CN103896980B - The method of purification of silicoorganic compound - Google Patents
The method of purification of silicoorganic compound Download PDFInfo
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Abstract
The invention provides a kind of method of purification of silicoorganic compound, the method for purification of described silicoorganic compound at least comprises: silicoorganic compound and magnetic being stirred at a first temperature is formed with the mixture of organic silicon compound and magnetic; Silicoorganic compound are extracted from the mixture of described silicoorganic compound and magnetic.The present invention adopts magnetic and needs the silicoorganic compound of purifying to mix, and is adsorbed by the metallic impurity in silicoorganic compound to utilize magnetic.Also by the mode of rectifying, the organic impurity in silicoorganic compound is removed in addition, obtain the silicoorganic compound that purity is greater than 99.9%.
Description
Technical field
The present invention relates to a kind of integrated circuit processing technique field, particularly relate to a kind of method of purification of silicoorganic compound.
Background technology
Along with the reduction of the size of integrated circuit (IC) chip, low-k deposited film is the key of advanced semiconductor manufacturing, and the risk that the electrical signal because metal wire can be made to encapsulate more closely on a single die for it between adjacent layers leaks is less.
In semiconductor fabrication process, the silicoorganic compound such as tetramethylsilane, dimethyldimethoxysil,ne, octamethylcyclotetrasiloxane, trifluoro propyl cyclotrisiloxane can be used as the raw material of low-k deposited film.
But commercially available above-mentioned silicoorganic compound are usually containing metallic impurity and organic impurity, and impurity concentration is quite high.These metallic impurity and organic impurity affect larger on the quality of film and dielectric constant values.Particularly metallic impurity, can increase the dielectric constant values of deposit film significantly.Therefore, before commercially available silicoorganic compound being applied to semiconductor production manufacture, metal wherein and organic impurity must be removed.
Be in the European patent document of EP0957105B1 in the patent No., disclose and process to organoalkoxysilane or based on the composition of organoalkoxysilane with gac, reduce the content of wherein residual halogens and improve colour.But gac, to wherein adsorption of metal ions power is less, is difficult to remove wherein trace metal ion.
Be in the Chinese patent literature of 200980149421.8 in the patent No., disclose and sorbent material is mixed with silicon compound, then remove the metallic impurity in silicon compound by the method for metre filter.The method technique is simple, easy to operate, but the trace metal impurities in the organic impurity cannot removed in silicon compound and more difficult removal cyclopolysiloxane, because the anion of the ring texture of cyclopolysiloxane and Si-O key, make part metals ion easily and cyclopolysiloxane complexing, as K+, Na+ etc.
Be in the american documentation literature of US007879198B2 in the patent No., disclose a kind of rectifying tower of applying to the method and system of silicoorganic compound of purifying.The method is easy to operate, but cannot remove the trace metal impurities in silicoorganic compound completely.
Be in the american documentation literature of US20110259818A1 in the patent No., disclose the filtration medium melt-blown non-woven base material be made up of cyclic olefine copolymer or cyclic olefin polymer being made decontaminating liquid, its function removing metallic compound and metal ion is given by introducing ion-exchange group or chelation group on this nonwoven substrates, the method can remove acid, alkaline solution, ultrapure water, metallic impurity in the liquid that the viscosity such as organic solvent are less, but be difficult to remove the trace metal impurities of organo-siloxane particularly in cyclopolysiloxane.
To sum up, the purification mode of the silicoorganic compound provided in conventional art is all difficult to remove the metallic impurity in silicoorganic compound and organic impurity completely, along with further developing of integrated circuit technology, need a kind of mode of better purification silicoorganic compound, highly purified silicoorganic compound are provided.
Summary of the invention
The shortcoming of prior art in view of the above, the object of the present invention is to provide a kind of method of purification of silicoorganic compound, is difficult to remove completely the problem of metallic impurity in silicoorganic compound and organic impurity for solving in prior art.
