CN110527098A - The post-processing approach and polysiloxanes of polysiloxanes synthesis - Google Patents
The post-processing approach and polysiloxanes of polysiloxanes synthesis Download PDFInfo
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Abstract
The invention discloses the post-processing approach and polysiloxanes of polysiloxanes synthesis.The post-processing approach of above-mentioned polysiloxanes synthesis, includes the following steps: the reaction material of polysiloxanes carrying out first time vacuum distillation；Active carbon is added in the reaction material after first time is evaporated under reduced pressure to be adsorbed；The reaction material after activated carbon adsorption is filtered, filtrate is obtained；The post-processing approach that polysiloxanes is synthesized by above-mentioned polysiloxanes is handled and is obtained.The post-processing approach of polysiloxanes synthesis of the present invention, can reduce the dosage of water and the wastewater flow rate of discharge.
Description
Technical field
The present invention relates to polysiloxanes synthesis technical fields, and in particular to the post-processing approach and poly- silicon of polysiloxanes synthesis
Oxygen alkane.
Background technique
Polysiloxanes is polymerized by silicon monomer, due to the special construction of polysiloxanes, makes it have some excellent objects
Reason and chemical property, such as excellent heat resistance, radiation resistance, heat-resisting quantity, oxidative resistance, resistance to chemical industry and metallurgy, aviation, boat
It, medical material marquis property, highly-breathable etc..Polysiloxanes be widely used in electrician and electronics, building, daily necessities, makeup
The fields such as product, weaving.
During synthesizing polysiloxanes, the presence of the impurity such as a large amount of acid, salt, such as acetic acid, sulfate, sulfonic acid are had
The low-boiling by-products generated in salt and reaction process, the presence of the impurity such as these acid, salt influence whether that polysiloxanes is producing again
Application in product needs to post-process reaction product.Traditional processing method is by largely washing, and gradient reduces
Its impurity content, until impurity content does not influence the application performance of product.But this method water resources consumption is big, can also generate
A large amount of waste water brings huge pollution to environment, seriously threatens the health of the mankind.Also document report inhales using active carbon
Attached technique reduces the impurity in polysiloxanes, but still then is reduced by the suction-operated of active carbon miscellaneous by massive laundering
Matter content not can be reduced the generation for beating a large amount of waste water of money.In today that environmental protection is increasingly taken seriously, traditional processing method is difficult
Think after.
Summary of the invention
Based on this, it is necessary to provide the polysiloxanes conjunctions that one kind can reduce the dosage of water and the wastewater flow rate of discharge by the present invention
At post-processing approach.
The present invention also provides a kind of polysiloxanes.
In order to achieve the object of the present invention, the invention adopts the following technical scheme:
A kind of post-processing approach of polysiloxanes synthesis, includes the following steps:
The reaction material of polysiloxanes is subjected to first time vacuum distillation；
Active carbon is added in the reaction material after first time is evaporated under reduced pressure to be adsorbed；
The reaction material after activated carbon adsorption is filtered, filtrate is obtained.
The post-processing approach of above-mentioned polysiloxanes synthesis, can be removed by the way of vacuum distillation and activated carbon adsorption
Impurity, the uses of water such as the low-boiling by-products generated in acid, salt and reaction process greatly reduce compared to traditional technology, save
A large amount of water resource, and a large amount of waste water will not be discharged, reduce the subsequent technique of processing waste water, reduces production cost；
It is detected, obtained polysiloxanes is had excellent performance, and shows that this method can replace traditional elution process.
In some of embodiments, the vacuum degree of the first time vacuum distillation is 0.06MPa-0.1MPa.
In some of embodiments, the temperature of the first time vacuum distillation is 50 DEG C -80 DEG C.
In some of embodiments, before the reaction material of polysiloxanes is carried out the step of being evaporated under reduced pressure for the first time, also
With following steps: water is added in the reaction material.
In some of embodiments, the addition quality of the water is the 1 ‰ -1% of the quality of the reaction material.
In some of embodiments, the reaction material by polysiloxanes carry out the step of being evaporated under reduced pressure for the first time with it is described
It is added between the step of active carbon is adsorbed in the reaction material after first time is evaporated under reduced pressure, also there are following steps:
Organic solvent is added in the reaction material after first time is evaporated under reduced pressure, material must be diluted.
