CN113683635A - Application method of ceramic membrane technology in production of tetramethyl divinyl disiloxane - Google Patents
Application method of ceramic membrane technology in production of tetramethyl divinyl disiloxane Download PDFInfo
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- CN113683635A CN113683635A CN202111024276.XA CN202111024276A CN113683635A CN 113683635 A CN113683635 A CN 113683635A CN 202111024276 A CN202111024276 A CN 202111024276A CN 113683635 A CN113683635 A CN 113683635A
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- ceramic membrane
- filtration system
- collection tank
- production
- membrane filtration
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- 239000012528 membrane Substances 0.000 title claims abstract description 42
- 239000000919 ceramic Substances 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 16
- 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 title claims abstract description 12
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 238000005516 engineering process Methods 0.000 title claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 25
- 238000005374 membrane filtration Methods 0.000 claims abstract description 15
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 230000004907 flux Effects 0.000 claims abstract description 7
- 238000005086 pumping Methods 0.000 claims abstract description 6
- 239000011148 porous material Substances 0.000 claims abstract description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 229910052710 silicon Inorganic materials 0.000 abstract description 2
- 239000010703 silicon Substances 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 32
- 239000011780 sodium chloride Substances 0.000 description 16
- 239000007787 solid Substances 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 238000001514 detection method Methods 0.000 description 3
- 238000011143 downstream manufacturing Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 3
- 229920002554 vinyl polymer Polymers 0.000 description 3
- 238000004821 distillation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000011001 backwashing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- FSIJKGMIQTVTNP-UHFFFAOYSA-N bis(ethenyl)-methyl-trimethylsilyloxysilane Chemical compound C[Si](C)(C)O[Si](C)(C=C)C=C FSIJKGMIQTVTNP-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- MMAADVOQRITKKL-UHFFFAOYSA-N chromium platinum Chemical compound [Cr].[Pt] MMAADVOQRITKKL-UHFFFAOYSA-N 0.000 description 1
- XODWWDLLPURTOQ-UHFFFAOYSA-N ethyl-[ethyl(dimethyl)silyl]oxy-dimethylsilane Chemical compound CC[Si](C)(C)O[Si](C)(C)CC XODWWDLLPURTOQ-UHFFFAOYSA-N 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000011020 pilot scale process Methods 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/0834—Compounds having one or more O-Si linkage
- C07F7/0838—Compounds with one or more Si-O-Si sequences
- C07F7/0872—Preparation and treatment thereof
- C07F7/089—Treatments not covered by a preceding group
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
- B01D65/02—Membrane cleaning or sterilisation ; Membrane regeneration
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Water Supply & Treatment (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention relates to the technical field of organic silicon synthesis, in particular to an application method of a ceramic membrane technology in the production of tetramethyl divinyl disiloxane; the method comprises the following steps: pumping the distillate into a collection tank, pumping the distillate in the collection tank into a ceramic membrane filtration system, filtering by the ceramic membrane filtration system, then enabling the clear liquid to flow into a clear liquid tank, and returning the filtered concentrated liquid to the collection tank; the ceramic membrane filtration system has the following relevant parameters: the ceramic membrane has a pore diameter of 20-100nm and a membrane flux of 500-800L/m2h, the outlet pressure of the ceramic membrane is 0.1-0.2Mpa, the transmembrane pressure difference is 0.05-0.2Mpa, and the flow rate of the membrane surface is 4 m/s.
Description
Technical Field
The invention relates to the technical field of organic silicon synthesis, in particular to an application method of a ceramic membrane technology in production of tetramethyl divinyl disiloxane.
Background
Tetramethyldivinyldisiloxane, the chinese alias 1, 3-diethyl-1, 1,3, 3-tetramethyldisiloxane; divinyltetramethyldisiloxane; 1, 3-divinyltetramethyldisiloxane; 1, 3-divinyltetramethyldioxane; 1, 3-divinyltetramethyldioxane; vinyl double seal head. The additive (intermediate) is suitable for the production processes of addition type silicone rubber, silicone gel, liquid silicone, vinyl silicone resin, vinyl silicone oil, platinum-chromium complex and the like. At present, the production process of tetramethyl divinyl disiloxane is shown in figure 2, reaction materials contain sodium chloride, ethanol, a single end enclosure and other raw materials, the sodium chloride exists in a solid form, most of the sodium chloride is evaporated to dryness in a distillation process, a small part of the sodium chloride enters a collecting tank along with distillate, two modes are generally adopted before clear liquid enters the collecting tank to prevent the sodium chloride solid from entering a downstream process, a filter bag is firstly used for filtering part of the sodium chloride, the sodium chloride penetrating through the filter bag is naturally settled, namely the collecting tank utilizes bottom feeding and upper overflow, the particle size of the sodium chloride solid in a system is very small, the particle size of the sodium chloride solid is between 0.92 microns and 13.31 microns detected by an Europe and America particle size tester, the filter cloth and other filtering methods of the filter bag are difficult to completely retain the sodium chloride solid, the sodium chloride solid is very light, and the liquid is slightly stirred, the solid is difficult to settle, so the sodium chloride solid can enter a downstream procedure again, the packing of the rectifying tower is blocked, the pipeline is blocked, and the product quality is unqualified.