For achieving the above object and other relevant objects, the invention provides a kind of method of purification of silicoorganic compound, the method for purification of described silicoorganic compound at least comprises:
Silicoorganic compound and magnetic are stirred at a first temperature and is formed with the mixture of organic silicon compound and magnetic;
Silicoorganic compound are extracted from the mixture of described silicoorganic compound and magnetic.
Preferably, the chemical formula of described magnetic is Fe
3o
4, Fe
3o
4tiO
2nH
2o or Fe
3o
4siO
2tiO
2nH
2one or more in O, wherein n=1 ~ 5.
Preferably, the particle diameter of described magnetic is 5 μm ~ 20 μm.
Preferably, adopt magnetic agitation well heater to carry out the stirring of described silicoorganic compound and magnetic, the time that stirring is carried out is more than or equal to 3h.
Preferably, described first temperature is more than or equal to 25 DEG C, is less than the minimum boiling point of organic impurity.
Preferably, the method for silicoorganic compound is extracted described in for distillation, rectifying or filtration.
Preferably, adopt the mode of rectifying to extract silicoorganic compound from the mixture of described silicoorganic compound and magnetic, comprising:
Heat the mixture of described silicoorganic compound and magnetic, Heating temperature is the second temperature;
Vacuumize and carry out condensation;
Collect the cut of the first cut temperature, to obtain organic impurity;
Heat the mixture of described silicoorganic compound and magnetic, Heating temperature is warming up to the 3rd temperature;
Collect the cut of the second cut temperature, to obtain organic impurity and silicoorganic compound;
Heat the mixture of described silicoorganic compound and magnetic, Heating temperature maintains the 4th temperature, collect the cut of the 3rd cut temperature, obtain the silicoorganic compound that purity is greater than 99.9%, described 4th temperature is the Heating temperature of cut temperature-stable when the 3rd cut temperature.
Preferably, adopt rectifying tower to carry out rectifying, described smart tower comprises rectifying still; Describedly silicoorganic compound and magnetic to be stirred at a first temperature and the operation of mixture of the described silicoorganic compound of described heating and magnetic is all carried out in rectifying still.
Preferably, described second temperature and described 3rd temperature are more than or equal to the boiling point of part organic impurity; Described 3rd temperature is greater than the maximum boiling point of organic impurity, is less than or equal to the boiling point of described silicoorganic compound; Described first cut temperature is between described first temperature and the second temperature; Described second cut temperature is less than or equal to described 3rd cut temperature.
Preferably, before the mixture forming described silicoorganic compound and magnetic, the step knowing organic impurity in described silicoorganic compound is also comprised.
Preferably, before the mixture forming described silicoorganic compound and magnetic, also comprise the process being carried out by described magnetic activating, comprising:
Described magnetic and dilute nitric acid solution are shaken 3h under 50 DEG C of constant temperature, takes out magnetic;
Adopt ultrapure water by described magnetic cleaning to neutral;
By described magnetic in a vacuum, dry at 110 DEG C.
Preferably, before the mixture forming described silicoorganic compound and magnetic, or after extracting silicoorganic compound, also comprise the step of the metal element content in the described silicoorganic compound of test.
As mentioned above, the method for purification of silicoorganic compound of the present invention, has following beneficial effect:
By by the silicoorganic compound containing impurity and magnetic mixing in technical scheme provided by the invention, magnetic absorption is utilized to fall metallic impurity in silicoorganic compound.
In addition, magnetic absorption and rectifying can also be combined in technical scheme provided by the invention, magnetic namely can be utilized to adsorb the removal realizing metallic impurity, rectifying also can be utilized to be extracted by highly purified silicoorganic compound.Complete the purification of silicoorganic compound in the lump, simplify operation, reduce production cost.
Accompanying drawing explanation
Fig. 1 is shown as the schematic diagram of the method for purification of the silicoorganic compound provided in embodiments of the invention one.
The schematic diagram of the rectifying tower that the method for purification that Fig. 2 is shown as the silicoorganic compound provided in embodiments of the invention two uses.
Fig. 3 is shown as the schematic diagram of the method for purification of the silicoorganic compound provided in embodiments of the invention two.
