CN106501296B - The detection method of silicon hydrogen content in organosilicon polymer - Google Patents
The detection method of silicon hydrogen content in organosilicon polymer Download PDFInfo
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Abstract
The present invention relates to a kind of detection methods of silicon hydrogen content in organosilicon polymer, include the following steps：(1) internal standard substance solution is prepared：Internal standard compound is dissolved in non-deuterated solvent, internal standard substance solution is obtained；The internal standard compound is dioxane or metaformaldehyde；(2) sample to be tested：Internal standard substance solution and organosilicon polymer accurately are weighed, is stirred up to sample to be tested；(3) it measures：The sample to be tested is detected using Nuclear Magnetic Resonance, the peak area of the proton peak of the internal standard compound and the peak area of the proton peak of the organosilicon polymer is recorded, calculates to obtain the final product.The detection method of residual silicon hydrogen content in above-mentioned organosilicon polymer, Practical time-saving easy to operate；By selecting the non-deuterated solvent good to organosilicon polymer solubility property, a kind of rapid detection method for the silicon hydrogen content that detection limit is low, Repeatability is good, accuracy is high has been invented.
Description
Technical field
The present invention relates to chemical analysis technology fields, more particularly to a kind of detection of silicon hydrogen content in organosilicon polymer
Method.
Background technology
Organosilicon is known as the title of " industrial monosodium glutamate ", is widely used in building, electronic apparatus, volume with its excellent performance
Knit, automobile, machinery, leather, papermaking, coating, in the industries such as medicine.In recent years, with the rapid development of organosilicon industry, pass through
Hydrosilylation introduces different segment functional groups, research and development synthesized elastomer silicone, long-chain alkyl-silicone oil, polyether silicone oil and
The products such as chain alkyl polyethers co-modified silicone oil are widely used in each to impart the special performance of polysiloxanes
Field and industry.
The size of residual silicon hydrogen content is to control an important indicator of product quality in organosilicon polymer, is directly affected
The stability of product, therefore need to detect wherein remaining silicon hydrogen content, to improve product quality.Existing measurement silicon hydrogen content
Method mainly include chemical method, infra-red sepectrometry, mass spectrography and1H NMR internal standard methods, wherein chemical method is more ripe, but operates numerous
Trivial, efficiency is low, and makees solvent using toxic carbon tetrachloride；Patent application No. is 201310734091.7 is infrared in using
Spectrometer measures the analysis method of containing hydrogen silicone oil silicon hydrogen content, need to be that standard specimen draws silicon hydrogen with the containing hydrogen silicone oil of known silicon hydrogen content
Content (%) and peak area (the infrared signature absorption peak 2160cm of Si -- H bond-1Left and right) standard curve, quantified by external standard method silicon hydrogen
Content, but the substances such as cyanogen class, acetylenic and certain double bond compounds are in 2160cm-1There is absorption in left and right, influences measurement result, this point
Analysis method has certain limitation；It is control that mass spectrography, which needs the containing hydrogen silicone oil of accurate hydrogen content,；1H NMR internal standard methods are to be both needed to
It is solvent to want deuterated reagent, and deuterated reagent type is limited, and certain organosilicon polymers are insoluble in deuterated reagent, increase measurement
Difficulty, therefore, it is necessary to develop a kind of detection method that can meet residual silicon hydrogen content in organosilicon polymer.
Invention content
Based on this, the purpose of the present invention is to provide a kind of detection methods of residual silicon hydrogen content in organosilicon polymer.
Specific technical solution is as follows：
The detection method of silicon hydrogen content, includes the following steps in a kind of organosilicon polymer：
(1) internal standard substance solution is prepared
Internal standard compound is dissolved in non-deuterated solvent, internal standard substance solution is obtained；The internal standard compound is dioxane or metaformaldehyde；
(2) sample to be tested
Internal standard substance solution and organosilicon polymer accurately are weighed, is stirred up to sample to be tested；
(3) it measures
The sample to be tested is detected using Nuclear Magnetic Resonance, record the proton peak of the internal standard compound peak area and
The peak area of the proton peak of the organosilicon polymer, is calculated as follows to obtain the final product：
A in formulaMark：The peak area of internal standard compound proton peak；
ASample：The peak area of organosilicon polymer silicon proton peak；
mMark：The quality of internal standard substance solution, g；
mSample：The quality of organosilicon polymer, g；
MMark：The concentration of internal standard substance solution, wt%；
X：The ratio between proton number and molecular weight of internal standard compound.
In wherein some embodiments, the organosilicon polymer is selected from elastomer silicone, long-chain alkyl-silicone oil or poly-
Ether silicone oil or chain alkyl polyether modified silicon oil.
In wherein some embodiments, a concentration of 0.01wt%-0.1wt% of internal standard compound in the internal standard substance solution.
In wherein some embodiments, the non-deuterated solvent is selected from octamethylcy-clotetrasiloxane, five silica of decamethyl ring
Alkane or the dimethicone that viscosity is 50-100cst.
In wherein some embodiments, the mass ratio of the internal standard substance solution and the organosilicon polymer is 1:0.8-
1.2。
In wherein some embodiments, the Nuclear Magnetic Resonance is selected1The pulse train of H spectrums is measured.
Beneficial effects of the present invention are as follows：
The detection method of residual silicon hydrogen content in above-mentioned organosilicon polymer, Practical time-saving easy to operate；Pass through selection pair
The good non-deuterated solvent of organosilicon polymer solubility property has invented the silicon that a kind of detection limit is low, Repeatability is good, accuracy is high
The rapid detection method of hydrogen content.
