CN104558015A - Preparation method of high-purity organosilicone monomer - Google Patents
Preparation method of high-purity organosilicone monomer Download PDFInfo
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Abstract
The invention provides a preparation method of a high-purity organosilicone monomer and particularly relates to a method for preparing an electronic grade high-purity organosilicone monomer by carrying out the following steps on an industrial organosilicone monomer: multiple rectifying; membrane filtration; multiple sub-boiling distillation and the like. The method provided by the invention is simple in process operation and high in safety, the purity of the prepared organosilicone monomer is greater than 99.99%, the content of a single metal ion impurity is less than 0.1ppb and the density of solid particles which are greater than or equal to 0.5 micron is less than 5/ml. Moreover, the product is stable in quality and can satisfy the preparation requirement of an ultra large scale integration circuit.
Description
Technical field
The invention provides a kind of preparation method producing high-purity organosilicon monomer, be specifically related to the purification process of the liquid source monomer of a kind of organosilicon for semicon industry.
Background technology
Organosilane is because having excellent dielectric properties, and being important source material required in super large-scale integration manufacturing processed, is one of indispensable micro-electronics chemicals.The purity of organosilane product directly affects the performance of unicircuit, the existence of impurity especially metal ion in product, be easy to the generation causing staggered floor, thus increase leakage current, cause the life-span puncturing and reduce current carrier, for nanometer-grade IC, several metal ion or dust granule are just enough to scrap whole circuit.Therefore, the high-purity organosilicon liquid source of the growth requirement electronic-grade of super large-scale integration.
The purification process of high-purity organosilicon alkane mainly includes the removal of machine impurity, metal ion and solia particle.Wherein, the removal of organic impurity mainly adopts the method for absorption and rectifying, solia particle is then removed by filtration procedure, but the removal difficulty of metal ion is larger, conventional purification process is not obvious to metal ion removal effect, is difficult to reach below ppm, but for the silane of high-end chip, require to control within 10ppb to metal ion content, therefore need a kind of purification technique producing high purity organosilane monomer.
US Patent No. 2008314728A1 discloses a kind of method of purifying trichlorosilicane and silicon tetrachloride, polymkeric substance precipitation is formed by adding complexing agent complexes metal ion, and then pass through the method for rectifying purifying, the last metal ion content of the method can only reach 0.1ppm, can not meet the preparation requirement of electronic grade high-purity siloxanes.
US Patent No. 5312947A discloses a kind of method increasing ionic crystal size exclusion, by introducing polar solvent in silane systems, evaporation after fully stirring at a certain temperature, increase the object realizing filtering based on metal ion crystalline size, but metal ion can only be controlled in ppm rank by the method.
US Patent No. 20050054211A1 discloses the organosilyl method of a kind of absorption tower absorption purification, be dissolved in solvent by silane, then the absorption tower by being equipped with sorbent material is filtered, then evaporates and concentrate, and then repetitive operation has reached the object of removing metal ion.The method has certain for metal ion effect, but needs a large amount of organic solvent as carrier, produce productive rate low, and treating processes needs Real-Time Monitoring, repeatedly repeats, treating processes poor controllability, cannot be applied to suitability for industrialized production.
Chinese patent CN102245618A discloses a kind of method by adsorbent metal ion purification silicon compound, the metal ion of the method to particular types has certain removal effect, but only can not ensure, to so the metal ion of kind is removed, can not ensure because of activated carbon of sorbent or diatomaceously add the introducing causing other impurity by simple physisorptive filter.
Therefore, in the removal organosilicon of, economical and efficient simple in the urgent need to a kind of technological operation, the method for metal ion, to obtain electronic grade high-purity organosilicon, is particularly useful for the high-purity organosilicon liquid source of large-scale integrated circuit.
Summary of the invention
The object of this invention is to provide the purification process of the liquid source monomer of organosilicon that a kind of technological operation is simple, quality product is high.
