oil. S6, performing alkali washing treatment on the weak acid high-boiling silicone oil to obtain neutral high-boiling silicone oil and alkali liquor. S7, drying and filtering the medium high-boiling silicone oil to obtain the finished product high-boiling silicone oil. The high-quality high-boiling silicone oil is ensured to be produced by improving the production process and the production system.
Description
Technical Field
The invention relates to the technical field of silicone oil production, in particular to a high-boiling silicone oil production process and a production system.
Background
The high boiling silicone oil is prepared from methyl chlorosilane monomer by Si-Si, si-0-Si and Si-CH 2 High-boiling chlorosilane mixtures with Si bonds as main chain, with pungent odor and strong corrosiveness are used as raw materials, and the polymethyl siloxane is produced through hydrolysis or alcoholysis. The high-boiling silicone oil has excellent performance, excellent waterproof, high and low temperature resistance, low viscosity temperature coefficient and other characteristics, and has wide application in the market of low-end silicone oil products.
The comprehensive utilization method of the organic silicon high-boiling monomer mainly comprises the following steps: hydrolysis, cleavage, incineration, and the like. The method for producing the high-boiling silicone oil product by the hydrolysis method has the highest efficiency and the least pollutant. However, the existing high-boiling silicone oil production method has the problems of lag production process, uneven product quality and the like. Most high boiling silicone oil production processes adopt a mode of hydrolysis reaction in a stirring kettle, and patent CN115069182A and CN115197424A both describe kettle type hydrolysis methods. The hydrolysis raw materials are unevenly mixed by the mode, the hydrolysis reaction is slow, and the heat release amount of local reaction in the reaction kettle is too large, so that the quality of the high-boiling silicone oil is unstable. Patent CN101619072B describes a pressurized loop hydrolysis process of dimethyldichlorosilane, but because the flash point of high-boiling silicone oil is 17-23 ℃, the flash point is lower, so that potential safety hazards exist in the pressurized loop hydrolysis. Therefore, most domestic high-boiling silicone oil production processes fall behind, so that most products do not meet the requirements of the industry standard of the high-boiling silicone oil of the China fluorine-silicon organic materials industry society T_FSI 007-2017.
Disclosure of Invention
In view of the above, the invention aims to provide a production process and a production system of high-boiling silicone oil, which are used for solving the problems of unstable product quality, potential safety hazard and the like of the existing production process of the high-boiling silicone oil.
Based on the above purpose, the invention provides a high-boiling silicone oil production process, which comprises the following steps:
s1, introducing an organosilicon high-boiling monomer and first dilute hydrochloric acid into a loop hydrolysis unit in proportion to carry out mixed hydrolysis treatment, so as to obtain a hydrolysis mixture.
S2, layering the hydrolysis mixture at constant temperature by using a layering device, and separating out the first acidic high-boiling silicone oil and the raw material concentrated hydrochloric acid.
S3, separating the raw material concentrated hydrochloric acid to obtain second acidic high-boiling silicone oil and first concentrated hydrochloric acid.
S4, separating the first acidic high-boiling silicone oil from the second acidic high-boiling silicone oil to obtain second concentrated hydrochloric acid and pretreated acidic high-boiling silicone oil.
S5, washing the pretreated acidic high-boiling silicone oil to obtain second dilute hydrochloric acid and weak acidic high-boiling silicone oil.
S6, performing alkali washing treatment on the weak acid high-boiling silicone oil to obtain neutral high-boiling silicone oil and alkali liquor.
S7, drying and filtering the medium high-boiling silicone oil to obtain the finished product high-boiling silicone oil.
Further, the concentration of the first dilute hydrochloric acid in the S1 is 1-6%, and the volume ratio of the organic silicon high-boiling monomer to the first dilute hydrochloric acid is 1:1.6-2.5; the temperature of the hydrolysis treatment is controlled to be 10-45 ℃, and the pressure of a circulating pump outlet in the hydrolysis treatment is 0.15-0.20 MPa.
Further, the temperature of constant-temperature layering in the step S2 is controlled to be 10-30 ℃.
Further, the temperature of the water washing treatment in the step S5 is 70-85 ℃.
Further, in the step S6, sodium bicarbonate solution with the concentration of 15-25% is adopted for the alkaline washing treatment, and the temperature of the alkaline washing treatment is 70-85 ℃.
