CN112358616A - Process method for removing residual chlorine at terminal hydroxyl of polysiloxane hydrolysate - Google Patents
Process method for removing residual chlorine at terminal hydroxyl of polysiloxane hydrolysate Download PDFInfo
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- CN112358616A CN112358616A CN202010730719.6A CN202010730719A CN112358616A CN 112358616 A CN112358616 A CN 112358616A CN 202010730719 A CN202010730719 A CN 202010730719A CN 112358616 A CN112358616 A CN 112358616A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/32—Post-polymerisation treatment
- C08G77/34—Purification
Abstract
The invention relates to the technical field of organic silicon, in particular to a process for removing residual chlorine at hydroxyl groups at terminals of polysiloxane hydrolysate, which comprises a hydrolysate buffer tank, a membrane filter, a hydrolysate feeding pump, a static mixer, an oil-water separator, a hydrolysate product tank and other equipment, wherein the process comprises the steps of adopting a membrane filtration static mixing coalescence separation process method to filter chlorine-containing polysiloxane by a membrane, adopting micron-sized filtration precision to separate water molecules containing siloxane, the materials added with pure water and separated from the siloxane containing chlorine are sent to a static mixer, the two materials are fully mixed and absorbed by the static mixer and enter an oil-water separator device for separating an oil phase from a water phase, the oil-water separator adopts a combined separation structure, the oil phase discharged from the upper part obtains polysiloxane hydrolysate with the hydroxyl chlorine content of less than 5PPm, and the water phase discharged from the bottom part contains the siloxane with the hydroxyl chlorine content of less than 5PPm and enters a hydrolysis section to be used as supplementary water.
Description
Technical Field
The invention relates to the technical field of organic silicon, in particular to a process method for removing residual chlorine at the hydroxyl end of polysiloxane hydrolysate.
Background
The organosilicon production process usually adopts a direct method to synthesize methyl chlorosilane, namely a method for producing methyl chlorosilane mixed monomer by reacting silicon powder and chloromethane gas under a copper catalytic system. The dimethyl dichlorosilane and other refined monomers are obtained by rectifying and separating the synthesized mixed methyl monomer, and the dimethyl dichlorosilane is hydrolyzed, cracked, rectified and the like to prepare polysiloxane which is a basic raw material for further processing products of various organic silicon polymers.
Hydrolysate (polysiloxane) of dimethyldichlorosilane is an important intermediate in the organosilicon industry, and the polysiloxane generated after hydrolysis is a main raw material for producing a series of downstream products of organosilicon. Can be directly used for preparing alpha, omega-dihydroxy polydimethylsiloxane (107 silicon rubber) or dimethyl cyclosiloxane mixture (DMC) prepared by cracking, and further preparing products such as silicone oil, silicon rubber, silicon resin and the like.
Polysiloxanes (hydrolysates) are usually prepared by concentrated acid hydrolysis processes, where the polysiloxanes contain chlorine in amounts which have a significant adverse effect on the quality of the product downstream of the production.
The chlorine of the initial polysiloxane prepared by hydrolysis of the dimethyldichlorosilane exists in two forms, one is CL-CL (structural chlorine), the other is free chlorine CL-, and the dechlorination process needs to gradually remove the chlorine in the form, so that the hydrolysate polysiloxane with the chloride ion content of less than 5PPM is finally obtained.
At present, there are several process methods for removing chlorine content from organosilicon hydrolysate (polysiloxane);
the acidic polysiloxane is subjected to alkali washing and water washing to remove chloride ions, and the method inevitably generates a large amount of waste alkali liquor, waste water discharge and the like, so that environmental pollution and material loss are caused.
Acidic polysiloxane is subjected to a multistage countercurrent mixing washing process, and a large amount of deionized water is adopted for extracting a solvent, so that a large amount of low-concentration acidic wastewater can be generated.