Element numbers explanation
11 magnetic force heating stirrers
12 rectifying stills
13 rectifying columns
14 condensers
15,16,17 receiving bottles
18,19,110 valves
S11 ~ S12 step
S21 ~ S22 step
Embodiment
The invention provides a kind of method of purification of silicoorganic compound, by by the silicoorganic compound containing impurity and magnetic mixing, utilize magnetic to adsorb to fall metallic impurity in silicoorganic compound.
In addition, the present invention separately provides a kind of method of purification of silicoorganic compound, magnetic absorption and rectifying combine by it, both magnetic can have been utilized to adsorb the removal realizing metallic impurity, also rectifying can be utilized to be extracted by highly purified silicoorganic compound, complete the purification of silicoorganic compound in the lump, simplify operation, reduce production cost.
Below by way of specific specific examples, embodiments of the present invention are described, those skilled in the art the content disclosed by this specification sheets can understand other advantages of the present invention and effect easily.The present invention can also be implemented or be applied by embodiments different in addition, and the every details in this specification sheets also can based on different viewpoints and application, carries out various modification or change not deviating under spirit of the present invention.
Refer to Fig. 1 to Fig. 3.It should be noted that, the diagram provided in the present embodiment only illustrates basic conception of the present invention in a schematic way, then only the assembly relevant with the present invention is shown in graphic but not component count, shape and size when implementing according to reality is drawn, it is actual when implementing, and the kenel of each assembly, quantity and ratio can be a kind of change arbitrarily, and its assembly layout kenel also may be more complicated.
Embodiment one
The present embodiment adopts magnetic and needs the silicoorganic compound of purifying to mix, and is adsorbed by the metallic impurity in silicoorganic compound to utilize magnetic.Wherein, described metallic impurity comprise: metal simple-substance, metal oxide and metal-salt etc.Wherein, metallic impurity comprise various metallic element and comprise: Fe, Na, K, Gr, Pt etc.
As shown in Figure 1, the method for purification of described silicoorganic compound that the present embodiment provides at least comprises:
First, step S11 is performed: silicoorganic compound and magnetic are stirred at a first temperature and be formed with the mixture of organic silicon compound and magnetic;
Preferably, before described silicoorganic compound are mixed with magnetic, also comprise the mensuration of carrying out metal content in silicoorganic compound and activation treatment is carried out to described magnetic.
In the present embodiment, the mensuration of described metal content specifically comprises:
1) testing sample getting a certain amount of silicoorganic compound puts into PFA counteracting tank;
2) add appropriate super-pure nitric acid and ultra-pure hydrogen fluoric acid successively, put into microwave dissolver and clear up;
Wherein, described super-pure nitric acid by metal simple-substance in metallic impurity and convert metal oxides be ionizable go out metal ion (metal-salt).Further, the C-O key in silicoorganic compound, C-Si key can interrupt by described ultra-pure hydrogen fluoric acid, and the metal ion by the silicoorganic compound of some ring-types surround is released, and are beneficial to and measure all metal contents fully.
3), after having cleared up, take out with a certain amount of 2% dust technology dilution, then use ICP-MS (InductivelyCoupledPlasmaMassSpectrometry, inductive coupling plasma mass) to test metal element content.
Described dust technology act as dilute reaction solution, make ICP-MS can bear the pH value of described reaction solution.
In the present embodiment, activation treatment is carried out to described magnetic and specifically comprises:
1) get 5g magnetic and put into 100ml single necked round bottom flask, then add the dilute nitric acid solution of 50gPH=3, constant temperature oscillator shakes 3h at 50 DEG C, take out to divide and remove dilute nitric acid solution;
2) ultrapure water is adopted by described magnetic cleaning to neutral;
3) again magnetic is put into vacuum drying oven, drying 5 hours at 110 DEG C, then magnetic is taken out and use.
Through described activation treatment, the metallic impurity utilizing dust technology and pure water rinsing to eliminate magnetic to adsorb in the environment, make described magnetic to have the adsorption effect had most.
