CN218089402U - Purification device of hexamethyldisiloxane - Google Patents
Purification device of hexamethyldisiloxane Download PDFInfo
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- CN218089402U CN218089402U CN202222399464.7U CN202222399464U CN218089402U CN 218089402 U CN218089402 U CN 218089402U CN 202222399464 U CN202222399464 U CN 202222399464U CN 218089402 U CN218089402 U CN 218089402U
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Abstract
A purification device for hexamethyldisiloxane is characterized in that a hexamethyldisiloxane storage tank system A1 is connected with a nanofiber membrane adsorption system F2; the nanofiber membrane adsorption system F2 is connected with the preheater H; the preheater H is connected with an overweight system G3; the overweight system G3 is connected with the anion exchange resin system Y4; the hexamethyldisiloxane storage tank system A1, the nanofiber membrane adsorption system F2, the preheater H and the overweight system G3 anion exchange resin system Y4 form a height drop from top to bottom. The utility model discloses a device and process method of purification of thick hexamethyldisiloxane, essential equipment move towards from top to bottom along the material and distribute, do not have high energy consumption rectification process energy consumption and hang down, and the equipment is long-pending little, and product purity is high, the water content is low.
Description
Technical Field
The utility model relates to a purification technology of crude hexamethyldisiloxane, which belongs to the technical field of chemical equipment and engineering technology.
Background
Hexamethyldisiloxane is an organic compound, colorless transparent liquid, having a flash point of-2 ℃, a melting point of-59 ℃, a boiling point of 101 ℃, a saturated vapor pressure of 5.6kPa (25 ℃) (the saturated vapor pressure of water is 3.1699 KPa,25 ℃), is insoluble in water, is soluble in most organic solvents, and is mainly used as a capping agent, a cleaning agent, a mold release agent, an organic synthesis intermediate and the like.
When hexamethyldisiloxane is used as an end-capping agent or modifier, the reason is that H 2 O is more active than hexamethyldisiloxane, H 2 O preferentially reacts with hydroxyl, alkoxy and other groups to influence the quality of the polymer; secondly, the chloride ion affects the activity of the acid-base catalyst, further affects the polymerization rate of the polymerization reaction, and increases the risk of equipment corrosion. CN101362777B, CN102617625B, CN103319519B, CN111004267A and the like in China are mainly purified by methods such as solid-liquid centrifugal separation and filtration, high-temperature distillation, inorganic salt water removal agent adsorption and the like. In particular to Chinese patent CN103951692B, trimethylchlorosilane is dripped into a reactor kettle containing water and one or more condensation catalysts of cation exchange resin, activated clay and zeolite, and the cation exchange resin is added in the hydrolysis processEtc., intended to promote the condensation of trimethylsilanol to hexamethyldisiloxane. However, the kettle contains a large amount of water, strong acids such as cation exchange resin are easy to lose and remain in hydrolysate, and the difficulty of chloride ion and wastewater treatment is increased.
Hexamethyldisiloxane, which is produced mainly by a trimethylchlorosilane hydrolysis method in the prior art, has high water content and chloride ion content, wherein the purity of the commercial product is 98.5-99.0 percent, the water content is more than 200ppm, and the chloride ion content is 20-50 mg/kg.
SUMMERY OF THE UTILITY MODEL
The utility model discloses aim at the weak point that product water content is higher, the purity is not high to public hexamethyldisiloxane MM production technology risk height, equipment are bulky and the market is sold, utility model relates to a device of the purification of safe low energy consumption, equipment is small, product moisture content is low thick hexamethyldisiloxane.
The utility model adopts the following technical scheme:
a purification device for hexamethyldisiloxane is characterized in that a hexamethyldisiloxane storage tank system A1 is connected with a nanofiber membrane adsorption system F2;
the nanofiber membrane adsorption system F2 is connected with the preheater H;
the preheater H is connected with an overweight system G3;
the overweight system G3 is connected with the anion exchange resin system Y4;
the hexamethyldisiloxane storage tank system A1, the nanofiber membrane adsorption system F2, the preheater H and the overweight system G3 anion exchange resin system Y4 form a height drop from top to bottom.
The hexamethyldisiloxane storage tank system A1 comprises two storage tanks connected in parallel, namely a hexamethyldisiloxane storage tank A1A and a hexamethyldisiloxane storage tank II A1B, wherein condensers, namely a condenser A1A-1 and a condenser II A1B-2, are arranged on the upper portions of the hexamethyldisiloxane storage tank A1A and the hexamethyldisiloxane storage tank II A1B. The operation temperature of the cooling medium of the condenser is-40 to 0 ℃, and preferably-20 to-5 ℃.