In the drying and filtering treatment in the step S7, light sodium carbonate solid is adopted as a drying agent, and the mass of the light sodium carbonate solid is 5-8% of that of the neutral high-boiling silicone oil.
The high-boiling silicone oil production system comprises a dilute hydrochloric acid buffer tank, an organosilicon high-boiling monomer storage tank, a hydrolysis loop unit, a constant-temperature layering device, a concentrated acid phase separator, an acid-oil phase separator, a water washing kettle, an alkaline washing kettle, a layering device, a drying kettle and a filtering tank; the dilute hydrochloric acid buffer tank discharge port and the organic silicon high-boiling monomer storage tank discharge port are respectively connected with the hydrolysis loop unit feed port, the hydrolysis loop unit discharge port is connected with the constant temperature layering device feed port, the two discharge ports of the constant temperature layering device are respectively connected with the concentrated acid phase separator feed port and the acid-oil phase separator feed port, the discharge port of the concentrated acid phase separator is connected with the acid-oil phase separator feed port, the acid-oil phase separator discharge port is connected with the water washing kettle feed port, the two discharge ports of the water washing kettle are respectively connected with the dilute hydrochloric acid buffer tank feed port and the alkaline washing kettle feed port, the alkaline washing kettle discharge port is connected with the layering device feed port, the layering device discharge port is connected with the drying kettle feed port, and the drying kettle discharge port is connected with the filter tank.
Further, the hydrolysis loop unit comprises a mixer, a circulating pump, a cooler, a reactor and a distributor, wherein a discharge hole of a dilute hydrochloric acid buffer tank and a discharge hole of an organic silicon high-boiling monomer storage tank are respectively connected with a feed hole of the mixer, the discharge hole of the mixer is connected with a feed hole of the circulating pump, the discharge hole of the circulating pump is connected with a feed hole of the cooler, the discharge hole of the cooler is connected with a feed hole of the reactor, the discharge hole of the reactor is connected with a feed hole of the distributor, and two discharge holes of the distributor are respectively connected with the feed hole of the mixer and the feed hole of the constant-temperature layering device.
Further, the system also comprises an alkali liquor tank, an alkali liquor outlet is arranged on the layering device, the alkali liquor outlet is connected with a liquid inlet of the alkali liquor tank, and a liquid outlet of the alkali liquor tank is connected with a feed inlet of the alkali washing kettle.
Further, the feed inlets of the water washing kettle and the alkaline washing kettle are respectively provided with a washing mixer.
Compared with the prior art, the invention has the beneficial effects that: according to the invention, the dilute hydrochloric acid and the organic silicon high-boiling monomer are mixed by the mixer, and hydrolysis is carried out in the hydrolysis loop unit, so that the problems of uneven raw material mixing, slow hydrolysis reaction, overlarge local reaction exotherm in the reaction kettle and the like in a kettle type hydrolysis mode in the prior art are solved, and the products after the hydrolysis reaction are sequentially subjected to treatments such as constant-temperature layering, separation, water washing, alkali washing and the like. The high-boiling silicone oil production process and the device are improved, so that the produced finished high-boiling silicone oil has high quality, and the safety risk in the production process is reduced.
Drawings
FIG. 1 is a flow chart of a production process of high-boiling silicone oil provided by the embodiment of the invention;
FIG. 2 is a diagram showing the connection relationship of the high-boiling silicone oil production system provided by the embodiment of the invention;
FIG. 3 is a schematic diagram of a mixer of a high boiling silicone oil production system according to an embodiment of the present invention;
fig. 4 is a schematic diagram of a washing mixer of the high-boiling silicone oil production system according to the embodiment of the invention.
Marked in the figure as: 1. a dilute hydrochloric acid inlet; 2. an organosilicon high-boiling monomer inlet; 3. a mixed material outlet; 4. a fin mixing element; 5. a washing liquid inlet; 6. a high boiling silicone oil inlet; 7. a mixed liquid outlet; 8. a cylindrical perforated mixing element; 9. a dilute hydrochloric acid buffer tank; 10. an organosilicon high-boiling monomer storage tank; 11. a mixer; 12. a circulation pump; 13. a cooler; 14. a reactor; 15. a distributor; 16. a constant temperature delaminator; 17. a concentrated acid buffer tank; 18. a concentrated acid phase separator; 19. an acid-oil phase separator; 20. a concentrated acid tank; 21. washing the kettle; 22. alkali washing of the kettle; 23. a base tank; 24. a delaminator; 25. a buffer tank; 26. a drying kettle; 27. a filter tank; 28. and (5) a finished product tank.