A first aspect of the present invention, provide a kind of preparation method of high-purity organosilicon monomer, described preparation method comprises the steps:
(1), make industrial organosilane monomer by multiple rectifying tower, thus multiple rectifying is carried out to it, obtain the first purifying organosilane monomer;
(2), make the first described purifying organosilane monomer by the first film filter, thus carry out coarse filtration, obtain the second purifying organosilane monomer;
(3), make the second described purifying organosilane monomer enter multiple sub-boiling distillation device, multiple sub-boiling distillation is carried out to it, and collects cut, obtain the 3rd purifying organosilane monomer;
(4), the 3rd described purifying organosilane monomer is filtered by the second film filter, obtain product high-purity organosilicon monomer.
In another preference, described organosilane monomer is organosilane, is preferably liquid organosilicon alkane.
In another preference, described multiple rectifying tower has the rectifying tower of 1 ~ 10 group of serial or parallel connection, preferably has the rectifying tower of 2 ~ 8 groups of serial or parallel connections; Wherein, often organize rectifying tower inside and there are more than 2 rectifying tower cylinders of mutually connecting.
In another preference, in described multiple rectifying tower, the cylinder of cylinder independently of one another for being selected from lower group of each rectifying tower: stainless steel cylinder, quartzy cylinder, PFA liner cylinder, or its combination; And/or
In described multiple rectifying tower, the filler of filler independently of one another for being selected from lower group in each rectifying tower or rectifying tower cylinder: the random packing that the coated structured packing of stainless steel structured packing, stainless steel random packing, quartzy structured packing, quartzy random packing, PFA, PFA are coated, or its combination.
In another preference, in described step (1), described multiple rectifying is carried out under 0.02 ~ 0.1MPa pressure.
In another preference, the first described film filter and the second film filter are PP film filter or PTFE film strainer; Preferably, the first described film filter and the aperture of the second film filter are 0.002 ~ 0.5 μm.
In another preference, the aperture of the first described film filter is 0.05-0.5 μm.
In another preference, the aperture of the second described film filter is 0.002-0.1 μm.
In another preference, described step (3) is carried out under ultra-clean condition; And/or described step (3) is carried out under an inert atmosphere.
In another preference, described step carries out referring in described step under an inert atmosphere, and (being preferably in multiple sub-boiling distillation device) in purifying environment has inert atmosphere protection.
In another preference, described inert atmosphere is nitrogen atmosphere or argon gas atmosphere.
In another preference, described multiple sub-boiling distillation utensil has the sub-boiling distillation device of many group serial or parallel connections, preferably has the sub-boiling distillation device of 2 ~ 8 groups of serial or parallel connections; Preferably, described sub-boiling distillation device body adopts stainless steel or the high purity quartz material of PFA liner.
In another preference, described sub-boiling distillation device is can the sub-boiling distillation device of accurate temperature controlling.
In another preference, also comprise in described step (3): the cut collecting (T-100) ~ T DEG C; Wherein, described T is the boiling point of target organosilane monomer; Preferably, the cut of (T-80) ~ (T-5) DEG C is collected.
A second aspect of the present invention, provide a kind of high-purity organosilicon monomer production plant, described equipment comprises: multiple rectifying tower assembly, the first film filter assembly, multiple sub-boiling distillation device assembly, the second film filter assembly; And be connected by transfer line between each assembly.
In another preference, described transfer line is stainless steel, quartz, the stainless steel of PFA liner or the pipeline of PTFE material.
In another preference, the first described film filter assembly comprises: the first film filter, and intermediates storage tank.
In another preference, described multiple sub-boiling distillation device assembly comprises: the sub-boiling distillation device of multiple mutual series connection, and the 3rd intermediates storage tank.