In the present embodiment, carried out above-mentioned metal content mensuration and after activation treatment is carried out to described magnetic, perform step S11 again, wherein, adopt magnetic agitation well heater to carry out the stirring of described silicoorganic compound and magnetic, the time that stirring is carried out is more than or equal to 3h, stirring velocity is 0r/min ~ 2400r/min, to make described magnetic better to be disperseed, can more fully come out and contact silicoorganic compound in the surface of magnetic powder particle, adsorb more metallic impurity.
Wherein, the mass ratio of silicoorganic compound and magnetic is 10000:1 ~ 10:1, can reach the effect of good adsorbing metal impurity.Concrete mass ratio also needs the content of the metallic impurity of the silicoorganic compound according to prediction to determine.
Described first temperature, higher than the fusing point of silicoorganic compound, is generally room temperature (25 DEG C), also can be slightly high, the viscosity that temperature raises silicoorganic compound can reduce, molecular motion is accelerated, and is more conducive to dispersed-powder dispersion, and fully contacts with metallic impurity.But described first temperature needs the minimum boiling point being less than organic impurity.
Described magnetic needs there is adsorptivity to the metallic impurity in silicoorganic compound, and metallic impurity firmly can be fixed on around magnetic, and metallic impurity can not be pulled away in the process extracting silicoorganic compound.
Described magnetic comprises: (chemical formula is Fe to magnetic F1
3o
4), (chemical formula is Fe to magnetic T6
3o
4tiO
2nH
2o, wherein n=1 ~ 5) or magnetic Si47 (chemical formula is Fe
3o
4siO
2tiO
2nH
2o, wherein n=1 ~ 5).
Described magnetic F1 is common magnet, can attract the ferromagnetic materials such as fe, cobalt, nickel and Z 250.Described magnetic F1 can be adsorbed with the part metals impurity in organic silicon compound in the present embodiment, as
the metallic impurity such as iron, cobalt, nickel.Magnet can attract the ferromagnetic materials such as fe, cobalt, nickel and Z 250.And magnetic T6 and magnetic Si47 contains certain magnetic can be adsorbed with part metals impurity in organic silicon compound, positively charged metal ion can firmly be fixed containing electronegative active group by its surface simultaneously, thus shows the effect of excellent removal metallic impurity.
The particle diameter of described magnetic is 5 μm ~ 20 μm, can better adsorbing metal impurity.The magnetic of equal in quality, particle diameter is less, and its specific surface area is larger, and what contact with metallic impurity is more abundant, can reduce the consumption of magnetic simultaneously, and through experiment, the magnetic effect of this particle size range is best.
Then, step S12 is performed: from the mixture of described silicoorganic compound and magnetic, extract silicoorganic compound.The described method of silicoorganic compound that extracts is for distillation, rectifying or filtration.
By step S12, the silicoorganic compound not having metallic impurity can be obtained.
Embodiment two
The present embodiment adopts the mode of rectifying to extract silicoorganic compound from the mixture of described silicoorganic compound and magnetic on the basis of embodiment one.General, the carbochain of the organic impurity in silicoorganic compound is shorter than silicoorganic compound, its boiling point, also lower than silicoorganic compound, so can be separated from silicoorganic compound by described organic impurity by the mode of rectifying in the present embodiment, realizes the purification of organosilicon compound.
Figure 2 shows that the structural representation of the rectifying device in the present embodiment.As shown in Figure 2, described rectifying device comprises: magnetic force heating stirrer 11, rectifying still 12, rectifying column 13 and condenser 14.
Residing magnetic force heating stirrer 11 coordinates with rectifying still 12, is suitable for the material that is distillated in rectifying still 12 to carry out stirring and heating.Described rectifying still 12, its material is quartz or stainless steel, and opening can have two, three or four, and size is 5L ~ 20L.
Described rectifying column 13 is positioned at the overthe openings of described rectifying still 12, and its material is quartz or stainless steel, and internal diameter is 30mm ~ 80mm, post height 1.2m ~ 2m, the packing height of filler is 1.2m-2m, can be stainless steel θ ring filler, the helical packing of stainless steel triangle, quartzy θ ring filler etc.