Detailed Description
The present invention will be further described in detail with reference to specific embodiments in order to make the objects, technical solutions and advantages of the present invention more apparent.
As shown in FIG. 1, the production process of the high-boiling silicone oil provided by the invention is carried out according to the following steps:
s1, introducing an organosilicon high-boiling monomer and first dilute hydrochloric acid into a hydrolysis loop unit in proportion for mixed hydrolysis treatment, wherein the concentration of the first dilute hydrochloric acid is 1-6%, the volume ratio of the organosilicon high-boiling monomer to the first dilute hydrochloric acid is 1:1.6-2.5, and the temperature of the hydrolysis treatment is controlled at 10-45 ℃ to obtain a hydrolysis mixture.
S2, carrying out constant-temperature layering treatment on the hydrolysis mixture by using a layering device 24, controlling the temperature of constant-temperature layering at 10-30 ℃, and separating the hydrolysis mixture into first acidic high-boiling silicone oil and raw material concentrated hydrochloric acid.
S3, separating the raw material concentrated hydrochloric acid through a concentrated acid phase separator 18 to obtain second acidic high-boiling silicone oil and first concentrated hydrochloric acid, wherein the first concentrated hydrochloric acid is used as a raw material of the deep desorption treatment device.
S4, the first acidic high-boiling silicone oil and the second acidic high-boiling silicone oil are fed into an acid oil phase separator 19 together for separation to obtain second concentrated hydrochloric acid and pretreated acidic high-boiling silicone oil, and the second concentrated hydrochloric acid enters an concentrated acid tank 20.
And S5, carrying out water washing treatment on the pretreated acidic high-boiling silicone oil, wherein the temperature of the water washing treatment is 70-85 ℃, and obtaining second dilute hydrochloric acid and weak acidic high-boiling silicone oil.
And S6, feeding second dilute hydrochloric acid serving as a raw material into the mixer 11, and performing alkaline washing treatment on the weak acid high-boiling silicone oil, wherein the alkaline washing treatment adopts sodium bicarbonate solution with the concentration of 15-25%, and the alkaline washing treatment temperature is 70-85 ℃ to obtain neutral high-boiling silicone oil and alkali liquor.
S7, returning the alkali liquor to the alkali liquor tank 23, and drying and filtering the neutral high-boiling silicone oil to obtain the finished product high-boiling silicone oil. And drying and filtering, wherein light sodium carbonate solid is used as a drying agent, and the mass of the light sodium carbonate solid is 5-8% of that of the neutral high-boiling silicone oil.
As shown in FIG. 2, the high-boiling silicone oil production system consists of a dilute hydrochloric acid buffer tank 9, an organosilicon high-boiling monomer storage tank 10, a hydrolysis loop unit, a constant-temperature delaminator 16, a concentrated acid phase separator 18, an acid-oil phase separator 19, a water washing kettle 21, an alkaline washing kettle 22, a delaminator 24, a drying kettle 26, a filtering tank 27 and the like.
The dilute hydrochloric acid buffer tank 9 is used for storing first dilute hydrochloric acid, and the organosilicon high-boiling monomer storage tank 10 is used for storing organosilicon high-boiling monomers. The hydrolysis loop unit is used for carrying out mixed hydrolysis reaction, and consists of a mixer 11, a circulating pump 12, a cooler 13, a reactor 14, a distributor 15 and the like. As shown in fig. 3, the mixer 11 is composed of a dilute hydrochloric acid inlet 1, an organosilicon high-boiling monomer inlet 2, a mixed material outlet 3, a fin mixing original 4 and the like. The mixer 11 is used for mixing the first dilute hydrochloric acid and the organosilicon high-boiling monomer, the discharge port of the dilute hydrochloric acid buffer tank 9 is connected with the dilute hydrochloric acid inlet 1, and the discharge port of the organosilicon high-boiling monomer storage tank 10 is connected with the organosilicon high-boiling monomer inlet 2. The mixer 11 equipment shell is made of steel lining polytetrafluoroethylene, a fin mixing element is arranged in the mixer, and the mixing unit is made of polytetrafluoroethylene.