The reaction material in some of embodiments, after the addition quality of the organic solvent and for the first time vacuum distillation
Mass ratio be 0.5-2:1.
In some of embodiments, the addition number of the active carbon is at least 2 times, after the completion of every primary absorption of addition again
It is added next time；The addition quality of each active carbon and the mass ratio of the reaction material after first time vacuum distillation are
0.8-1.2:100；The time of each activated carbon adsorption is 1h-10h, and when absorption is stirred.
In some of embodiments, the temperature of the activated carbon adsorption is 25 DEG C -40 DEG C.
In some of embodiments, it is added what active carbon was adsorbed in the reaction material after first time is evaporated under reduced pressure
After step, also there are following steps: the reaction material after activated carbon adsorption being filtered, filtrate is obtained.
In some of embodiments, the step of reaction material after activated carbon adsorption is filtered, obtains filtrate it
Afterwards, also there are following steps: the filtrate being carried out second and is evaporated under reduced pressure.
In some of embodiments, the vacuum degree of second of vacuum distillation is 0.06MPa-0.1MPa, temperature 50
℃-150℃。
The present invention also provides a kind of polysiloxanes, the post-processing approach synthesized by the polysiloxanes is handled and is obtained.
Specific embodiment
It to facilitate the understanding of the present invention, below will be to invention is more fully described.But the present invention can be to be permitted
Mostly different form is realized, however it is not limited to embodiment described herein.On the contrary, purpose of providing these embodiments is makes
It is more thorough and comprehensive to the understanding of the disclosure.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.
The present invention provides a kind of post-processing approach of polysiloxanes synthesis, includes the following steps:
Depickling step: the reaction material of polysiloxanes is subjected to first time vacuum distillation；
Steps of activated carbon adsorption: active carbon is added in the reaction material after first time is evaporated under reduced pressure and is adsorbed；
Filtration step: the reaction material after activated carbon adsorption is filtered, filtrate is obtained.
This method first passes through to be generated in the biggish acid of acetic acid same-size ratio and reaction process in vacuum distillation removing reaction material
Low-boiling by-products, then the impurity such as remaining micro acid, salt are removed by way of activated carbon adsorption, so that wherein
Most of impurity can remove, compared to a traditional post-processing approach is played, greatly reduce the usage amount of water, save water money
Source；A large amount of waste water would not be also generated without using a large amount of water, to reduce the discharge of waste water, protect environment, reduce place
The subsequent technique for managing waste water, reduces production cost；Through detecting, it is had excellent performance using the polysiloxanes that this method is handled,
Show that this method can replace traditional elution process.
The vacuum degree of vacuum distillation is 0.06MPa-0.1MPa for the first time.I.e. vacuum degree can be set is in vacuum degree
Between 0.06MPa-0.1MPa, it can be adapted to the boiling point of acid therein, realize the purpose that impurity acid is removed under reduced pressure.
The temperature of vacuum distillation is 50 DEG C -80 DEG C for the first time.The temperature of vacuum distillation is too small, and distillation process progress is too slow,
It can delay treatment progress, and temperature is excessively high, can make that side reaction occurs in reaction material, influences the generation of polysiloxanes.Reaction material
It is evaporated under reduced pressure at such a temperature, vacuum degree can be cooperated, be adapted to the boiling point of impurity acid therein, impurity is removed under reduced pressure in realization
The purpose of acid, and will not influence the polysiloxanes of generation.
In one embodiment, before the reaction material of polysiloxanes is carried out the step of being evaporated under reduced pressure for the first time, also have dilute
It releases step: water being added in reaction material.When water in reaction material system is fewer, steaming for impurity will affect, water is added can be with
Impurity therein is dissolved, so that taking away impurity therein when water evaporation, such impurity is easier to steam；And it is convenient for after water is added
Active carbon is adsorbed, and adsorption efficiency is improved.
The addition quality of water is the 1 ‰ -1% of the quality of reaction material.The ratio of impurity in reaction material is held in centainly
In range, therefore, it is necessary to the amounts for the water for being determined to be added according to the total amount of reaction material, under the premise of saving water resource,
Achieve the purpose that impurity is taken away in distillation.
