CN113683635B - 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 PDF

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Publication number
CN113683635B
CN113683635B CN202111024276.XA CN202111024276A CN113683635B CN 113683635 B CN113683635 B CN 113683635B CN 202111024276 A CN202111024276 A CN 202111024276A CN 113683635 B CN113683635 B CN 113683635B
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ceramic membrane
liquid
membrane
collecting tank
clear liquid
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CN113683635A (en
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何小敏
王涛
冯海杰
刘旭红
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Shanghai Saiao Separation Technology Engineering Co ltd
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Shanghai Saiao Separation Technology Engineering Co ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07FACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F7/00Compounds containing elements of Groups 4 or 14 of the Periodic Table
    • C07F7/02Silicon compounds
    • C07F7/08Compounds having one or more C—Si linkages
    • C07F7/0834Compounds having one or more O-Si linkage
    • C07F7/0838Compounds with one or more Si-O-Si sequences
    • C07F7/0872Preparation and treatment thereof
    • C07F7/089Treatments not covered by a preceding group
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D61/00Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D65/00Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
    • B01D65/02Membrane cleaning or sterilisation ; Membrane regeneration
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process 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 organosilicon synthesis, in particular to an application method of ceramic membrane technology in tetramethyl divinyl disiloxane production; the method comprises the following steps: the distilled liquid is pumped into a collecting tank, the distilled liquid in the collecting tank is pumped into a ceramic membrane filtering system, clear liquid filtered by the ceramic membrane filtering system flows into a clear liquid tank, and filtered concentrated liquid returns into the collecting tank; the relevant parameters of the ceramic membrane filtration system are as follows: the pore diameter of the ceramic membrane is 20-100nm, and the membrane flux is 500-800L/m 2 h, ceramic membrane outlet pressure is 0.1-0.2Mpa, transmembrane pressure difference is 0.05-0.2Mpa, and membrane surface flow rate is 4m/s.