In another preference, described multiple rectifying tower assembly has the rectifying tower of 1 ~ 10 group of serial or parallel connection, preferably has the rectifying tower of 2 ~ 8 groups of serial or parallel connections; Wherein, often organize rectifying tower inside and there are more than 2 rectifying tower cylinders of mutually connecting;
Preferably, in described multiple rectifying tower, the cylinder of cylinder independently of one another for being selected from lower group of each rectifying tower: stainless steel cylinder, quartzy cylinder, PFA liner cylinder, or its combination; And/or
In described multiple rectifying tower, the filler of filler independently of one another for being selected from lower group of each rectifying tower: the random packing that the coated structured packing of stainless steel structured packing, stainless steel random packing, quartzy structured packing, quartzy random packing, PFA, PFA are coated, or its combination.
In another preference, in described multiple rectifying tower assembly, each rectifying tower also has tower reactor, front-end volatiles storage tank, the first intermediates storage tank and after cut storage tank.
In another preference, the first described film filter and the second film filter are PP film filter or PTFE film strainer; Preferably, the first described film filter and the aperture of the second film filter are 0.002 ~ 0.5 μm.
In another preference, the aperture of the first described film filter is 0.05-0.5 μm.
In another preference, the aperture of the second described film filter is 0.002-0.01 μm.
In another preference, described multiple sub-boiling distillation utensil has the sub-boiling distillation device of many group serial or parallel connections, preferably has the sub-boiling distillation device of 2 ~ 8 groups of serial or parallel connections.
In another preference, described sub-boiling distillation device is can the sub-boiling distillation device of accurate temperature controlling.
In another preference, described sub-boiling distillation device body adopts stainless steel or the high purity quartz material of PFA liner.
Should be understood that within the scope of the present invention, above-mentioned each technical characteristic of the present invention and can combining mutually between specifically described each technical characteristic in below (eg embodiment), thus form new or preferred technical scheme.As space is limited, tiredly no longer one by one to state at this.
Accompanying drawing explanation
Fig. 1 is device schematic diagram of the present invention, and in figure, each legend is as follows:
111,112 rectifying tower
121,122 tower reactors
131,132 front-end volatiles storage tanks
141,142 first intermediates storage tanks
23 second intermediates storage tanks
34 the 3rd intermediates storage tanks
151,152 after cut storage tanks
161,21,31,41 volume pumps
22 first film filters
31,32 sub-boiling distillation devices
42 second film filters.
Embodiment
The present inventor is through long-term and deep research, be surprised to find that, organosilicon liquid source passes through rectifying, coarse filtration, sub-boiling distillation, refilter, the product of high purity (purity is greater than 99.99%), low metal ion (single impurity metal ion content is less than 0.1ppb) can be obtained, meet the preparation requirement of great scale integrated circuit to high-purity organosilicon liquid source.Based on above-mentioned discovery, contriver completes the present invention.
Term
As used herein, term " multiple rectifying tower " refers to the assembly of the rectifying tower with more than one group serial or parallel connection, wherein, often organizes rectifying tower and all has two or more rectifying tower cylinders of connecting mutually.
The preparation of high-purity organosilicon monomer
The invention provides a kind of preparation method of high-purity organosilicon monomer, described preparation method comprises the steps:
(1), make industrial organosilane monomer by multiple rectifying tower, thus multiple rectifying is carried out to it, obtain the first purifying organosilane monomer;
(2), make the first described purifying organosilane monomer by the first film filter, thus carry out coarse filtration, obtain the second purifying organosilane monomer;
(3), make the second described purifying organosilane monomer enter multiple sub-boiling distillation device, it is distilled, and collects cut, obtain the 3rd purifying organosilane monomer;
(4), the 3rd described purifying organosilane monomer is filtered by the second film filter, obtain product high-purity organosilicon monomer.
In another preference, described organosilane monomer is organosilane, is preferably liquid organosilicon alkane.The product high-purity organosilicon monomer obtained can directly be packed after exporting.
Described multiple rectifying tower preferably has the cylinder of 2 ~ 10 series connection, preferably has the cylinder of 2 ~ 8 series connection.When producing high-purity organosilicon monomer, being flowed to by regulation and control, make industrial organosilane monomer by more than one rectifying column thus carry out multiple rectifying.Described multiple rectifying tower also can have many groups rectifying tower in parallel (often organizing the rectifying column that rectifying tower comprises more than 2 mutual series connection), and when producing, the rectifying tower of each group parallel connection passes into industrial organosilane monomer simultaneously and carries out multiple rectifying.