Described condenser 14 is positioned at above described rectifying column 13, and wherein phlegma is entered by import b, goes out from outlet c.The open top v of described condenser is suitable for connecting vacuum board, is suitable for being evacuated.
Described receiving bottle 15,16,17 is connected with rectifying column 13, is suitable for the cut receiving different boiling respectively.
Valve 18,19,110 is connected to receiving bottle 15, be mainly between 16,17 and rectifying column 13 and control different fractions and flow into different receiving bottle.
Concrete, as shown in Figure 3, the method for purification of the described silicoorganic compound that the present embodiment provides at least comprises:
First, step S21 is performed: silicoorganic compound and magnetic are stirred at a first temperature and be formed with the mixture of organic silicon compound and magnetic;
Wherein, the described rectifying still 12 silicoorganic compound and magnetic being put into the rectifying device shown in Fig. 2, utilizes magnetic force heating stirrer 11 to carry out heating and stirring.
The details of other this step and the operation before performing this step and the step S11 in embodiment one similar, be not repeated at this.
In addition, before execution next step, also comprise the step of the kind of the organic impurity in the silicoorganic compound known and be purified, so that in the distillation operation carried out in subsequent step, according to the boiling point setting Heating temperature of organic impurity and the temperature range of extraction cut.General, commercially available silicoorganic compound can indicate wherein contained dopant species, in addition also can by carrying out to silicoorganic compound to be purified the kind that Measurement and analysis determines organic impurity.The kind of concrete Measurement and analysis organic impurity knows technology for those skilled in the art, is again not repeated.
Then, perform step S22: the mixture heating described silicoorganic compound and magnetic, Heating temperature is the second temperature;
The described silicoorganic compound of described heating are the same with described operation silicoorganic compound and magnetic stirred at a first temperature with the operation of the mixture of magnetic, all carry out in rectifying still 12.Like this, the carrying out that can link up of step S21 and step S22.
Described second temperature is more than or equal to the boiling point of part organic impurity, makes this part of organic impurity can be evaporated in rectifying tower like this.
Then, step S23 is performed: vacuumize and carry out condensation;
Described vacuumizing is undertaken by described condenser overhead opening v, and vacuum degree control is at 0.1KPa-101.325KPa.Identical silicoorganic compound boiling point under different vacuum tightness is different, and vacuum tightness is higher, and the external pressure namely residing for silicoorganic compound is less, and corresponding silicoorganic compound boiling point is lower.When the setting of vacuum tightness needs to take into account the vacuum tightness that rectifier unit can reach, according to the respective boiling point size of silicoorganic compound and organic impurity and between them boiling point extent decide.
Then, step S24 is performed: the cut collecting the first cut temperature, to obtain organic impurity;
Described first cut temperature is less than the second temperature, this is due in rectifying, a temperature head is had to rectifying column top from bottom rectifying column, that is: temperature reduces successively from top to bottom, the temperature at rectifying column top be corresponding compound under corresponding pressure boiling point, so the Heating temperature of well heater is greater than the boiling point of this material under corresponding pressure.
Described first temperature does not reach the minimum boiling point of each impurity in silicoorganic compound, and described first cut temperature is greater than described first temperature.
Described second temperature is more than or equal to the boiling point of part organic impurity, makes this part of organic impurity can be evaporated in rectifying tower like this.In this step, valve 18 can be opened, this part of organic impurity is collected in receiving bottle 15.Centralized collection organic impurity, is conducive to " refuse " recycling of organic impurity.
Then, perform step S25: the mixture heating described silicoorganic compound and magnetic, Heating temperature is warming up to the 3rd temperature;
Described 3rd temperature is greater than the maximum boiling point of organic impurity, is less than or equal to the boiling point of described silicoorganic compound; Like this, guarantee that nearly all organic impurity is evaporated, make the organic impurity in the silicoorganic compound be left few as much as possible.Inevitably, in this step, part silicoorganic compound also may be evaporated.