The acidic polysiloxane is subjected to a method of evaporation and steam stripping, partial chloride ions are taken away by heating and evaporating the moisture of hydrolysate, and the chloride ions in the polysiloxane hydrolysate are stripped in a countercurrent mode by adopting a stripping tower to obtain a finished product. Therefore, there is a need to provide a method for removing residual chlorine at the terminal hydroxyl group of polysiloxane hydrolyzate to solve the above technical problems.
The documents relating to the removal of chlorine from polysiloxanes are as follows;
CN101323666A discloses a combined steam column and phase separator dechlorination method.
CN101817505A discloses a method for removing chloride ions by water washing, neutralization and water washing.
CN102002163A discloses a multistage countercurrent mixing separation method for removing chloride ions.
CN103214508A discloses a process for dechlorinating hydrolysate by five-stage counter-current washing of concentrated acid hydrolysis.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a process method for removing residual chlorine at the terminal hydroxyl of polysiloxane hydrolysate, which adopts a membrane separation static mixing coalescence separation process, and the content of the obtained product terminal hydroxyl chlorine is less than 5 PPm. The method comprises a process for removing residual chlorine at the hydroxyl end of hydrolysate after concentrated acid hydrolysis and azeotropic acid hydrolysis, and has the advantages that the prepared polysiloxane hydrolysate does not need to be cracked, downstream products are directly processed to prepare alpha, omega-dihydroxy polydimethylsiloxane (107 glue), and a process system is combined and configured according to the initial chlorine content of the hydrolyzed chlorine-containing polysiloxane and the chlorine index of a finished product. Currently, the chlorine content of hydrolysate polysilane is about 1000 ppm.
The technical scheme adopted by the invention for solving the technical problems is as follows: a process for removing residual chlorine from the end hydroxyl groups of polysiloxane hydrolyzate includes such steps as buffering tank, membrane filter, hydrolyzate feeding pump, static mixer, oil-water separator, and hydrolyzing tank. The preparation method comprises the following steps: the method adopts a membrane dispersion static mixing coalescence separation process, chlorine-containing polysiloxane is subjected to membrane separation and filtration, micro-molecules of the chlorine-containing siloxane are dispersed by adopting micron-sized filtration precision, deionized water and materials for dispersing the chlorine-containing siloxane are added and sent to a static mixer, the two materials are fully mixed by the static mixer and enter oil-water separator equipment for separating an oil phase from a water phase, the oil-water separator adopts a combined separation structure, the oil phase discharged from the upper part of the oil-water separator obtains the organopolysiloxane with the chlorine content of less than 5PPm, the organopolysiloxane enters a product collection tank, and the water phase discharged from the bottom of the oil-water separator returns to a hydrolysis working section to.
The invention is further configured to: the membrane filter adopts an inner part with precise micron-sized filtering precision and adopts a mode of feeding from outside to inside, so that the small molecules of the chloro-siloxane are fully dispersed, and the water-in-oil of the siloxane is fully separated.
The invention is further configured to: the static mixer adopts a pipeline form, the internal parts are provided with mixed fillers, the selection of the dispersion degree needs to ensure that liquid and liquid are fully mixed, and the emulsification phenomenon cannot be formed.
The invention is further configured to: the oil-water separator adopts a combined separating mechanism and a coalescence-separation structure, adopts modified fiber materials to coalesce very small oil drops, adopts hydrophobic materials to separate the water phase of the oil phase, and is designed with a separating structure device of the oil phase (light phase) and the water phase (heavy phase).
The invention is further configured to: the oil-water separation adopts an internal part structure form, a feeding distributor, a coalescence filler, a coarse-fine separation filler, an oil-water two-phase separation device and the like.
The invention is further configured to: the mass ratio of the chlorine-containing hydrolysate polysiloxane to the supplement soft water is 7: 1.
The invention is further configured to: wherein the quality requirement of the soft water is supplemented, and the hardness of the soft water reaches less than or equal to 0.03 mmol/L.