In described multiple rectifying tower, the cylinder of each rectifying tower is not particularly limited, such as (but being not limited to) cylinder independently of one another for being selected from lower group: stainless steel cylinder, quartzy cylinder, PFA liner cylinder, or its combination.
In described multiple rectifying tower, the filler of each rectifying tower has no particular limits, and can be structured packing or random packing.In another preference, the filler of filler independently of one another for being selected from lower group of each rectifying tower: the random packing that the coated structured packing of stainless steel structured packing, stainless steel random packing, quartzy structured packing, quartzy random packing, PFA, PFA are coated, or its combination.
In the preferred embodiments of the present invention, the multiple rectifying in described step (1) under normal pressure or reduced pressure, such as, can be carried out under 0.02 ~ 0.1MPa pressure.In a preferred embodiment of the invention, first carry out one or more groups rectifying at ambient pressure, then carry out one or more groups rectifying more at reduced pressure conditions.
In described step (1), in described multiple rectification step, by collecting intermediates (the i.e. cut of (T-3) ~ (T+3) DEG C; Be more preferably (T-2) ~ the cut of (T+2) DEG C), obtain the first required purifying organosilane monomer.Wherein, described T is the boiling point of target organosilane monomer under corresponding pressure, T value under normal pressure can be determined according to the kind of target organosilane monomer by those skilled in the art, and the T value under reduced pressure can be drawn by the account form that this area is conventional by those skilled in the art.
In described step (2) and (4), the first described film filter and the kind of the second film filter have no particular limits, and can select the film filter of any appropriate, such as PP film filter or PTFE film strainer; Preferably, the first described film filter and the aperture of the second film filter are 0.002 ~ 0.5 μm.
In another preference, the first described film filter and the aperture of the second film filter are different, such as, first film filter (for coarse filtration) selects aperture to be the film filter of 0.05-0.5 μm, and the second film filter (again filter and obtain end product) selects aperture to be the film filter of 0.002-0.1 μm.
In another preference, described step (3) is carried out under ultra-clean condition; And/or described step (3) is carried out under an inert atmosphere.
In another preference, described step carries out referring in described step under an inert atmosphere, has inert atmosphere protection in purifying environment (being preferably multiple sub-boiling distillation device).
In another preference, described inert atmosphere is nitrogen atmosphere or argon gas atmosphere.
In another preference, described multiple sub-boiling distillation utensil has the sub-boiling distillation device of many group serial or parallel connections, preferably has the sub-boiling distillation device of 2 ~ 8 groups of serial or parallel connections.Described sub-boiling distillation device is preferably can the sub-boiling distillation device of accurate temperature controlling.
In another preference, described sub-boiling distillation device body adopts stainless steel or the high purity quartz material of PFA liner.
In described step (3) after distillation, preferably collect the cut of (T-100) ~ T DEG C; Wherein, described T is the boiling point of target organosilane monomer; More preferably, the cut of (T-80) ~ (T-5) DEG C is collected.
In described preparation process, the flow of liquid phase has no particular limits, and can adjust, particularly according to output of products flow, can set according to the size of distiller, such adjustment is that those skilled in the art can learn apparently after having read content disclosed by the invention.In particularly preferred embodiment of the present invention, the inventory that flow control makes to enter in each reaction member (as multiple sub-boiling distillation device) and flow out of liquid phase is substantially suitable, such as, the amount of the second purifying organosilane monomer passed in multiple sub-boiling distillation device and the 3rd purifying organosilane monomer of outflow quite or substantially suitable.
Described method can obtain the electronic-grade organosilicon liquid source that can be applicable to large-scale integrated circuit, in preferred embodiments more of the present invention, preparation-obtained product purity is greater than 99.99%, single impurity metal ion content is less than 0.1ppb, and a particle diameter >=0.5 μm solid particulate is less than 5/ml.