In one embodiment, the reaction material of polysiloxanes is subjected to the step of being evaporated under reduced pressure for the first time and decompression is steamed in first time
It is added between the step of active carbon is adsorbed in reaction material after evaporating, also there are following steps: after first time is evaporated under reduced pressure
Reaction material (taking off low material) in be added organic solvent, material must be diluted.Organic solvent diluting is added, dissolves polysiloxanes therein,
It convenient for later period filtering, then is carried out absorbing acid and salt therein with active carbon, the solvent of addition will not influence active carbon except impurity
Process.Organic solvent herein selects the solvent that can be mixed with polysiloxanes, when preferably selection polysiloxanes reacts
Reactant organic solvent, such later period are easier except solvent.For example, the organic solvent is toluene solution
The mass ratio of reaction material (taking off low material) after the addition quality of organic solvent and for the first time vacuum distillation is 0.5-
2:1.The ratio of polysiloxanes and impurity in reaction material be held in it is a certain range of, be added excessive later period remove it is organic molten
The process of agent can be longer, very few to have undissolved polysiloxanes, and the organic solvent of above-mentioned quality is added, and is saving organic solvent
Under the premise of, polysiloxanes can be dissolved.Therefore preferably the additional amount of organic solvent is controlled within the above range.
The addition quality of active carbon and the mass ratio of dilution material are 0.8-1.2:100.Similarly, active carbon is added very little
Impurity therein can be absorbed by being difficult to ensure, active carbon is kept within the above range, can be while saving active carbon, most
Absorb to big degree the impurity such as acid therein, salt.
The temperature of activated carbon adsorption is 25 DEG C -40 DEG C.When activated carbon adsorption, the micropore that temperature enters active carbon to impurity has
It influences, within the above range, micropore is stronger to acid, the adsorption capacity of salt for temperature.
Active carbon therein can be one or more of coaly activated carbon, cocoanut active charcoal and wood activated charcoal.It is living
Property charcoal granular size be -400 mesh of 10 mesh.Active carbon in adsorbing contaminant, need to guarantee its internal capillary in OK range, it is micro-
Kong Tai little, impurity are difficult to adsorb, and micropore is excessive, after impurity enters micro channel, it is easy to it is back in reaction material, it is therefore, living
Property charcoal particle keep within the above range, it is ensured that adsorption effect, reduce adsorption time.
The addition number of active carbon is at least 2 times, is added next time after the completion of every primary absorption of addition.Repeatedly absorption can
To guarantee preferable adsorption effect.Such as 2-5 active carbon is added and is adsorbed.
The time of each activated carbon adsorption is 1h-10h, and when absorption is stirred.It needs to remove after active carbon use,
The adsorption time can make active carbon play its maximum utility, to reduce the waste of resource.
Filtration step is to filter twice, uses large aperture filter paper or filter cloth for the first time, second using small-bore filter paper or
Filter cloth.The mesh of filter paper or filter cloth therein is -300 mesh of 10 mesh.Filter cloth is terylene filter cloth, polytetrafluoroethylene (PTFE) filter cloth, polyphenylene sulfide
The combination of one or both of ether fiber filter cloth and PP filter cloth.Can remove impurity therein, and touch the acid in impurity,
When salt, the property of filter cloth is more stable.
In one embodiment, after the step of being filtered the reaction material (absorption is expected) after activated carbon adsorption, also have
Vacuum removes solvent step: filtrate being carried out second and is evaporated under reduced pressure.Second of vacuum distillation, which can remove in the reaction material of front, to be added
The low-boiling point materials such as the solvent of reaction are had neither part nor lot in water, organic solvent and the reaction material entered, the purity of obtained polysiloxanes
It is higher.
Wherein, the vacuum degree of second of vacuum distillation is 0.06MPa-0.1MPa.The temperature of second of vacuum distillation is 50
℃-150℃.Above-mentioned vacuum degree and at a temperature of, water therein, organic solvent etc. can remove.
The present invention also protects a kind of polysiloxanes, and the post-processing approach synthesized by above-mentioned polysiloxanes is handled and obtained.