The invention is further configured to: the mixed dispersed particle size of the static mixer adopts a structural form of 1-20 microns.
The invention is further configured to: the retention time of the mixed liquid of the chlorine-containing siloxane and the soft water after the membrane separation in the static mixer is at least 180s, the mixing time is prolonged, and the chlorine-containing siloxane and the soft water are fully mixed and absorbed.
The invention is further configured to: the content of chlorine in the siloxane in the oil phase separated by the oil-water separator is controlled to be less than 5ppm, and the content of siloxane in the water phase is less than 5 ppm.
The invention is further configured to: the mixing temperature of the static mixer is controlled to be 60-70 degrees, the temperature of the oil-water separator is controlled to be about 60 degrees, and the pressure is controlled to be 0.05 MPa.
The invention is further configured to: the method mainly comprises the following steps:
(1) sending the mixture of hydrolyzed chlorine-containing polysiloxane to an intermediate buffer tank;
(2) pumping the chlorine-containing polysiloxane in the buffer tank into a membrane filter by a pump for separation, and removing impurities and alkali glue particles;
(3) returning the impurities discharged by the membrane filtration separator to a collecting tank for centralized treatment;
(4) mixing the clean chlorine-containing siloxane subjected to membrane separation with soft water, and feeding the mixture into a static mixer;
(5) the filler in the static mixer is fully mixed and enters the oil-water separator equipment;
(6) the mixed liquid enters an oil-water separation device through a feeding pipe distributor, passes through a coalescence filler and a coarse-fine separation filler, and then enters a separation space to carry out oil-water two-phase separation;
(7) the less than 5PPM chlorine polysiloxane discharged from the upper part of the oil-water separator separation space enters a product tank;
(8) the lower part of the oil-water separator separation space discharges an aqueous phase containing less than 5PPM siloxane and enters a hydrolysis section.
The invention is further configured to: the technological process is based on the purification and separation of the quality of the polysiloxane hydrolysate, and the equipment comprises: the device comprises a chlorine-containing siloxane buffer tank, a feeding pump, a membrane filter, a static mixer, an oil-water separator, a siloxane product tank and an impurity collecting tank.
The invention is further configured to: the import intercommunication of hydrolysate buffer tank and hydrolysate charge pump, hydrolysate charge pump export and membrane filter intercommunication, membrane filter separator lateral part mouth of pipe and static mixer intercommunication, it is connected with static mixer upper portion to supply soft water pipeline, static mixer lower part discharge gate and oil water separator charge-in pipeline are connected, oil water separator export upper portion and hydrolysate finished product jar are connected, oil water separator export lower part drainage pipe and hydrolysis system are connected, the bottom and the hydrolysate finished product charge-in pump pipe connection of hydrolysate finished product jar, hydrolysate finished product charge-in pump exit linkage packaging system connects.
The invention is further configured to: and (3) pumping the chlorine-containing polysiloxane in the hydrolysis buffer tank in the step (2) into a membrane filter for separation by a pump, removing impurities and alkali glue particles, and separating by using a micron-size material according to a membrane separation principle to disperse polysiloxane water molecules.
The invention is further configured to: and (4) mixing the clean chlorine-containing siloxane subjected to membrane separation with soft water, and feeding the mixture into a static mixer, wherein the dispersed particle size of the static mixer adopts a structural form of 1-20 microns, and fully mixing and absorbing.
The invention is further configured to: and (5) the mixed liquid enters oil-water separation equipment through a feeding pipe distributor, passes through coalescence filler and coarse-fine separation filler, and then enters a separation space to carry out oil-water two-phase separation.