The nanofiber membrane adsorption system F2 comprises two adsorption storage tanks connected in parallel, namely a nanofiber membrane adsorption storage tank I F2A and a nanofiber membrane adsorption storage tank II F2B. Each set of nanofiber membrane is composed of a plurality of layers of nanofiber membranes, and each layer of nanofiber membrane is matched with a heating module.
The hypergravity system G3 comprises a heat-preservation storage tank G3-1 with a heating jacket and a low-molecular receiving tank G3-3, wherein the heat-preservation storage tank G3-1 with the heating jacket, a nanofiber membrane adsorption storage tank I F2A and a nanofiber membrane adsorption storage tank II F2B are respectively connected with the low-molecular receiving tank G3-3 through pipelines; the low molecular receiving tank G3-3 is provided with a vacuum pump G3-2.
The top of the low molecular receiving tank G3-3 is connected with a first condenser A1A-1 and a second condenser A1B-2;
the bottom is connected with a first condenser A1A-1 and a second condenser A1B-2 through a material transfer pump G3-3P.
The anion exchange resin system Y4 is connected with the first condenser A1A-1 and the second condenser A1B-2.
Through the technical scheme, the utility model discloses following technological effect has:
1. the separation and purification process of the crude hexamethyldisiloxane is safe, efficient and low in energy consumption, high-temperature and high-pressure are avoided, low-molecular tail gas is recycled, and material conveying mainly depends on gravity natural flow or micro-pressure conveying. The disclosed process method has high energy consumption for high-temperature rectification, high-altitude exhaust of tail gas and high safety risk.
2. The utility model discloses requirement to vacuum system is not high, owing to pack the porous filler of nanometer in the hypergravity system, becomes micron to nanometer's liquid film, liquid silk and liquid drop to liquid dispersion under huge shearing force, the increase and the ultrafast update of the more conventional stirring order of magnitude of phase interface, make the improvement 1 ~ 3 order of magnitude in the alternate mass transfer rate ratio traditional tower, the temperature and the vacuum that the phase separation needs all reduce by a wide margin.
3. The utility model discloses equipment is small, and under the hypergravity condition, the improvement 1 ~ 3 orders of magnitude in the alternate mass transfer rate ratio traditional tower, gaseous linear velocity increases substantially, and the production efficiency of unit equipment volume improves 1 ~ 2 orders of magnitude, and hypergravity equipment only is 1/5 ~ 1/10 of rectification tower volume.
Drawings
FIG. 1 is an equipment diagram of a purification device for hexamethyldisiloxane, which comprises a hexamethyldisiloxane storage tank system A1, a hexamethyldisiloxane storage tank A1A, a hexamethyldisiloxane storage tank II A1B, a condenser A1A-1, a condenser II A1B-2, a nanofiber membrane adsorption system F2, a nanofiber membrane adsorption storage tank F2A, a nanofiber membrane adsorption storage tank II F2B, a preheater H, an overweight system G3, a heat preservation storage tank G3-1 with a heating jacket, a vacuum pump G3-2, a low-molecular receiving tank G3-3 and an anion exchange resin system Y4.
Detailed Description
Example 1
A purification device for hexamethyldisiloxane is characterized in that a hexamethyldisiloxane storage tank system A1 is connected with a nanofiber membrane adsorption system F2;
the nanofiber membrane adsorption system F2 is connected with the preheater H;
the preheater H is connected with an overweight system G3;
the overweight system G3 is connected with an anion exchange resin system Y4;
the hexamethyldisiloxane storage tank system A1, the nanofiber membrane adsorption system F2, the preheater H and the overweight system G3 anion exchange resin system Y4 form a height drop from top to bottom.
The hexamethyldisiloxane storage tank system A1 comprises two storage tanks connected in parallel, namely a hexamethyldisiloxane storage tank A1A and a hexamethyldisiloxane storage tank II A1B, wherein condensers, namely a condenser A1A-1 and a condenser II A1B-2, are arranged on the upper portions of the hexamethyldisiloxane storage tank A1A and the hexamethyldisiloxane storage tank II A1B.
The nanofiber membrane adsorption system F2 comprises two adsorption storage tanks connected in parallel, namely a nanofiber membrane adsorption storage tank I F2A and a nanofiber membrane adsorption storage tank II F2B.
The hypergravity system G3 comprises a heat preservation storage tank G3-1 with a heating jacket and a low molecular receiving tank G3-3, wherein the heat preservation storage tank G3-1 with the heating jacket, a first nanofiber membrane adsorption storage tank F2A and a second nanofiber membrane adsorption storage tank F2B are respectively connected with the low molecular receiving tank G3-3 through pipelines; the low molecular receiving tank G3-3 is provided with a vacuum pump G3-2.
The top of the low molecular receiving tank G3-3 is connected with a first condenser A1A-1 and a second condenser A1B-2;
the bottom is connected with a first condenser A1A-1 and a second condenser A1B-2 through a material transfer pump G3-3P.