Description

Application method of ceramic membrane technology in production of tetramethyl divinyl disiloxane
Technical Field
The invention relates to the technical field of organosilicon synthesis, in particular to an application method of ceramic membrane technology in tetramethyl divinyl disiloxane production.
Background
Tetramethyl divinyl disiloxane, chinese alias 1, 3-diethyl-1, 3-tetramethyl disiloxane; divinyl tetramethyl disiloxane; 1, 3-divinyl tetramethyl disiloxane; 1, 3-divinyl tetramethyl disiloxane; 1, 3-divinyl tetramethyl disiloxane; vinyl double seal head. The method is suitable for additives (intermediates) in the production process of addition type silicone rubber, silicone gel, liquid silica gel, vinyl silicone resin, vinyl silicone oil, platinum chromium compound and the like. In the existing production process of tetramethyl divinyl disiloxane, as shown in fig. 2, the reaction materials contain sodium chloride, ethanol, a single end socket and other raw materials, sodium chloride exists in a solid form, most of sodium chloride is evaporated to dryness in a distillation process, a small part of sodium chloride enters a collecting tank along with distilled liquid, two modes are generally adopted to avoid sodium chloride solids entering a downstream process before clear liquid enters the collecting tank, firstly, a filter bag is used for filtering part of sodium chloride, the sodium chloride passing through the filter bag is naturally settled again, namely, the collecting tank utilizes bottom feeding, and an upper overflow mode enters a clear liquid tank, and as the particle size of the sodium chloride solids in the system is small, the particle size of the sodium chloride is detected to be between 0.92 microns and 13.31 microns by a European and American particle size tester, the filter bag is very light, the sodium chloride solids are very difficult to settle down, and the sodium chloride solids enter a downstream process to cause the blockage of a rectifying tower, and the quality of a product is unacceptable.
In summary, the selection of a suitable filter is a significant task in this process, and typical filters are bag filters, candle filters, plate frame filters, cartridge filters, titanium rod filters, and the like. Such filters generally suffer from the following disadvantages: either the filtering precision can not meet the requirement, or when the filter element or the filter cloth is replaced, liquid is exposed to the air, and great potential safety hazards exist.
Therefore, in order to improve the quality and yield of tetramethyl divinyl disiloxane products, 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 needed.
Disclosure of Invention
In order to solve the technical problems, the invention provides an application method of ceramic membrane technology in the production of tetramethyl divinyl disiloxane.
The application method of the ceramic membrane technology in the production of tetramethyl divinyl disiloxane comprises the following steps:
the distilled liquid is pumped into a collecting tank, the distilled liquid in the collecting tank is pumped into a ceramic membrane filtering system, clear liquid filtered by the ceramic membrane filtering system flows into a clear liquid tank, and filtered concentrated liquid returns into the collecting tank;
the relevant parameters of the ceramic membrane filtration system are as follows: the pore diameter of the ceramic membrane is 20-100nm, and the membrane flux is 500-800L/m 2 h, ceramic membrane outlet pressure is 0.1-0.2Mpa, transmembrane pressure difference is 0.05-0.2Mpa, and membrane surface flow rate is 4m/s.
Further, before the ceramic membrane filtration system stops working, the clear liquid in the clear liquid tank is used for back flushing the ceramic membrane.
Compared with the prior art, the invention has the beneficial effects that: (1) The prior filtering equipment is abandoned, and the procedures of frequently replacing consumable materials such as filter bags, filter cloth, filter elements and the like are avoided;
(2) The service life of the ceramic membrane element is 3-5 years, so that leakage of feed liquid such as ethanol caused by frequent disassembly of the filtering equipment is avoided, and the safety of work is enhanced;
(3) The blockage of the packing of the rectifying tower and the blockage of the tube array in the downstream rectifying process are prevented, and the rectifying efficiency is improved;
(4) The sodium chloride solid in the system is trapped and concentrated in the collecting tank through the entrapment of the ceramic membrane filtration system instead of being left in each downstream process, so that slag is conveniently discharged, and the product quality of finished products in each downstream process is improved;
(5) The concentrated solution of the ceramic membrane system can be continuously returned to the distillation process, so that sodium chloride is recovered, clear liquid is recovered, and the utilization rate of 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, clean liquid tank, etc. of the present invention.
Detailed Description
The following describes in further detail the embodiments of the present invention with reference to the drawings and examples. The following examples are illustrative of the invention and 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 Langmuir film technologies Co., ltd;
ceramic membrane equipment: customizing Shanghai Saio separation technology engineering Co., ltd;
embodiment case 1:
(1) The distilled liquid is firstly fed into a collecting tank, and the liquid is the stock solution of the ceramic membrane filtration system;
(2) The pore diameter of the ceramic membrane is 20-100nm, and the membrane flux is 500-800L/m 2 h, the pressure of the membrane outlet is 0.1-0.2Mpa, and the transmembrane pressure difference is0.05-0.2MPa, and the flow rate of the membrane surface is 4m/s;
(3) The ceramic membrane is generally applied to the fields of food and biological fermentation, the ceramic membrane is creatively introduced into the production field of tetramethyl divinyl disiloxane, the characteristics of pollution resistance, high flux, good separation performance and long service life of the ceramic membrane are fully utilized, and sodium chloride in an ethanol system is efficiently separated;
(4) The turbidity of the liquid before ceramic membrane filtration is more than or equal to 3NTU, and the turbidity after filtration is less than or equal to 0.1NTU;
(5) And (5) before stopping each time, back flushing with ceramic membrane clear liquid for 1-2min for standby. The method comprises the steps of carrying out a first treatment on the surface of the
(6) The obtained clear liquid has low turbidity, meets the quality requirement of downstream working procedures, and solves the problems of blockage and unqualified quality in the prior process.
Embodiment case 2:
turbidity and concentration multiple
Collecting 20L distillate, concentrating 2 times, 3 times, 4 times, and 5 times respectively by ceramic membrane filtration system, collecting clear liquid and concentrated liquid, detecting turbidity, respectively obtaining 5 groups of data, continuously measuring for 3 days, and collecting the data as follows:
first day detection data:
the following day of test data:
third day test data:
the result shows that the turbidity of the clear liquid filtered by the ceramic membrane is always below 0.1NTU along with the increase of the concentration multiple of the membrane, and the good filtering performance is shown.
Embodiment 3:
relationship of recoil to flux
The experiment is a pilot experiment, the experiment site is used for 3 months continuously in the lead mountain industrial park, the detection data are sampled when the experiment site is just started to be used respectively, the detection data are sampled after 45 days, the detection data are sampled after 90 days, and the statistics are as follows:
data at the beginning of use:
membrane inlet pressure Mpa Pressure Mpa at membrane outlet Flux L/m 2 h
0.2 0.1 583
0.25 0.15 696
0.3 0.2 804
Data after 45 days of use:
membrane inlet pressure Mpa Pressure Mpa at membrane outlet Flux L/m 2 h
0.2 0.1 554
0.25 0.15 687
0.3 0.2 798
Data after 90 days of use:
membrane inlet pressure Mpa Pressure Mpa at membrane outlet 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 the clear liquid is used for washing for 1-2 minutes before shutdown. From the above data, the flux of the ceramic membrane is between 500 and 850, with a duration of 450h.
The foregoing is merely a preferred embodiment of the present invention, and it should be noted that it will be apparent to those skilled in the art that modifications and variations can be made without departing from the technical principles of the present invention, and these modifications and variations should also be regarded as the scope of the 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:
the distilled liquid is pumped into a collecting tank, the distilled liquid in the collecting tank is pumped into a ceramic membrane filtering system, clear liquid filtered by the ceramic membrane filtering system flows into a clear liquid tank, and filtered concentrated liquid returns into the collecting tank;
the relevant parameters of the ceramic membrane filtration system are as follows: the pore diameter of the ceramic membrane is 20-100nm, and the membrane flux is 500-800L/m 2 h, ceramic membrane outlet pressure is 0.1-0.2Mpa, transmembrane pressure difference is 0.05-0.2Mpa, and membrane surface flow rate is 4m/s.
2. The method for applying ceramic membrane technology in the production of tetramethyl divinyl disiloxane according to claim 1, wherein the ceramic membrane is backwashed with clear liquid in a clear liquid tank before the ceramic membrane filtration system is shut down.
CN202111024276.XA 2021-09-02 2021-09-02 Application method of ceramic membrane technology in production of tetramethyl divinyl disiloxane Active CN113683635B (en)