The invention has the beneficial effects that:
(1) the invention provides a process method for removing residual chlorine at the hydroxyl end of polysiloxane hydrolysate, which aims at the problem defects in the prior art, and adopts a membrane separation static mixing coalescence separation process, so that the content of the obtained product of the residual chlorine at the hydroxyl end is less than 5 PPm;
(2) the process method for removing residual chlorine at the hydroxyl end of the polysiloxane hydrolysate has the advantages that the prepared polysiloxane hydrolysate does not need to be cracked, downstream products are directly processed to prepare alpha, omega-dihydroxy polydimethylsiloxane (107 glue), and a process system is combined and configured according to the initial chlorine content of the hydrolyzed chlorine-containing polysiloxane and the chlorine index of the finished product.
Drawings
The invention is further illustrated with reference to the following figures and examples.
FIG. 1 is a schematic structural diagram of a preferred embodiment of the method for removing residual chlorine at the hydroxyl end of polysiloxane hydrolyzate provided by the present invention.
In the figure: 1. a hydrolysate buffer tank; 2. a hydrolysate feed pump; 3. a membrane filter; 4. a static mixer; 5. an oil-water separator; 6. a hydrolysate finished product tank; 7. a hydrolysate finished product feeding pump; 8. an impurity collecting tank.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
As shown in figure 1, the process for removing residual chlorine at the terminal hydroxyl group of polysiloxane hydrolysate comprises a hydrolysate buffer tank, a membrane filter, a hydrolysate feeding pump, a static mixer, an oil-water separator, a hydrolysate tank and the like. The preparation method comprises the following steps: the method adopts a membrane dispersion static mixing coalescence separation process, chlorine-containing polysiloxane is subjected to membrane separation and filtration, micro-molecules of the chlorine-containing siloxane are dispersed by adopting micron-sized filtration precision, deionized water and materials for dispersing the chlorine-containing siloxane are added and sent to a static mixer, the two materials are fully mixed by the static mixer and enter oil-water separator equipment for separating an oil phase from a water phase, the oil-water separator adopts a combined separation structure, the oil phase discharged from the upper part of the oil-water separator obtains the organopolysiloxane with the chlorine content of less than 5PPm, the organopolysiloxane enters a product collection tank, and the water phase discharged from the bottom of the oil-water separator returns to a hydrolysis working section to.
Furthermore, the membrane filter adopts an inner part with precise micron-sized filtering precision, and adopts a mode of feeding from outside to inside to fully disperse the small molecules containing the chloro-siloxane, so that the water-in-oil of the siloxane is fully separated.
Furthermore, the form of the static mixer adopts a pipeline form, the internal parts are provided with mixed fillers, the selection of the dispersion degree needs to ensure that liquid and liquid are fully mixed, and the emulsification phenomenon cannot be formed.
Furthermore, the oil-water separator adopts a combined separation mechanism and a coalescence-separation structure, adopts modified fiber materials to coalesce small oil drops, adopts hydrophobic materials to separate the water phase of the oil phase, and is provided with separation structure equipment of the oil phase (light phase) and the water phase (heavy phase).
Furthermore, the oil-water separation internal part adopts a feed distributor, a coalescence filler, a coarse-fine separation filler, an oil-water two-phase separation device and the like.
Further, the mass ratio of the chlorine-containing hydrolysate polysiloxane to the supplementary soft water is 7: 1.
Furthermore, the quality requirement of supplementing soft water is that the hardness of the soft water reaches less than or equal to 0.03 mmol/L.
Further, the mixing and dispersing particle size of the static mixer adopts a structural form of 1-20 microns.
Furthermore, the retention time of the mixed liquid of the chlorine-containing siloxane and the soft water after membrane separation in the static mixer is at least 180s, the mixing time is prolonged, and the chlorine-containing siloxane and the soft water are fully mixed and absorbed.
Furthermore, the content of chlorine in the siloxane in the oil phase separated by the oil-water separator is controlled to be less than 5ppm, and the content of siloxane in the water phase is controlled to be less than 5 ppm.
Further, the mixing temperature of the static mixer is controlled to be 60-70 degrees, the temperature of the oil-water separator is controlled to be about 60 degrees, and the pressure is controlled to be 0.05 MPa.