Hereinafter embodiments of the present invention will be further illustrated by several embodiments.
Embodiment one
The post-processing approach of the synthesis of polysiloxanes described in the present embodiment, including depickling step, dilution step, active carbon are inhaled
Attached step, filtration step and vacuum remove solvent step.
Polysiloxanes preparation step are as follows: in 4 necks for being furnished with thermometer, mechanical agitator, isobaric dropping funel and condenser
182.29 aminomethyl phenyl dimethoxysilanes, 161.2g1,1,3,3 tetramethyl disiloxane and the 1g concentrated sulfuric acid are added in 1L flask,
Under agitation, 240g glacial acetic acid is added dropwise dropwise in 30min.After the addition was complete, liquid is heated under agitation
Mixture maintains temperature at 50 DEG C to 50 DEG C.After having added, react 2 hours.The reaction material for obtaining polysiloxanes, contains phenyl
Silicone product.Impurity contains more acetic acid, a small amount of sulfuric acid and generates some low-boiling by-products after the reaction was completed.
Post-processing approach specifically:
1, depickling step: 1g water being added into reaction material, and vacuum is deviate under the conditions of temperature 60 C and vacuum degree 0.09MPa
The low-boiling by-products generated in acetic acid and reaction process enter collector by condenser.Collector is transferred to storage tank, remaining anti-
It should expect to obtain de- low material.
2, at room temperature toward the addition of 1:1 in mass ratio toluene solution in low material is taken off, material must dilution step: be diluted.
3, steps of activated carbon adsorption: under the conditions of 30 DEG C, 1% active carbon of dilution material total amount being added into dilution material,
Stirring 4 hours, then toward the active carbon for diluting addition 1% in material, stir 4 hours, material must be adsorbed.
4, filtration step: at room temperature, by absorption material by Buchner funnel coarse filtration one time, filtering using sand core funnel,
Obtain filtrate.
5, vacuum removes solvent step: under the conditions of 120 DEG C of temperature and vacuum degree 0.08MPa, filter vacuum deviates from toluene, water
And the low-boiling-point substances such as low-boiling by-products, obtain finished product polysiloxanes.
Embodiment two
The post-processing approach of the synthesis of polysiloxanes described in the present embodiment, including depickling step, dilution step, active carbon are inhaled
Attached step, filtration step and vacuum remove solvent step.
The preparation step of polysiloxanes are as follows: in 4 equipped with thermometer, mechanical agitator, isobaric dropping funel and condenser
136.22g methyltrimethoxysilane, 241.74g1,1,3,3 tetramethyl disiloxane and the 1g concentrated sulfuric acid are added in neck 1L flask,
Under agitation, 360g glacial acetic acid is added dropwise dropwise in 30min.After the addition was complete, liquid is heated under agitation
Mixture maintains temperature at 50 DEG C -60 DEG C to 60 DEG C.After having added, 2h is reacted.Obtain polysiloxanes reaction material.Reaction is completed
Rear impurity contains more acetic acid, a small amount of sulfuric acid and generates some low-boiling by-products.
Post-processing approach specifically:
1, depickling step: 1g water being added into reaction material, and vacuum is deviate under the conditions of 80 DEG C of temperature and vacuum degree 0.06MPa
The low-boiling by-products generated in acetic acid and reaction process enter collector by condenser.Collector is transferred to storage tank.It is remaining anti-
It should expect to obtain de- low material.
2, at room temperature toward the addition of 2:1 in mass ratio toluene solution in low material is taken off, material must dilution step: be diluted.
3, under the conditions of 25 DEG C, 1.2% active carbon of total amount, stirring 5 steps of activated carbon adsorption: are added into dilution material
Hour, then toward the active carbon for diluting addition 1.2% in material, stir 3 hours, material must be adsorbed.
4, filtration step: at room temperature, by absorption material by Buchner funnel coarse filtration one time, filtering using sand core funnel,
Obtain filtrate.
5, vacuum removes solvent step: under the conditions of 110 DEG C of temperature and vacuum degree are 0.09MPa, filter vacuum deviates from low boiling
Object obtains finished product polysiloxanes.