The anion exchange resin system Y4 is connected with the first condenser A1A-1 and the second condenser A1B-2.
Example 2
Selecting coarse MM with the purity of 95.0% as a starting raw material, starting a bottom valve A1A of a coarse MM-2 storage tank A by 10% of opening degree, starting a feed valve of a nanofiber membrane adsorption system F2A, starting a preheater H before entering a hypergravity system G3 to enable the temperature of the preheater H to be stabilized at 65 ℃, and starting the hypergravity system G3, a heating and heat-preserving module G3-1 and a vacuum pump G3-2;
the coarse MM-2 stays for 10min in a nanofiber membrane adsorption system F2A and then is MM-A2, the MM-A2 enters a 10G hypergravity system G3 after being preheated by a preheater H at the temperature of about 55-60 ℃, the vacuum degree in the G3 is maintained at-85 kpa, the material is extracted by negative pressure and enters a low molecular receiving tank G3-3, and the material after being processed by the hypergravity system is MM-C2; after partial storage of MM-C2, the feed valve of the anion exchange resin system Y4 is opened, and MM-C2 stays in Y4 for 10min to obtain MM-D2.MM-D2, the chroma is 2Hazen, the purity is 99.991%, the water content is 7ppm, and the chloride ion content is not detected through tests such as GC and potentiometric titration analysis.
Example 3
When the nanofiber membrane adsorption system F2A is used for 2 days or 8 batches of crude MM are processed, A1A or A1B is switched to be connected with F2B, the processing port is closed after the A1A material is completely discharged, a heating module matched with F2A is started, the temperature is set to be 85 ℃, a vacuum system F2-2 and a connecting valve with the nanofiber membrane adsorption system F2A are started, and negative pressure treatment is carried out for 10 hours. The balance was the same as in step 2, and the purified MM-D12 had a chroma of 3Hazen, a purity of 99.92%, a water content of 6ppm and a chloride ion content of 1ppm.
Claims (6)
1. The hexamethyldisiloxane purification device is characterized in that a hexamethyldisiloxane storage tank system (A1) is connected with a nanofiber membrane adsorption system (F2);
the nanofiber membrane adsorption system (F2) is connected with the preheater (H);
the preheater (H) is connected with the overweight system (G3);
the overweight system (G3) is connected with the anion exchange resin system (Y4);
the hexamethyldisiloxane storage tank system (A1), the nanofiber membrane adsorption system (F2), the preheater (H) and the overweight system (G3) are provided with an anion exchange resin system (Y4) which forms a height drop from top to bottom.
2. The purification device for hexamethyldisiloxane according to claim 1, wherein the hexamethyldisiloxane storage tank system (A1) comprises two parallel storage tanks, namely, a first hexamethyldisiloxane storage tank (A1A) and a second hexamethyldisiloxane storage tank (A1B), and condensers, namely, the first condenser (A1A-1) and the second condenser (A1B-2), are disposed on the upper portions of the first hexamethyldisiloxane storage tank (A1A) and the second hexamethyldisiloxane storage tank (A1B).
3. The hexamethyldisiloxane purification apparatus according to claim 2, wherein said nanofiber membrane adsorption system (F2) comprises two adsorption tanks connected in parallel, namely nanofiber membrane adsorption tank one (F2A) and nanofiber membrane adsorption tank two (F2B).
4. The hexamethyldisiloxane purification apparatus according to claim 3, wherein the overweight system (G3) comprises a thermal insulation storage tank (G3-1) with a heating jacket and a low molecular receiving tank (G3-3), wherein the thermal insulation storage tank (G3-1) with a heating jacket, the first nanofiber membrane adsorption storage tank (F2A) and the second nanofiber membrane adsorption storage tank (F2B) are respectively connected with the low molecular receiving tank (G3-3) through pipes; the low molecular receiving tank (G3-3) is provided with a vacuum pump (G3-2).
5. The hexamethyldisiloxane purification apparatus according to claim 4, wherein the top of the low molecular weight receiver tank (G3-3) is connected to the first condenser (A1A-1) and the second condenser (A1B-2);
the bottom is connected with a first condenser (A1A-1) and a second condenser (A1B-2) through a material transfer pump (G3-3P).
6. The hexamethyldisiloxane purification apparatus according to claim 2, wherein the anion exchange resin system (Y4) is connected to the first condenser (A1A-1) and the second condenser (A1B-2).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202222399464.7U CN218089402U (en) | 2022-09-09 | 2022-09-09 | Purification device of hexamethyldisiloxane |
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| CN202222399464.7U CN218089402U (en) | 2022-09-09 | 2022-09-09 | Purification device of hexamethyldisiloxane |
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