The mixed material outlet 3 is connected with a feeding port of the circulating pump 12, a discharging port of the circulating pump 12 is connected with a feeding port of the cooler 13, and the pressure of the outlet of the circulating pump 12 is 0.15-0.20 MPa. The discharge port of the cooler 13 is connected with the feed port of the reactor 14, the discharge port of the reactor 14 is connected with the feed port of the distributor 15, the top end of the distributor 15 is at normal pressure, and the two discharge ports of the distributor 15 are respectively connected with the dilute hydrochloric acid inlet 1 of the mixer 11 and the feed port of the constant temperature layering device 16.
The constant temperature layering device 16 is used for carrying out constant temperature layering, two discharge ports of the constant temperature layering device 16 are respectively connected with a feed port of the concentrated acid buffer tank 17 and a feed port of the acid-oil phase separator 19, separated first acidic high-boiling silicone oil flows into the acid-oil phase separator 19, and separated raw material concentrated hydrochloric acid flows into the concentrated acid buffer tank 17.
The discharge port of the concentrated acid buffer tank 17 is connected with the feed port of the concentrated acid phase separator 18, the concentrated acid phase separator 18 is used for separating raw material concentrated hydrochloric acid, the concentrated acid phase separator 18 comprises two discharge ports, one discharge port is connected with the feed port of the acid-oil phase separator 19, and the separated second acidic high-boiling silicone oil is introduced into the acid-oil phase separator 19; the other is connected with the concentrated acid tank 20, and the separated first concentrated hydrochloric acid is introduced into the concentrated acid tank 20 for collection, so that the second use in other processes is facilitated.
The acid-oil phase separator 19 is used for separating the first acidic high-boiling silicone oil and the second acidic high-boiling silicone oil, the acid-oil phase separator 19 comprises two discharge ports, one discharge port is connected with the concentrated acid tank 20, and the separated second concentrated hydrochloric acid is introduced into the concentrated acid tank 20 for collection, so that the second concentrated hydrochloric acid can be conveniently reused in other processes.
The feed inlet of the water washing kettle 21 is provided with a washing mixer, as shown in fig. 4, which consists of a washing liquid inlet 5, a high-boiling silicone oil inlet 6, a mixed liquid outlet 7, a columnar open pore mixing original 8 and the like. The washing liquid inlet 5 is used for introducing process water, the high-boiling silicone oil inlet 6 is connected with the other discharge port of the acid-oil phase separator 19, and the mixed liquid outlet 7 is connected with the feed inlet of the water washing kettle 21. The washing mixer equipment shell is made of steel lining polytetrafluoroethylene, a columnar open-pore mixing element is arranged in the washing mixer equipment shell, and the mixing element is made of titanium alloy. After evenly mixing the process water and the pretreated high-boiling silicone oil, the mixture enters a water washing kettle 21 for water washing. Two discharge ports of the water washing kettle 21 are respectively connected with a feed port of the dilute hydrochloric acid buffer tank 9 and a feed port of the alkaline washing kettle 22. And introducing the second dilute hydrochloric acid obtained after the water washing treatment into a dilute hydrochloric acid buffer tank 9, and continuously recycling the second dilute hydrochloric acid as a production raw material. The slightly acidic high boiling silicone oil obtained after the water washing treatment enters an alkaline washing kettle 22 for alkaline washing treatment.
The alkali washing kettle 22 is provided with a washing mixer at the feed inlet, and alkali liquor used for alkali washing is evenly mixed with the weak acid high boiling silicone oil and then enters the alkali washing kettle 22 for alkali washing. The discharge port of the alkaline cleaning kettle 22 is connected with the feed port of the delaminator 24, the delaminator 24 is provided with a discharge port and an alkaline liquid outlet, and the alkaline liquid outlet is connected with the liquid inlet of the alkaline liquid tank 23. An alkali liquor inlet is arranged on the alkali washing kettle 22 and is connected with a liquid outlet of the alkali liquor tank 23. The alkali liquor separated after the alkali washing treatment is introduced into an alkali liquor tank 23 and is continuously used for the alkali washing treatment. The discharge port of the layering device 24 is connected with the feed port of the buffer tank 25, and the buffer tank 25 plays a role in buffering. The discharge port of the buffer tank 25 is connected with the feed port of the drying kettle 26, and the drying kettle 26 is used for drying treatment. The discharge port of the drying kettle 26 is connected with the feed port of a filter tank 27, and the filter tank 27 is used for filtering treatment. The discharge port of the filter tank 27 is connected with a finished product tank 28, and the finished product tank 28 is used for collecting finished high-boiling silicone oil.