Embodiment three
The post-processing approach of the synthesis of polysiloxanes described in the present embodiment, including depickling step, dilution step, active carbon are inhaled
Attached step, filtration step and vacuum remove solvent step.
Polysiloxanes preparation step are as follows: in 4 necks for being furnished with thermometer, mechanical agitator, isobaric dropping funel and condenser
182.29 aminomethyl phenyl dimethoxysilanes, 161.2g1,1,3,3 tetramethyl disiloxane and the 1g concentrated sulfuric acid are added in 1L flask,
Under agitation, 240g glacial acetic acid is added dropwise dropwise in 30min.After the addition was complete, liquid is heated under agitation
Mixture maintains temperature at 48 DEG C -55 DEG C to 50 DEG C.After having added, react 2 hours.Obtain the reaction material of polysiloxanes.Reaction
Rear impurity is completed to contain more acetic acid, a small amount of sulfuric acid and generate some low-boiling by-products.
Post-processing approach specifically:
1, depickling step: reaction material vacuum abjection acetic acid and reaction process under the conditions of temperature 50 C and vacuum degree 0.1MPa
The low-boiling by-products of middle generation enter collector by condenser.Collector is transferred to storage tank, and remaining reaction material must take off low material.
2, at room temperature toward the addition of 0.5:1 in mass ratio toluene solution in low material is taken off, material must dilution step: be diluted.
3, under the conditions of 40 DEG C, 0.8% activity of dilution material total amount steps of activated carbon adsorption: is added into dilution material
Charcoal stirs 8 hours, then 1% active carbon is added into dilution material, stirs 3 hours, must adsorb material.
4, filtration step: at room temperature, by absorption material by Buchner funnel coarse filtration one time, filtering using sand core funnel,
Obtain filtrate.
5, vacuum removes solvent step: under the conditions of 150 DEG C of temperature and vacuum degree are 0.06MPa, filter vacuum deviates from low boiling
Object obtains finished product polysiloxanes.
Example IV
The post-processing approach of the synthesis of polysiloxanes described in the present embodiment, including depickling step, steps of activated carbon adsorption, mistake
It filters step and vacuum removes solvent step.
Polysiloxanes preparation step are as follows: in 4 necks for being furnished with thermometer, mechanical agitator, isobaric dropping funel and condenser
182.29 aminomethyl phenyl dimethoxysilanes, 161.2g1,1,3,3 tetramethyl disiloxane and the 1g concentrated sulfuric acid are added in 1L flask,
Under agitation, 240g glacial acetic acid is added dropwise dropwise in 30min.After the addition was complete, liquid is heated under agitation
Mixture maintains temperature at 48 DEG C -55 DEG C to 50 DEG C.After having added, react 2 hours.Obtain the reaction material of polysiloxanes.Reaction
Rear impurity is completed to contain more acetic acid, a small amount of sulfuric acid and generate some low-boiling by-products.
Post-processing approach specifically:
1, depickling step: 6g water is added into reaction material, reaction material is under the conditions of temperature 70 C and vacuum degree are 0.08MPa
The low-boiling by-products generated in vacuum abjection acetic acid and reaction process, enter collector by condenser.Collector is transferred to
Storage tank, remaining reaction material must take off low material.
2, steps of activated carbon adsorption: under the conditions of 30 DEG C, being added 1% active carbon for taking off low material total amount toward taking off in low material,
Stirring 10 hours, then toward the active carbon for diluting addition 1% in material, stir 1 hour, material must be adsorbed.
3, filtration step: at room temperature, by absorption material by Buchner funnel coarse filtration one time, filtering using sand core funnel,
Obtain filtrate.
4, vacuum removes solvent step: under the conditions of temperature 50 C and vacuum degree 0.1MPa, filter vacuum deviates from low-boiling-point substance, obtains
To finished product polysiloxanes.
Embodiment five
Polysiloxanes described in the present embodiment synthesis post-processing approach, including depickling step, steps of activated carbon adsorption and
Filtration step.