In summary, the selection of a suitable filter becomes a significant task in this process, and typical filters are bag filters, candle filters, plate and frame filters, cartridge filters, titanium rod filters, and the like. Such filters generally suffer from the following disadvantages: or the filtration precision can not meet the requirement, or when the filter element or the filter cloth is replaced, liquid is exposed in the air, and great potential safety hazard exists.
Therefore, in order to improve the quality and yield of the product of the tetramethyldivinyldisiloxane, prevent the filler pipeline from being blocked and ensure the normal operation of the process, a high-efficiency and safe solid-liquid separation method is urgently needed.
Disclosure of Invention
In order to solve the technical problems, the invention provides an application method of a ceramic membrane technology in production of tetramethyl divinyl disiloxane.
The application method of the ceramic membrane technology in the production of the tetramethyl divinyl disiloxane comprises the following steps:
pumping the distillate into a collection tank, pumping the distillate in the collection tank into a ceramic membrane filtration system, filtering by the ceramic membrane filtration system, then enabling the clear liquid to flow into a clear liquid tank, and returning the filtered concentrated liquid to the collection tank;
the ceramic membrane filtration system has the following relevant parameters: the ceramic membrane has a pore diameter of 20-100nm and a membrane flux of 500-800L/m2h, the outlet pressure of the ceramic membrane is 0.1-0.2Mpa, the transmembrane pressure difference is 0.05-0.2Mpa, and the flow rate of the membrane surface is 4 m/s.
Further, before the ceramic membrane filtration system stops working, the clear liquid in the clear liquid tank is used for backwashing the ceramic membrane.
Compared with the prior art, the invention has the beneficial effects that: (1) the prior filtering equipment is abandoned, and the process of frequently replacing consumables such as a filter bag, filter cloth, a filter element and the like is avoided;
(2) the service life of the ceramic membrane element is 3-5 years, the leakage of feed liquid such as ethanol and the like caused by frequently disassembling the filtering equipment is avoided, and the working safety is enhanced;
(3) the packing of the rectifying tower and the tube nest in the downstream rectifying process are prevented from being blocked, and the rectifying efficiency is improved;
(4) by the interception of the ceramic membrane filtration system, sodium chloride solids in the system are intercepted and concentrated in the collection tank instead of being left in each downstream process, so that slag is conveniently discharged, and the product quality of each downstream process including finished products is improved;
(5) the concentrated solution of the ceramic membrane system can continuously return to the distillation process, so that the sodium chloride and the clear solution are recovered, and the utilization rate of the raw materials is improved.
Drawings
FIG. 1 is a flow chart of the present invention;
FIG. 2 is a flow chart of the prior art;
FIG. 3 is a flow chart of the collection tank, ceramic membrane and clear liquid tank of the present invention.
Detailed Description
The following detailed description of embodiments of the present invention is provided in connection with the accompanying drawings and examples. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Description of the materials involved in the following examples:
ceramic membrane element: 20-100nm, Shanghai Langmuim science and technology, Inc.;
ceramic membrane equipment: customization, shanghai seoi separation technology engineering ltd;
example 1:
(1) the distillate firstly enters a collecting tank, and the liquid is the stock solution of the ceramic membrane filtration system;
(2) the ceramic membrane has a pore diameter of 20-100nm and a membrane flux of 500-800L/m2h, the membrane outlet pressure is 0.1-0.2MPa, the transmembrane pressure difference is 0.05-0.2MPa, and the membrane surface flow rate is 4 m/s;
(3) the ceramic membrane is generally applied to the fields of food and biological fermentation, is creatively introduced into the production field of tetramethyl divinyl disiloxane, fully utilizes the characteristics of pollution resistance, high flux, good separation performance and long service life of the ceramic membrane, and efficiently separates sodium chloride in an ethanol system;
(4) the turbidity of the liquid before the ceramic membrane filtration is more than or equal to 3NTU, and the turbidity after the filtration is less than or equal to 0.1 NTU;
(5) and (4) backflushing with the clear liquid of the ceramic membrane for 1-2min for later use before finishing each time. (ii) a
(6) The obtained clear liquid has low turbidity, meets the quality requirement of downstream procedures and solves the problems of blockage and unqualified quality in the prior art.