High-purity organosilicon monomer production plant
Present invention also offers a kind of high-purity organosilicon monomer production plant being applicable to the inventive method, described equipment comprises: multiple rectifying tower assembly, the first film filter assembly, multiple sub-boiling distillation device assembly, the second film filter assembly; And be connected by transfer line between each assembly.
In another preference, described transfer line is be selected from the pipeline of lower group: the stainless steel pipeline of stainless steel pipeline, quartzy pipeline, PFA liner, or the pipeline of PTFE material.
In another preference, described multiple rectifying tower preferably has the cylinder of 2 ~ 10 series connection, preferably has the cylinder of 2 ~ 8 series connection.Described multiple rectifying tower also can have many groups rectifying tower in parallel (often organizing the rectifying column that rectifying tower comprises more than 2 mutual series connection).
In another preference, in described multiple rectifying tower, the cylinder of cylinder independently of one another for being selected from lower group of each rectifying tower: stainless steel cylinder, quartzy cylinder, PFA liner cylinder, or its combination.
In another preference, in described multiple rectifying tower, the filler of filler independently of one another for being selected from lower group of each rectifying tower: the random packing that the coated structured packing of stainless steel structured packing, stainless steel random packing, quartzy structured packing, quartzy random packing, PFA, PFA are coated, or its combination.
In another preference, the first described film filter and the second film filter are PP film filter or PTFE film strainer; Preferably, the first described film filter and the aperture of the second film filter are 0.002 ~ 0.5 μm.In another preference, the aperture of the first described film filter is 0.05-0.5 μm; The aperture of the second described film filter is 0.002-0.1 μm.
In another preference, described multiple sub-boiling distillation utensil has the sub-boiling distillation device of many group serial or parallel connections, preferably has the sub-boiling distillation device of 2 ~ 8 groups of serial or parallel connections.
In another preference, described sub-boiling distillation device is can the sub-boiling distillation device of accurate temperature controlling.
In another preference, described sub-boiling distillation device body adopts stainless steel or the high purity quartz material of PFA liner.
In a preferred embodiment of the invention, described production unit has structure (be only the structure that the application's production unit is schematically described herein, and not show most preferred situation) as shown in Figure 1.Wherein, described equipment comprises two groups of rectifying tower 111,112, and each group rectifying tower comprises tower reactor (tower reactor 121,122 namely in figure), front-end volatiles storage tank (the front-end volatiles storage tank 131,132 namely in figure), intermediates storage tank (the intermediates storage tank 141,142 namely in figure) and after cut storage tank (the after cut storage tank 151,152 namely in figure).The front-end volatiles obtained in rectifying are stored in described front-end volatiles storage tank, and after cut is stored in after cut storage tank, and required cut to be stored in each the first intermediates storage tank and to be entered the relevant device of subsequent step by transfer line.Described equipment also comprises one first film filter, the first described film filter have one filter for storage films after the second intermediates storage tank 23 of the second purifying organosilane monomer of obtaining.The second described purifying organosilane monomer enters multiple sub-boiling distillation device by transfer line, there is in described multiple sub-boiling distillation device the sub-boiling distillation device (the sub-boiling distillation device 31,32 namely in figure) of multiple series connection, and the 3rd intermediates storage tank 34 of the 3rd purifying organosilane monomer for obtaining after storing sub-boiling distillation.The 3rd described purifying organosilane monomer enters the second film filter by transfer line, after membrane filtration purifying, obtains the finished product high-purity organosilicon monomer.
In the apparatus, preferably also comprise one or more volume pump, to control material flow.In a preferred case, described equipment comprises: be positioned at and be communicated with intermediates storage tank 141 and the volume pump 161 on the connecting pipeline of tower reactor 122, be positioned at and be communicated with intermediates storage tank 142 and the volume pump 21 on the connecting pipeline of the first film filter 22, be positioned at and be communicated with intermediates storage tank 23 and the volume pump 31 on the connecting pipeline of multiple sub-boiling distillation device 31 and the volume pump 41 be positioned on the connecting pipeline being communicated with intermediates storage tank 34 and the second film filter 42.