Polysiloxanes preparation step are as follows: in 4 necks for being furnished with thermometer, mechanical agitator, isobaric dropping funel and condenser
182.29 aminomethyl phenyl dimethoxysilanes, 161.2g1,1,3,3 tetramethyl disiloxane and the 1g concentrated sulfuric acid are added in 1L flask,
Under agitation, 240g glacial acetic acid is added dropwise dropwise in 30min.After the addition was complete, liquid is heated under agitation
Mixture maintains temperature at 48 DEG C -55 DEG C to 50 DEG C.After having added, react 2 hours.Obtain the reaction material of polysiloxanes.Reaction
Rear impurity is completed to contain more acetic acid, a small amount of sulfuric acid and generate some low-boiling by-products.
Post-processing approach specifically:
1, vacuum abjection under the conditions of temperature 60 C and vacuum degree 0.09MPa after 1g water depickling step: is added in reaction material
The low-boiling by-products generated in acetic acid and reaction process enter collector by condenser.Collector is transferred to storage tank, remaining anti-
It should expect to obtain de- low material.
2, steps of activated carbon adsorption: under the conditions of 30 DEG C, being added 1% active carbon for taking off low material total amount toward taking off in low material,
Stirring 4 hours, then toward the active carbon for diluting addition 1% in material, stir 4 hours, material must be adsorbed.
3, filtration step: at room temperature, by absorption material by Buchner funnel coarse filtration one time, filtering using sand core funnel,
Obtain filtrate.
Comparative example one
The post-processing approach of the synthesis of polysiloxanes described in the comparative example, including water-washing step.
Polysiloxanes preparation step are as follows: in 4 necks for being furnished with thermometer, mechanical agitator, isobaric dropping funel and condenser
182.29 aminomethyl phenyl dimethoxysilanes, 161.2g1,1,3,3 tetramethyl disiloxane and the 1g concentrated sulfuric acid are added in 1L flask,
Under agitation, 240g glacial acetic acid is added dropwise dropwise in 30min.After the addition was complete, liquid is heated under agitation
Mixture maintains temperature at 48 DEG C -55 DEG C to 50 DEG C.After having added, react 2 hours.Obtain the reaction material of polysiloxanes.
Water-washing step are as follows: under the conditions of 30 DEG C, 1 times of the deionized water of otal investment into reaction material is stirred 30 minutes,
2 hours are stood, lower layer's water phase is removed.The deionized water of equivalent is put into again, is stirred 30 minutes, stands 2 hours, removes lower water
Phase.It washes 6 times repeatedly, obtains final product.
Comparative example two
The post-processing approach of the synthesis of polysiloxanes described in the comparative example, including dilution step, water-washing step and vacuum are removed
Solvent step.
Polysiloxanes preparation step are as follows: in 4 necks for being furnished with thermometer, mechanical agitator, isobaric dropping funel and condenser
182.29 aminomethyl phenyl dimethoxysilanes, 161.2g1,1,3,3 tetramethyl disiloxane and the 1g concentrated sulfuric acid are added in 1L flask,
Under agitation, 240g glacial acetic acid is added dropwise dropwise in 30min.After the addition was complete, liquid is heated under agitation
Mixture maintains temperature at 48 DEG C -55 DEG C to 50 DEG C.After having added, react 2 hours.Obtain the reaction material of polysiloxanes.
1, at room temperature toward the addition of 1:1 in mass ratio toluene solution in low material is taken off, material must dilution step: be diluted.
2, water-washing step: under the conditions of 30 DEG C, into dilution material, 1 times of deionized water of otal investment, is stirred 30 minutes,
2 hours are stood, lower layer's water phase is removed.The deionized water of equivalent is put into again, is stirred 30 minutes, stands 2 hours, removes lower water
Phase.It washes 6 times repeatedly, obtains final product.
3, vacuum removes solvent step: under the conditions of 120 DEG C of temperature and vacuum degree 0.09MPa, washing material vacuum deviates from low boiling
Object.Obtain finished product polysiloxanes.
Below by testing example one to embodiment five and the poly- silicon oxygen of the obtained finished product of comparative example one and comparative example two
The conductivity of alkane, test result are shown in Table one.