Example 2:
turbidity and concentration factor
Taking 20L of distillate, concentrating with ceramic membrane filtration system for 2 times, 3 times, 4 times, and 5 times respectively, taking clear liquid and concentrated solution to detect turbidity, respectively obtaining 5 groups of data, continuously measuring for 3 days, and counting the data as follows:
data detected on the first day:
the data detected the next day:
and (3) detecting data on the third day:
the results show that the turbidity of the clear liquid filtered by the ceramic membrane is always below 0.1NTU as the concentration multiple of the membrane is increased and the content of sodium chloride is increased, thereby showing good filtering performance.
Example 3:
recoil to flux relationship
This experiment is the pilot scale experiment, and the experiment place is in the lead mountain industry garden, uses 3 months in succession, and sample detection data when just beginning to use respectively uses 45 days later sample detection data, uses 90 days later sample detection data, and the statistics is as follows:
start of use data:
| membrane inlet pressure Mpa | Membrane outlet pressure Mpa | Flux L/m2h |
| 0.2 | 0.1 | 583 |
| 0.25 | 0.15 | 696 |
| 0.3 | 0.2 | 804 |
Data after 45 days used:
| membrane inlet pressure Mpa | Membrane outlet pressure Mpa | Flux L/m2h |
| 0.2 | 0.1 | 554 |
| 0.25 | 0.15 | 687 |
| 0.3 | 0.2 | 798 |
Data after 90 days use:
| membrane inlet pressure Mpa | Membrane outlet pressure Mpa | Flux L/m2h |
| 0.2 | 0.1 | 532 |
| 0.25 | 0.15 | 650 |
| 0.3 | 0.2 | 785 |
The experimental equipment is used for about 10 hours every day, and is washed for 1-2 minutes by clear liquid before stopping the machine. From the above data, the flux of the ceramic membrane was between 500-.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (2)
1. The application method of the ceramic membrane technology in the production of tetramethyl divinyl disiloxane is characterized by comprising the following steps:
pumping the distillate into a collection tank, pumping the distillate in the collection tank into a ceramic membrane filtration system, filtering by the ceramic membrane filtration system, then enabling the clear liquid to flow into a clear liquid tank, and returning the filtered concentrated liquid to the collection tank;
the ceramic membrane filtration system has the following relevant parameters: the ceramic membrane has a pore diameter of 20-100nm and a membrane flux of 500-800L/m2h, the outlet pressure of the ceramic membrane is 0.1-0.2Mpa, the transmembrane pressure difference is 0.05-0.2Mpa, and the flow rate of the membrane surface is 4 m/s.
2. The method of claim 1, wherein the ceramic membrane is backwashed with a clear solution from a clear solution tank before the ceramic membrane filtration system is shut down.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111024276.XA CN113683635B (en) | 2021-09-02 | 2021-09-02 | Application method of ceramic membrane technology in production of tetramethyl divinyl disiloxane |
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|---|---|---|---|
| CN202111024276.XA CN113683635B (en) | 2021-09-02 | 2021-09-02 | Application method of ceramic membrane technology in production of tetramethyl divinyl disiloxane |
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| Publication Number | Publication Date |
|---|---|
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| CN113683635B CN113683635B (en) | 2024-03-26 |
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|---|---|---|---|---|
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| CN101792460A (en) * | 2010-02-04 | 2010-08-04 | 南京工业大学 | Dry-process dust removal method for organochlorosilane production |
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| CN103534012A (en) * | 2011-04-08 | 2014-01-22 | 道康宁公司 | Method of preparing gas selective membrane using epoxy-functional siloxanes |
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| WO2017096569A1 (en) * | 2015-12-07 | 2017-06-15 | 江苏久吾高科技股份有限公司 | Method and apparatus for treating fracturing flowback of oil-gas field by using ceramic membrane |
| CN111363126A (en) * | 2020-04-29 | 2020-07-03 | 南京钛净流体技术有限公司 | Ceramic membrane reactor and method for extracting polyhydroxyalkanoate by using ceramic membrane reactor |
-
2021
- 2021-09-02 CN CN202111024276.XA patent/CN113683635B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB856371A (en) * | 1958-02-18 | 1960-12-14 | American Oil Co | Process of separating an azeotropic mixture |
| CN1243127A (en) * | 1998-04-02 | 2000-02-02 | 韦特科公司 | Method for removing dissolved silicate from solvent directly synthesized from alcohol-silicon |
| RU2214362C1 (en) * | 2002-07-19 | 2003-10-20 | Федеральное государственное унитарное предприятие "Государственный научно-исследовательский институт химии и технологии элементоорганических соединений" | Method of production of high-purity monosilane |
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| CN103797018A (en) * | 2011-09-06 | 2014-05-14 | Oci有限公司 | Method for preparing trialkoxysilane |
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| CN113683635B (en) | 2024-03-26 |
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