Compared with prior art, major advantage of the present invention comprises:
(1) method provided by the invention is applicable to the organosilicon liquid source required for the preparation of all unicircuit, wide adaptability.
(2) the present invention is by rectifying, and coarse filtration, sub-boiling distillation, refilters, simple to operate, process control, and stable yield can be used for suitability for industrialized production.
(3) product purity high (purity is greater than 99.99%), metal ion content low (single impurity metal ion content is less than 0.1ppb), solid particulate few (>=0.5 μm of particle is less than 5/ml), meets the requirement of large-scale integrated circuit to electronic-grade organosilicon liquid source completely.
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.The experimental technique of unreceipted actual conditions in the following example, usually conveniently condition, or according to the condition that manufacturer advises.Unless otherwise indicated, otherwise per-cent and number calculate by weight.
The preparation of the high-purity octamethylcyclotetrasiloxane of embodiment 1
(1) rectifying
Under atmospheric pressure state, Contained In Commercial OctamethylcyclotetraOnloxane is joined in reactor, then by four groups of rectifying column series connection continuous rectifications, control splitting ratio and column temperature, collect the cut of 173-175 DEG C.
(2) coarse filtration
By the cut collected by volume pump by 0.5 μm of film filter.
(3) sub-boiling distillation
Under nitrogen protection, by volume pump toward sub-boiling distillation device continuous sample introduction, two groups of sub-boiling distillation device series connection, Heating temperature is raised to 150 ~ 155 DEG C and collects cut.
(4) essence filter
The cut collected, by the film filter of volume pump by 0.005 μm, then outputs to directly filling.
Product detects through GC, ICP-MS and PMS, and product purity is 99.999%, and single metal ion content, lower than 1ppb, is more than or equal to 0.5 μm of particle and is less than 5/ml.
The preparation of the high-purity octamethylcyclotetrasiloxane of embodiment 2
(1) rectifying
Under atmospheric pressure state, Contained In Commercial OctamethylcyclotetraOnloxane is joined in reactor, then by five groups of rectifying column series connection continuous rectifications, control splitting ratio and column temperature, collect the cut of 173-175 DEG C.
(2) coarse filtration
By the cut collected by volume pump by 0.1 μm of film filter.
(3) sub-boiling distillation
Under nitrogen protection, by volume pump toward sub-boiling distillation device continuous sample introduction, three groups of sub-boiling distillation device series connection, Heating temperature is raised to 140 ~ 145 DEG C and collects cut.
(4) essence filter
The cut collected, by the film filter of volume pump by 0.005 μm, then exports directly filling.
Product detects through GC, ICP-MS and PMS, and product purity is 99.9999%, and single metal ion content, lower than 0.1ppb, is more than or equal to 0.5 μm of particle and is less than 5/ml.
The preparation of the high-purity octamethylcyclotetrasiloxane of embodiment 3
(1) rectifying
Under atmospheric pressure state, Contained In Commercial OctamethylcyclotetraOnloxane is joined in reactor, then by two groups of rectifying column series connection continuous rectifications, control splitting ratio and column temperature, collect the cut of 173-175 DEG C, then through two groups of rectifying column rectifying under 0.015MPa, collect the cut of 107-110 DEG C.
(2) coarse filtration
By the cut collected by volume pump by 0.1 μm of film filter.
(3) sub-boiling distillation
Under nitrogen protection, by volume pump to three groups of sub-boiling distillation devices in parallel continuous sample introduction respectively, then be connected in series to another group sub-boiling distillation device, Heating temperature is raised to 145 ~ 150 DEG C and collects cut.
(4) essence filter
The cut collected, by the film filter of volume pump by 0.005 μm, then exports directly filling.
Product detects through GC, ICP-MS and PMS, and product purity is 99.999%, and single metal ion content, lower than 0.5ppb, is more than or equal to 0.5 μm of particle and is less than 5/ml.