Table one
| Conductivity us/cm | |
| Embodiment one | 1.37 |
| Embodiment two | 1.45 |
| Embodiment three | 1.50 |
| Example IV | 1.58 |
| Embodiment five | 2.57 |
| Comparative example one | 6.08 |
| Comparative example two | 5.89 |
As can be seen from table 1, for embodiment one to the polysiloxanes of embodiment five, conductivity is significantly less than comparative example one
With comparative example two, illustrate that embodiment one to the polysiloxanes stability of embodiment five is apparently higher than comparative example one and comparative example two,
Product after polysiloxanes cooperation, thermal stability and storage performance improve, excellent combination property.
And embodiment three is plus water, conductivity is slightly larger than embodiment one, illustrates after water is not added, impurity when vacuum distillation
Band extracting rate reduces；The non-solubilizer of example IV dissolves polysiloxanes, and conductivity is greater than embodiment one and embodiment two, illustrates not
After solubilizer, impurity is not easy to be tightly held by activated carbon；The non-solubilizer of embodiment five, also non-vacuum removes solvent, and conductivity is big at this time
Embodiment in front illustrates that the removal of impurity in the method is less than preceding embodiment.
In addition, comparing comparative example one and comparative example two, the water consumption of each embodiment greatly reduces, simultaneously, it is possible to reduce row
Wastewater flow rate out.
Certainly, above-described embodiment and comparison illustrate the example for preparing phenyl polysiloxane, which can also fit
It should be in the preparation method of other polysiloxanes.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Protect range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (11)
1. a kind of post-processing approach of polysiloxanes synthesis, which comprises the steps of:
The reaction material of polysiloxanes is subjected to first time vacuum distillation；
Active carbon is added in the reaction material after first time is evaporated under reduced pressure to be adsorbed；
The reaction material after activated carbon adsorption is filtered, filtrate is obtained.
2. the post-processing approach of polysiloxanes synthesis according to claim 1, which is characterized in that the first time decompression is steamed
The vacuum degree evaporated is 0.06MPa-0.1MPa.
3. the post-processing approach of polysiloxanes synthesis according to claim 1 or 2, which is characterized in that the first time subtracts
The temperature of pressure distillation is 50 DEG C -80 DEG C.
4. the post-processing approach of polysiloxanes according to claim 1 synthesis, which is characterized in that by the anti-of polysiloxanes
Before should expecting to carry out the step of being evaporated under reduced pressure for the first time, also there are following steps: water is added in the reaction material.
5. the post-processing approach of polysiloxanes synthesis according to claim 4, which is characterized in that the addition quality of the water
It is the 1 ‰ -1% of the quality of the reaction material.
6. the post-processing approach of polysiloxanes according to claim 1 synthesis, which is characterized in that described by polysiloxanes
Reaction material carries out the step of being evaporated under reduced pressure for the first time and activity is added in the reaction material after first time is evaporated under reduced pressure
Between the step of charcoal is adsorbed, also with following steps: being added in the reaction material after first time is evaporated under reduced pressure organic
Solvent must dilute material.
7. the post-processing approach of polysiloxanes synthesis according to claim 6, which is characterized in that the organic solvent adds
The mass ratio of the reaction material after entering quality and being evaporated under reduced pressure for the first time is 0.5-2:1.
8. the post-processing approach of polysiloxanes synthesis according to claim 1, which is characterized in that the addition of the active carbon
Number is at least 2 times, is added next time after the completion of every primary absorption of addition；The addition quality and first of each active carbon
The mass ratio of the reaction material after secondary vacuum distillation is 0.8-1.2:100；The time of each activated carbon adsorption is 1h-
10h, when absorption, are stirred.
9. the post-processing approach of polysiloxanes synthesis according to claim 1, which is characterized in that after by activated carbon adsorption
Reaction material the step of being filtered, obtaining filtrate after, also there are following steps: the filtrate being carried out second and is depressurized
Distillation.
10. the post-processing approach of polysiloxanes synthesis according to claim 9, which is characterized in that second of decompression
The vacuum degree of distillation is 0.06MPa-0.1MPa, and temperature is 50 DEG C -150 DEG C.
11. a kind of polysiloxanes, which is characterized in that the post-processing synthesized by the described in any item polysiloxanes of claim 1-10
Method is handled and is obtained.
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| CN112961356A (en) * | 2021-02-05 | 2021-06-15 | 东莞市贝特利新材料有限公司 | Post-treatment method of polysiloxane |
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