China fluorosilicone organic materials industry society T_FSI007-2017 high boiling silicone oil industry standard: the appearance is oily liquid, and no obvious mechanical impurities are visible; high-boiling silicone oil type I (25 ℃) viscosity of 4-50 mm 2 S; the acid value (calculated by KOH) is less than or equal to 0.20mg/g; the density (25 ℃) is 0.90-1.10 g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the Refractive index of 1.43-1.47 n 25 D . The following description is made in connection with specific embodiments:
example 1:
the concentration of the first dilute hydrochloric acid is 1.5%, the volume ratio of the organic silicon high-boiling monomer to the first dilute hydrochloric acid is 1/1.6, the hydrolysis loop control temperature is 10 ℃, the outlet control pressure of the hydrolysis loop circulation pump 12 is 0.15MPa, and the top end of the hydrolysis loop distributor 15 is normal pressure. The temperature of the thermostatic delaminator 16 was controlled at 10 ℃. The water washing temperature is 70 ℃, and the alkaline washing temperature is 70 ℃. The lye is 15% sodium bicarbonate solution. The drying agent is light sodium carbonate solid, and the addition amount is 5% of the mass of the high-boiling silicone oil to be treated. Finally, the high-boiling silicone oil product is obtained after filtration in the filter tank 27.
The high-boiling silicone oil product obtained in this example was tested, and the test results were: the appearance is oily liquid, and no obvious mechanical impurities are visible; viscosity of 8mm 2 S; acid number (in KOH) 0.19mg/g; density of 0.96g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the Refractive index of 1.43n 25 D . Meets the industry standard of the high-boiling silicone oil of China fluorosilicone organic materials industry society T_FSI 007-2017.
Example 2:
the concentration of the first dilute hydrochloric acid is 2.0%, the volume ratio of the organic silicon high-boiling monomer to the first dilute hydrochloric acid is 1/1.8, the hydrolysis loop control temperature is 15 ℃, the outlet control pressure of the hydrolysis loop circulation pump 12 is 0.18MPa, and the top end of the hydrolysis loop distributor 15 is normal pressure. The temperature of the thermostatic delaminator 16 was controlled at 15 ℃. The water washing temperature was 75℃and the alkaline washing temperature was 75 ℃. The lye is 18% sodium bicarbonate solution. The drying agent is light sodium carbonate solid, and the addition amount is 6% of the mass of the high-boiling silicone oil to be treated. The high boiling silicone oil product is obtained after filtration in the filter tank 27.
The high-boiling silicone oil product obtained in this example was tested, and the test results were: the appearance is oily liquid, and no obvious mechanical impurities are visible; viscosity 9.5mm 2 S; acid number (in KOH) 0.17mg/g; density of 0.97g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the Refractive index of 1.44n 25 D . Meets the industry standard of the high-boiling silicone oil of China fluorosilicone organic materials industry society T_FSI 007-2017.
Example 3:
the concentration of the first dilute hydrochloric acid is 3.0%, the volume ratio of the organic silicon high-boiling monomer to the first dilute hydrochloric acid is 1/2.0, the hydrolysis loop control temperature is 20 ℃, the outlet control pressure of the hydrolysis loop circulation pump 12 is 0.19MPa, and the top end of the hydrolysis loop distributor 15 is normal pressure. The temperature of the thermostatic delaminator 16 is controlled at 20 ℃. The water washing temperature was 80℃and the alkaline washing temperature was 80 ℃. The lye is 20% sodium bicarbonate solution. The drying agent is light sodium carbonate solid, and the adding amount is 7% of the mass of the high-boiling silicone oil to be treated. The high boiling silicone oil product is obtained after filtration in the filter tank 27.
The high-boiling silicone oil product obtained in this example was tested, and the test results were: the appearance is oily liquid, and no obvious mechanical impurities are visible; viscosity of 11.5mm 2 S; acid number (in KOH) 0.15mg/g; density of 0.99g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the Refractive index of 1.45n 25 D . Meets the industry standard of the high-boiling silicone oil of China fluorosilicone organic materials industry society T_FSI 007-2017.