Then, step S26 is performed: the cut collecting the second cut temperature, to obtain organic impurity and silicoorganic compound;
In this step, valve 19 can be opened, this part of organic impurity is collected in receiving bottle 16.May be mixed with the silicoorganic compound of part in this part of organic impurity, its categorised collection got off specially, the recovery being beneficial to silicoorganic compound is purified again.
Then, perform step S27: the mixture heating described silicoorganic compound and magnetic, Heating temperature maintains the 4th temperature, collect the cut of the 3rd cut temperature, obtain the silicoorganic compound that purity is greater than 99.9%, described 4th temperature is the Heating temperature of cut temperature-stable when the 3rd cut temperature.
In this step, valve 110 can be opened, this part silicone compound is collected in receiving bottle 17.
In above process, organic impurity to be vaporized and condensation collects in rectifying; And metal simple-substance in metallic impurity or metal oxide are adsorbed by magnetic, the negative electric base unity on metal ion and magnetic surface synthesizes chemical bond and is adsorbed, the general density ratio of metallic impurity that can not be adsorbed by magnetic is comparatively large, nor can be dissolved in and be vaporized in silicoorganic compound and be evaporated.So composition that be finally left in this step, that be collected in the cut in receiving bottle 17 is pure silicoorganic compound.
Embodiment three
Need the silicoorganic compound be purified to be Contained In Commercial OctamethylcyclotetraOnloxane (purity 98.0%) in the present embodiment, wherein main organic sila matter is hexamethyl cyclotrisiloxane etc., and metal ion total content is 8.5ppm.
3000g Contained In Commercial OctamethylcyclotetraOnloxane and 5g magnetic T6 are joined in rectifying still (12), stirs 3h at normal temperatures and pressures.Being evacuated to vacuum tightness is 20KPa, and magnetic agitation heater temperature is raised to 140 DEG C, by tower top 80-105 DEG C fraction collection in receiving bottle (15).After flowing out without cut, magnetic agitation heater temperature is increased to 150 DEG C, by tower top 105-106 DEG C fraction collection in receiving bottle (16).Until overhead fraction temperature-stable after 106 DEG C, by tower top 106 DEG C of fraction collections in receiving bottle (17).Sampling analysis, by octamethylcyclotetrasiloxane purity 99.96% in the known receiving bottle of GC and ICP-MS test result (17), metal ion content is less than 1ppb.
Embodiment four
Need the silicoorganic compound be purified to be technical grade trifluoro propyl cyclotrisiloxane (purity 98.5%) in the present embodiment, main organic sila matter is high boiling point organo-siloxane etc., and metal ion total content is 6.2ppm.
2500g technical grade trifluoro propyl cyclotrisiloxane and 8g magnetic Si47 are joined in rectifying still (12), at ambient pressure magnetic agitation heater temperature is raised to 40 DEG C and stirs 3h.Being evacuated to vacuum tightness is 4.5KPa, and magnetic agitation heater temperature is raised to 150 DEG C, by tower top 60-136 DEG C fraction collection in receiving bottle (15).After flowing out without cut, magnetic agitation heater temperature is increased to 160 DEG C, by tower top 136-137 DEG C fraction collection in receiving bottle (16).Until overhead fraction temperature-stable after 137 DEG C, by tower top 137 DEG C of fraction collections in receiving bottle (17).Sampling analysis, by trifluoro propyl cyclotrisiloxane purity 99.98% in the known receiving bottle of GC and ICP-MS test result (17), metal ion content is less than 1ppb.
In sum, the present invention effectively overcomes various shortcoming of the prior art and tool high industrial utilization.
Above-described embodiment is illustrative principle of the present invention and effect thereof only, but not for limiting the present invention.Any person skilled in the art scholar all without prejudice under spirit of the present invention and category, can modify above-described embodiment or changes.Therefore, such as have in art usually know the knowledgeable do not depart from complete under disclosed spirit and technological thought all equivalence modify or change, must be contained by claim of the present invention.