Further, the process flow is based on the purification and separation of the quality of the polysiloxane hydrolyzate, and the equipment comprises: the device comprises a chlorine-containing siloxane buffer tank, a feeding pump, a membrane filter, a static mixer, an oil-water separator, a siloxane product tank and an impurity collecting tank.
Further, the import intercommunication of hydrolysate buffer tank 1 and hydrolysate charge pump 2, 2 exports of hydrolysate charge pump and membrane filter 3 intercommunication, 3 lateral part mouths of tubes and the 4 intercommunications of static mixer of membrane filtration separator, it is connected with 4 upper portions of static mixer to supply soft water pipeline, 4 lower part discharge gates of static mixer are connected with 5 feed line of oil water separator, 5 export upper portions of oil water separator are connected with hydrolysate finished product jar 6, 5 export lower part drainage pipe of oil water separator are connected with the system of hydrolysising, the bottom and the 7 pipe connection of hydrolysate finished product charge pump of hydrolysate finished product jar 6, 7 exit linkage packing system of hydrolysate finished product charge pump are connected.
Further, the chlorine-containing polysiloxane in the hydrolysis buffer tank in the step (2) is pumped into a membrane filter for separation by a pump to remove impurities and alkali glue particles, and the water molecules of the polysiloxane are dispersed by adopting the separation principle of a micron-size material by adopting a membrane separation principle.
Further, the clean chlorine-containing siloxane subjected to membrane separation in the step (4) and soft water are mixed and enter a static mixer, and the dispersed particle size of the static mixer adopts a structural form of 1-20 microns for full mixing and absorption.
And (3) further, the mixed liquid obtained in the step (5) enters oil-water separation equipment through a feeding pipe distributor, passes through a coalescence filler and a coarse-fine separation filler, and then enters a separation space for oil-water two-phase separation.
The working principle of the process method for removing the residual chlorine at the hydroxyl end of the polysiloxane hydrolysate is as follows:
firstly, moving the equipment to a position required by a user, and sending the mixture of the hydrolyzed chlorine-containing polysiloxane to an intermediate buffer tank; pumping the chlorine-containing polysiloxane in the buffer tank into a membrane filter by a pump for separation, and removing impurities and alkali glue particles; returning the impurities discharged by the membrane filtration separator to a collecting tank for centralized treatment; mixing the clean chlorine-containing siloxane subjected to membrane separation with soft water, and feeding the mixture into a static mixer; the filler in the static mixer is fully mixed and enters the oil-water separator equipment; the mixed liquid enters an oil-water separation device through a feeding pipe distributor, passes through a coalescence filler and a coarse-fine separation filler, and then enters a separation space to carry out oil-water two-phase separation; the less than 5PPM chlorine polysiloxane discharged from the upper part of the oil-water separator separation space enters a product tank; the lower part of the oil-water separator separation space discharges an aqueous phase containing less than 5PPM siloxane and enters a hydrolysis section.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "disposed," "mounted," "connected," and "fixed" are to be construed broadly, e.g., as meaning either fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art through specific situations.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and the embodiments and descriptions given above are only illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. A process for removing residual chlorine at the terminal hydroxyl of polysiloxane hydrolysate comprises the following steps: including equipment such as hydrolysate buffer tank, membrane filter, hydrolysate charge pump, static mixer, oil water separator are constituteed, hydrolysate product jar worker, its characterized in that: the process method for removing the residual chlorine at the hydroxyl group of the polysiloxane adopts a static mixing coalescence separation process system and a membrane separation static mixing coalescence separation process, chlorine-containing polysiloxane is subjected to membrane separation and filtration, micro-scale filtration precision is adopted to separate the micromolecules of the chlorine-containing siloxane, pure water is added and the materials for separating the chlorine-containing siloxane are sent to a static mixer, the two materials are fully mixed by the static mixer and enter an oil-water separator device for separating an oil phase from a water phase, the oil-water separator adopts a combined separation structure, the oil phase discharged from the upper part of the oil separator device obtains the organopolysiloxane with the chlorine content of less than 5PPm, the organopolysiloxane enters a product collection tank, and the water phase discharged from the bottom of the oil separator device returns to.