Example 4:
the concentration of the first dilute hydrochloric acid is 1.5%, the volume ratio of the organic silicon high-boiling monomer to the first dilute hydrochloric acid is 1/1.6, the hydrolysis loop control temperature is 10 ℃, the outlet control pressure of the hydrolysis loop circulation pump 12 is 0.15MPa, and the top end of the hydrolysis loop distributor 15 is normal pressure. The temperature of the thermostatic delaminator 16 was controlled at 10 ℃. The water washing temperature is 70 ℃, and the alkaline washing temperature is 70 ℃. The lye is 15% sodium bicarbonate solution. The drying agent is light sodium carbonate solid, and the addition amount is 4% of the mass of the high-boiling silicone oil to be treated. Finally, the high-boiling silicone oil product is obtained after filtration in the filter tank 27.
The high-boiling silicone oil product obtained in this example was tested, and the test results were: the appearance is oily liquid, and no obvious mechanical impurities are visible; viscosity of 9mm 2 S; acid number (in KOH) 0.22mg/g; density of 0.96g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the Refractive index of 1.43n 25 D . The index of the acid value does not accord with the industry standard of the high-boiling silicone oil of the China fluorosilicone organic material industry association T_FSI 007-2017.
Example 5:
the concentration of the first dilute hydrochloric acid is 1.5%, the volume ratio of the organic silicon high-boiling monomer to the first dilute hydrochloric acid is 1/1.6, the hydrolysis loop control temperature is 10 ℃, the outlet control pressure of the hydrolysis loop circulation pump 12 is 0.15MPa, and the top end of the hydrolysis loop distributor 15 is normal pressure. The temperature of the thermostatic delaminator 16 was controlled at 10 ℃. The water washing temperature was 65℃and the alkaline washing temperature was 70 ℃. The lye is 15% sodium bicarbonate solution. The drying agent is light sodium carbonate solid, and the addition amount is 5% of the mass of the high-boiling silicone oil to be treated. Finally, the high-boiling silicone oil product is obtained after filtration in the filter tank 27.
The high-boiling silicone oil product obtained in this example was tested, and the test results were: the appearance is oily liquid, and no obvious mechanical impurities are visible; viscosity of 8.5mm 2 S; acid number (in KOH) 0.21mg/g; the density is 0.96g/cm3; refractive index of 1.42n 25 D . The index of acid value and refractive index does not accord with the industry standard of China fluorosilicone organic materials industry association T_FSI007-2017 high boiling silicone oil.
The embodiments of the invention are intended to embrace all such alternatives, modifications and variances which fall within the broad scope of the appended claims. Therefore, any omission, modification, equivalent replacement, improvement, etc. of the present invention should be included in the scope of the present invention.
Claims (10)
1. The production process of the high-boiling silicone oil is characterized by comprising the following steps of:
s1, introducing an organosilicon high-boiling monomer and first dilute hydrochloric acid into a loop hydrolysis unit in proportion to carry out mixed hydrolysis treatment to obtain a hydrolysis mixture;
s2, layering the hydrolysis mixture at constant temperature by using a layering device, and separating out first acidic high-boiling silicone oil and raw material concentrated hydrochloric acid;
s3, separating raw material concentrated hydrochloric acid to obtain second acidic high-boiling silicone oil and first concentrated hydrochloric acid;
s4, separating the first acidic high-boiling silicone oil from the second acidic high-boiling silicone oil to obtain second concentrated hydrochloric acid and pretreated acidic high-boiling silicone oil;
s5, washing the pretreated acidic high-boiling silicone oil to obtain second dilute hydrochloric acid and weak acidic high-boiling silicone oil;
s6, performing alkali washing treatment on the weak acid high-boiling silicone oil to obtain neutral high-boiling silicone oil and alkali liquor;
s7, drying and filtering the medium high-boiling silicone oil to obtain the finished product high-boiling silicone oil.
2. The production process of high-boiling silicone oil according to claim 1, wherein the concentration of the first dilute hydrochloric acid in S1 is 1-6%, and the volume ratio of the organic silicon high-boiling monomer to the first dilute hydrochloric acid is 1:1.6-2.5; the temperature of the hydrolysis treatment is controlled to be 10-45 ℃, and the pressure of a circulating pump outlet in the hydrolysis treatment is 0.15-0.20 MPa.
3. The process for producing high-boiling silicone oil according to claim 1, wherein the temperature of constant temperature delamination in S2 is controlled to be 10-30 ℃.