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Citations (11)

* Cited by examiner, † Cited by third party
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
JP2007283219A (en) * 2006-04-17 2007-11-01 Nitsukatoo:Kk Ceramic filter and manufacturing method thereof
CN101277967A (en) * 2005-09-29 2008-10-01 莫门蒂夫功能性材料公司 Process for the recovery of alkoxysilanes obtained from the direct reaction of silicon with alkanols
CN101792460A (en) * 2010-02-04 2010-08-04 南京工业大学 A kind of organochlorosilane production dry dust removal method
CN103055769A (en) * 2012-12-24 2013-04-24 南京工业大学 Organic silicon monomer fluidized bed membrane reactor and process thereof
CN103534012A (en) * 2011-04-08 2014-01-22 道康宁公司 Method of preparing gas selective membrane using epoxy-functional siloxanes
CN103797018A (en) * 2011-09-06 2014-05-14 Oci有限公司 Process for preparing trialkoxysilanes
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

Patent Citations (11)

* Cited by examiner, † Cited by third party
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
CN101277967A (en) * 2005-09-29 2008-10-01 莫门蒂夫功能性材料公司 Process for the recovery of alkoxysilanes obtained from the direct reaction of silicon with alkanols
JP2007283219A (en) * 2006-04-17 2007-11-01 Nitsukatoo:Kk Ceramic filter and manufacturing method thereof
CN101792460A (en) * 2010-02-04 2010-08-04 南京工业大学 A kind of organochlorosilane production dry dust removal method
CN103534012A (en) * 2011-04-08 2014-01-22 道康宁公司 Method of preparing gas selective membrane using epoxy-functional siloxanes
CN103797018A (en) * 2011-09-06 2014-05-14 Oci有限公司 Process for preparing trialkoxysilanes
CN103055769A (en) * 2012-12-24 2013-04-24 南京工业大学 Organic silicon monomer fluidized bed membrane reactor and process thereof
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

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