Claims (11)
1. a method of purification for silicoorganic compound, is characterized in that, the method for purification of described silicoorganic compound at least comprises:
Silicoorganic compound and magnetic are stirred at a first temperature and is formed with the mixture of organic silicon compound and magnetic;
Silicoorganic compound are extracted from the mixture of described silicoorganic compound and magnetic; Described magnetic is Fe
3o
4, Fe
3o
4tiO
2nH
2o or Fe
3o
4siO
2tiO
2nH
2one or more in O, wherein n=1 ~ 5.
2. the method for purification of silicoorganic compound according to claim 1, is characterized in that: the particle diameter of described magnetic is 5 μm ~ 20 μm.
3. the method for purification of silicoorganic compound according to claim 1, is characterized in that: adopt magnetic agitation well heater to carry out the stirring of described silicoorganic compound and magnetic, the time that stirring is carried out is more than or equal to 3h.
4. the method for purification of silicoorganic compound according to claim 1, is characterized in that: described first temperature is more than or equal to 25 DEG C, is less than the minimum boiling point of organic impurity.
5. the method for purification of silicoorganic compound according to claim 1, is characterized in that: described in extract silicoorganic compound method be distillation, rectifying or filtration.
6. the method for purification of silicoorganic compound according to claim 1, is characterized in that: adopt the mode of rectifying to extract silicoorganic compound from the mixture of described silicoorganic compound and magnetic, comprising:
Heat the mixture of described silicoorganic compound and magnetic, Heating temperature is the second temperature;
Vacuumize and carry out condensation;
Collect the cut of the first cut temperature, to obtain organic impurity;
Heat the mixture of described silicoorganic compound and magnetic, Heating temperature is warming up to the 3rd temperature;
Collect the cut of the second cut temperature, to obtain organic impurity and silicoorganic compound;
Heat the mixture of described silicoorganic compound and magnetic, Heating temperature maintains the 4th temperature, collect the cut of the 3rd cut temperature, obtain the silicoorganic compound that purity is greater than 99.9%, described 4th temperature is the Heating temperature of cut temperature-stable when the 3rd cut temperature.
7. the method for purification of silicoorganic compound according to claim 6, is characterized in that: adopt rectifying tower to carry out rectifying, described rectifying tower comprises rectifying still; Describedly silicoorganic compound and magnetic to be stirred at a first temperature and the operation of mixture of the described silicoorganic compound of described heating and magnetic is all carried out in rectifying still.
8. the method for purification of silicoorganic compound according to claim 6, is characterized in that: described second temperature is more than or equal to the boiling point of part organic impurity; Described 3rd temperature is greater than the maximum boiling point of organic impurity, is less than or equal to the boiling point of described silicoorganic compound; Described first cut temperature is between described first temperature and the second temperature; Described second cut temperature is less than or equal to described 3rd cut temperature.
9. the method for purification of silicoorganic compound according to claim 1, is characterized in that: before the mixture forming described silicoorganic compound and magnetic, also comprise the step knowing organic impurity in described silicoorganic compound.
10. the method for purification of silicoorganic compound according to claim 1, is characterized in that: before the mixture forming described silicoorganic compound and magnetic, also comprise the process being carried out by described magnetic activating, comprising:
Described magnetic and dilute nitric acid solution are shaken 3h under 50 DEG C of constant temperature, takes out magnetic;
Adopt ultrapure water by described magnetic cleaning to neutral;
By described magnetic in a vacuum, dry at 110 DEG C.
The method of purification of 11. silicoorganic compound according to claim 1, it is characterized in that: before the mixture forming described silicoorganic compound and magnetic, or after extracting silicoorganic compound, also comprise the step of the metal element content in the described silicoorganic compound of test.
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| 水溶性氧化铁纳米粒子及TiO2/Fe3O4复合粒子的制备及其吸附性能研究;万洪亮;《中国优秀硕士学位论文 工程科技Ⅰ辑》;20131215;第6-7页 * |
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| CN103896980A (en) | 2014-07-02 |
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