4. The process for producing high-boiling silicone oil according to claim 1, wherein the temperature of the water washing treatment in S5 is 70-85 ℃.
5. The process for producing high-boiling silicone oil according to claim 1, wherein the alkaline washing treatment in S6 is performed by using 15-25% sodium bicarbonate solution, and the alkaline washing treatment temperature is 70-85 ℃.
6. The process for producing high-boiling silicone oil according to claim 1, wherein in the drying and filtering treatment in S7, light sodium carbonate solid is adopted as a drying agent, and the mass of the light sodium carbonate solid is 5-8% of that of the neutral high-boiling silicone oil.
7. A high-boiling silicone oil production system according to the high-boiling silicone oil production process of any one of claims 1 to 6, comprising a dilute hydrochloric acid buffer tank, an organosilicon high-boiling monomer storage tank, a hydrolysis loop unit, a constant temperature delaminator, a concentrated acid phase separator, an acid-oil phase separator, a water-washing kettle, an alkaline-washing kettle, a delaminator, a drying kettle and a filtration tank; it is characterized in that the method comprises the steps of,
the dilute hydrochloric acid buffer tank discharge port and the organic silicon high-boiling monomer storage tank discharge port are respectively connected with the hydrolysis loop unit feed port, the hydrolysis loop unit discharge port is connected with the constant temperature layering device feed port, the two discharge ports of the constant temperature layering device are respectively connected with the concentrated acid phase separator feed port and the acid-oil phase separator feed port, the discharge port of the concentrated acid phase separator is connected with the acid-oil phase separator feed port, the acid-oil phase separator discharge port is connected with the water washing kettle feed port, the two discharge ports of the water washing kettle are respectively connected with the dilute hydrochloric acid buffer tank feed port and the alkaline washing kettle feed port, the alkaline washing kettle discharge port is connected with the layering device feed port, the layering device discharge port is connected with the drying kettle feed port, and the drying kettle discharge port is connected with the filter tank.
8. The high-boiling silicone oil production system according to claim 7, wherein the hydrolysis loop unit comprises a mixer, a circulating pump, a cooler, a reactor and a distributor, wherein a dilute hydrochloric acid buffer tank discharge port and an organosilicon high-boiling monomer storage tank discharge port are respectively connected with a mixer feed port, the mixer discharge port is connected with a circulating pump feed port, the circulating pump discharge port is connected with a cooler feed port, the cooler discharge port is connected with the reactor feed port, the reactor discharge port is connected with the distributor feed port, and two discharge ports of the distributor are respectively connected with the mixer feed port and a constant-temperature layering device feed port.
9. The high-boiling silicone oil production system according to claim 7, further comprising an alkali liquid tank, wherein an alkali liquid outlet is arranged on the layering device, the alkali liquid outlet is connected with a liquid inlet of the alkali liquid tank, and a liquid outlet of the alkali liquid tank is connected with a feed inlet of the alkali washing kettle.
10. The high-boiling silicone oil production system as set forth in claim 7, wherein the feed inlets of the water washing tank and the alkaline washing tank are respectively provided with a washing mixer.
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| US6225490B1 (en) * | 1997-05-28 | 2001-05-01 | Shin-Etsu Chemical Co., Ltd. | Continuous hydrolysis of organochlorosilanes |
| US20060074189A1 (en) * | 2004-10-05 | 2006-04-06 | Gammie Andrew B | Hydrolysis of chlorosilanes |
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| CN114470875A (en) * | 2022-03-10 | 2022-05-13 | 新疆西部合盛硅业有限公司 | Novel efficient high-boiling silicon oil phase separation system and process |
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| US6225490B1 (en) * | 1997-05-28 | 2001-05-01 | Shin-Etsu Chemical Co., Ltd. | Continuous hydrolysis of organochlorosilanes |
| US20060074189A1 (en) * | 2004-10-05 | 2006-04-06 | Gammie Andrew B | Hydrolysis of chlorosilanes |
| CN203728751U (en) * | 2014-01-29 | 2014-07-23 | 浙江合盛硅业有限公司 | Dimethyldichlorosilane continuously pressurized hydrolysis loop system |
| CN114470875A (en) * | 2022-03-10 | 2022-05-13 | 新疆西部合盛硅业有限公司 | Novel efficient high-boiling silicon oil phase separation system and process |
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