The preparation of the high-purity Union carbide A-162 of embodiment 4
(1) rectifying
Under atmospheric pressure state, technical grade methyl triethoxyl silane is joined in reactor, then by three groups of rectifying column series connection continuous rectifications, control splitting ratio and column temperature, collect the cut of 141-143 DEG C.
(2) coarse filtration
By the cut collected by volume pump by 0.1 μm of film filter.
(3) sub-boiling distillation
Under nitrogen protection, by volume pump toward sub-boiling distillation device continuous sample introduction, three groups of sub-boiling distillation device series connection, Heating temperature is raised to 120 ~ 125 DEG C and collects cut.
(4) essence filter
The cut collected, by the film filter of volume pump by 0.002 μm, then exports directly filling.
Product detects through GC, ICP-MS and PMS, and product purity is 99.99%, and single metal ion content, lower than 0.1ppb, is more than or equal to 0.5 μm of particle and is less than 5/ml.
The preparation of the high-purity dimethyldimethoxysil,ne of embodiment 5
(1) rectifying
Under atmospheric pressure state, technical grade dimethyldimethoxysil,ne is joined in reactor, then by three groups of rectifying column series connection continuous rectifications, control splitting ratio and column temperature, collect the cut of 81-82 DEG C.
(2) coarse filtration
By the cut collected by volume pump by 0.2 μm of film filter.
(3) sub-boiling distillation
Under nitrogen protection, by volume pump toward sub-boiling distillation device continuous sample introduction, three groups of sub-boiling distillation device series connection, Heating temperature is warmed up to 65 ~ 70 DEG C and collects cut.
(4) essence filter
The cut collected, by the film filter of volume pump by 0.005 μm, then exports directly filling.
Product detects through GC, ICP-MS and PMS, and product purity is 99.99%, and single metal ion content, lower than 0.1ppb, is more than or equal to 0.5 μm of particle and is less than 5/ml.
The preparation of the high-purity octamethylcyclotetrasiloxane of comparative example
(1) rectifying
Under atmospheric pressure state, Contained In Commercial OctamethylcyclotetraOnloxane is joined in reactor, then by four groups of rectifying column series connection continuous rectifications, control splitting ratio and column temperature, collect the cut of 173-175 DEG C.
(2) filter
By the cut collected by volume pump by 0.005 μm of film filter, then export directly filling.
Product detects through GC, ICP-MS and PMS, and product purity is 99.98%, and single metal ion content is higher than 60ppb, and being more than or equal to 0.5 μm of particle is 18/ml.
Can be found out by above-mentioned comparative example and embodiment, the production technique of the application is the very preferred high-purity organosilicon oxygen alkane production technique of a class, as in production technique or several step is omitted time, namely there is very large difference in the quality of the organo-siloxane product obtained, cannot reach the requirement needed for unicircuit.
The all documents mentioned in the present invention are quoted as a reference all in this application, are just quoted separately as a reference as each section of document.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read above-mentioned teachings of the present invention, these equivalent form of values fall within the application's appended claims limited range equally.
Claims (10)
1. a preparation method for high-purity organosilicon monomer, is characterized in that, described preparation method comprises the steps:
(1), make industrial organosilane monomer by multiple rectifying tower, thus multiple rectifying is carried out to it, obtain the first purifying organosilane monomer;
(2), make the first described purifying organosilane monomer by the first film filter, thus carry out coarse filtration, obtain the second purifying organosilane monomer;
(3), make the second described purifying organosilane monomer enter multiple sub-boiling distillation device, multiple sub-boiling distillation is carried out to it, and collects cut, obtain the 3rd purifying organosilane monomer;
(4), the 3rd described purifying organosilane monomer is filtered by the second film filter, obtain product high-purity organosilicon monomer.