2. The process of claim 1, wherein the removal of residual chlorine at the hydroxyl end of the polysiloxane hydrolyzate comprises: the method mainly comprises the following steps:
(1) sending the mixture of the chlorine-containing polysiloxane to an intermediate buffer tank;
(2) pumping the chlorine-containing polysiloxane in the buffer tank into a membrane filter by a pump for separation, and removing impurities and alkali glue particles;
(3) returning the impurities discharged by the membrane filtration separator to a collecting tank for centralized treatment;
(4) mixing the clean chlorine-containing siloxane subjected to membrane separation with soft water, and feeding the mixture into a static mixer;
(5) the filler in the static mixer is fully mixed and enters the oil-water separator equipment;
(6) the mixed liquid enters an oil-water separation device through a feeding pipe distributor, passes through a coalescence filler and a coarse-fine separation filler, and then enters a separation space to carry out oil-water two-phase separation;
(7) the less than 5PPM chlorine polysiloxane discharged from the upper part of the oil-water separator separation space enters a product tank;
(8) the lower part of the oil-water separator separation space discharges an aqueous phase containing less than 5PPM siloxane and enters a hydrolysis section.
3. The process of claim 1, wherein the removal of residual chlorine at the hydroxyl end of the polysiloxane hydrolyzate comprises: the membrane filter structure adopts an inner part with precise micron-sized filtering precision, adopts a mode of entering from outside to inside, and fully disperses the water molecules of the chloro-siloxane, so that the water-in-oil of the siloxane is fully separated.
4. The process of claim 1, wherein the removal of residual chlorine at the hydroxyl end of the polysiloxane hydrolyzate comprises: the static mixer has mixing stuffing inside the mixer, and has dispersed particle size of 1-20 micron and dispersion degree required to ensure the liquid-liquid mixing.
5. The process of claim 1, wherein the removal of residual chlorine at the hydroxyl end of the polysiloxane hydrolyzate comprises: the oil-water separation adopts an internal part structure form, a feeding distributor, a coalescence filler, a coarse-fine separation filler, an oil-water two-phase separation device and the like.
6. The process of claim 1, wherein the removal of residual chlorine at the hydroxyl end of the polysiloxane hydrolyzate comprises: the mass ratio of the chlorine-containing hydrolysate polysiloxane to the supplementary soft water is 7:1, wherein the quality requirement of the supplementary soft water is that the hardness of the soft water reaches less than or equal to 0.03 mmol/L.
7. The process of claim 1, wherein the removal of residual chlorine at the hydroxyl end of the polysiloxane hydrolyzate comprises: the retention time of the mixed liquid of the chlorine-containing siloxane and the soft water after the membrane separation in the static mixer is at least 180s, the mixing time is prolonged, and the chlorine-containing siloxane and the soft water are fully mixed and absorbed.
8. The process of claim 1, wherein the removal of residual chlorine at the hydroxyl end of the polysiloxane hydrolyzate comprises: the mixing temperature of the static mixer is controlled to be 60-70 degrees, the temperature of the oil-water separator is controlled to be about 60 degrees, and the pressure is controlled to be 0.05 MPa.
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| WO2022213890A1 (en) * | 2021-04-09 | 2022-10-13 | 江西蓝星星火有机硅有限公司 | Process for producing organosilicon linear body |
| CN113617061A (en) * | 2021-07-27 | 2021-11-09 | 合盛硅业(鄯善)有限公司 | Method for treating methyl chlorosilane hydrolytic emulsion |
| CN113617061B (en) * | 2021-07-27 | 2022-12-27 | 合盛硅业(鄯善)有限公司 | Method for treating methyl chlorosilane hydrolysis emulsion |
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