2. the method for claim 1, is characterized in that, described multiple rectifying tower has the rectifying tower of 1 ~ 10 group of serial or parallel connection, preferably has the rectifying tower of 2 ~ 8 groups of serial or parallel connections; Wherein, often organize rectifying tower inside and there are more than 2 rectifying tower cylinders of mutually connecting.
3. method as claimed in claim 1 or 2, is characterized in that, in described multiple rectifying tower, and the cylinder of cylinder independently of one another for being selected from lower group of each rectifying tower: stainless steel cylinder, quartzy cylinder, PFA liner cylinder, or its combination; And/or
In described multiple rectifying tower, the filler of filler independently of one another for being selected from lower group in each rectifying tower or rectifying tower cylinder: the random packing that the coated structured packing of stainless steel structured packing, stainless steel random packing, quartzy structured packing, quartzy random packing, PFA, PFA are coated, or its combination.
4. the method for claim 1, is characterized in that, the first described film filter and the second film filter are PP film filter or PTFE film strainer; Preferably, the first described film filter and the aperture of the second film filter are 0.002 ~ 0.5 μm.
5. the method for claim 1, is characterized in that, described multiple sub-boiling distillation utensil has the sub-boiling distillation device of many group serial or parallel connections, preferably has the sub-boiling distillation device of 2 ~ 8 groups of serial or parallel connections; Preferably, described sub-boiling distillation device body adopts stainless steel or the high purity quartz material of PFA liner.
6. the method for claim 1, is characterized in that, also comprises in described step (3): the cut collecting (T-100) ~ T DEG C; Wherein, described T is the boiling point of target organosilane monomer; Preferably, the cut of (T-80) ~ (T-5) DEG C is collected.
7. a high-purity organosilicon monomer production plant, is characterized in that, described equipment comprises: multiple rectifying tower assembly, the first film filter assembly, multiple sub-boiling distillation device assembly, the second film filter assembly; And be connected by transfer line between each assembly.
8. production unit as claimed in claim 7, it is characterized in that, described multiple rectifying tower assembly has the rectifying tower of 1 ~ 10 group of serial or parallel connection, preferably has the rectifying tower of 2 ~ 8 groups of serial or parallel connections; Wherein, often organize rectifying tower inside and there are more than 2 rectifying tower cylinders of mutually connecting;
Preferably, in described multiple rectifying tower, the cylinder of cylinder independently of one another for being selected from lower group of each rectifying tower: stainless steel cylinder, quartzy cylinder, PFA liner cylinder, or its combination; And/or
In described multiple rectifying tower, the filler of filler independently of one another for being selected from lower group of each rectifying tower: the random packing that the coated structured packing of stainless steel structured packing, stainless steel random packing, quartzy structured packing, quartzy random packing, PFA, PFA are coated, or its combination.
9. production unit as claimed in claim 7, it is characterized in that, the first described film filter and the second film filter are PP film filter or PTFE film strainer; Preferably, the first described film filter and the aperture of the second film filter are 0.002 ~ 0.5 μm.
10. production unit as claimed in claim 7, is characterized in that, described multiple sub-boiling distillation utensil has the sub-boiling distillation device of many group serial or parallel connections, preferably has the sub-boiling distillation device of 2 ~ 8 groups of serial or parallel connections.
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| CN109912636A (en) * | 2019-04-11 | 2019-06-21 | 苏州金宏气体股份有限公司 | A kind of production method of high-purity ethyl orthosilicate |
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| CN101065324A (en) * | 2004-11-19 | 2007-10-31 | Memc电子材料有限公司 | Process and plant for the purification of trichlorosilane and silicon tetrachloride |
| CN103113401A (en) * | 2013-03-20 | 2013-05-22 | 上海中科高等研究院 | Method and device for producing high-purity organic silicon |
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| CN101065324A (en) * | 2004-11-19 | 2007-10-31 | Memc电子材料有限公司 | Process and plant for the purification of trichlorosilane and silicon tetrachloride |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109912636A (en) * | 2019-04-11 | 2019-06-21 | 苏州金宏气体股份有限公司 | A kind of production method of high-purity ethyl orthosilicate |
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