Specific implementation mode
To facilitate the understanding of the present invention, below with reference to relevant drawings to invention is more fully described.In attached drawing
Give presently preferred embodiments of the present invention.But the present invention can realize in many different forms, however it is not limited to this paper institutes
The embodiment of description.Keep the understanding to the disclosure more thorough on the contrary, purpose of providing these embodiments is
Comprehensively.
Unless otherwise defined, all technical and scientific terms used in the present invention and the technical field for belonging to the present invention
The normally understood meaning of technical staff it is identical.It is specific to be intended merely to description for used term in the description of the invention
The purpose of embodiment, it is not intended that in the limitation present invention.Term "and/or" used in the present invention includes one or more related
Listed Items any and all combinations.
Embodiment 1
1, experimental drug and instrument
1.1 containing hydrogen silicone oil：It is 0.19% that chemical method, which detects silicon hydrogen content,
1.2 low glutinous silicone oil：Viscosity is the dimethicone of 50cst
1.3 metaformaldehyde (purity>99.0%)
1.4 elastomer silicone
1.5 magnetic stirring apparatus, magnetic rotor
1.6 electronic balance：Sensibility reciprocal 0.0001g
1.7 pipettes, graduated cylinder, measuring cup, 150mL disposable plastic bottles
The NMR of 1.8BRUKER 400MHZ, 5mm nuclear magnetic tube
2, operating procedure
The preparation of 2.1 internal standard substance solutions
In the accurate metaformaldehyde to 150mL disposable plastic bottles for weighing 0.05g (being accurate to 0.0001g), 100g is added
The low glutinous silicone oil of (being accurate to 0.0001g), shakes up, and is made into the internal standard substance solution that concentration is about 0.05wt%.
2.2 samples to be tested prepare
Accurately weigh 2.0g (being accurate to 0.0001g) internal standard substance solutions and 1.6g (being accurate to 0.0001g) organosilicone elastic
In body to measuring cup, magnetic rotor is added to stir 10min；It takes in 0.5mL to 5mm nuclear magnetic tubes, closes the lid, set aside for use.
2.3 instrument condition
Proton working frequency=400.13MHZ, DS=2, TD=65536, D1=1s, TD0=1, DE=6.5usec, TE
=299K, NS=256.25.0 DEG C of probe temperature.
2.4 measure and calculate：
NMR parameters are according to condition set, the sample to be tested being ready for is placed,1H-NMR is detected, with internal standard compound-metaformaldehyde matter
Sub- peaking displacement study 5.10ppm calibrations, unimodal positioned at 4.70~4.90ppm is silicon proton peak.With the peak at the sub- peak of internal standard substance
Area (AMark) it is the 1.0 peak area (A for determining benchmark integral silicon proton peakSample), calculate its silicon hydrogen content C (W by formula (1)t, %)：
A in formulaMark：The peak area of internal standard compound proton peak；
ASample：The peak area of organosilicon polymer silicon proton peak；
mMark：The quality of internal standard substance solution, g；
mSample：The quality of organosilicon polymer, g；
MMark：The concentration of internal standard substance solution, wt%；
X：The ratio between proton number and molecular weight of internal standard compound=1/15
3, repeated experiment
Prepare elastomer silicone sample by 2.2,1H-NMR is detected.It calculates its content and is shown in Table 1, this batch of elastomer silicone
Average residual silicon hydrogen content be 0.0041%.
The repeated experiment result of residual silicon hydrogen content in table .1 elastomer silicones
Pass through above-mentioned repeated experiment, it can be seen that the detection method of the application has repeatability well.
4, recovery of standard addition is tested
Weigh elastomer silicone (silicon hydrogen content be 0.0041wt%) respectively) and internal standard substance solution 5.0g (be accurate to
0.0001g) in measuring cup plus after magnetic rotor stirs evenly, 2.0g (being accurate to 0.0001g) is weighed respectively by the addition of table 22
The containing hydrogen silicone oil (silicon hydrogen content is 0.19wt%) of different quality, solution to be measured is made by 2.2,1H-NMR is detected, and calculates its silicon
Hydrogen content and recovery of standard addition, recovery of standard addition is between 84~110%.
The recovery of standard addition experimental result of residual silicon hydrogen content in table .2 elastomer silicones
| Experiment numbers | 1 | 2 | 3 | 4 |
| The silicon hydrogen amount g of addition | 0.0132 | 0.0332 | 0.0247 | 0.0280 |
| Theoretical silicon hydrogen content wt% | 0.00661 | 0.01455 | 0.01010 | 0.01045 |
| Survey silicon hydrogen content wt% | 0.00730 | 0.01221 | 0.01071 | 0.11030 |
| Recovery of standard addition % | 110.1 | 84.1 | 106.0 | 105.5 |
Embodiment 2：
Remaining silicon hydrogen content in elastomer silicone is detected, is with five oxygen alkane (D of decamethyl ring silicon5) it is solvent, first will
Dioxane (purity>99.8%, the ratio between proton number and molecular weight are 1/11) accurate with becoming 0.01wt%) internal standard compound it is molten
Liquid；Again by internal standard substance solution and elastomer silicone with 1：1.2 ratio is made into solution to be measured；By 2.3 instruments in embodiment 1
Condition and 2.4 operating procedure measure.It is calibrated with dioxane proton peak chemical shift 3.47ppm.It is calculated by formula (1) organic
Remaining silicon hydrogen content, repeated experiment the results are shown in Table 3 in silicone elastomer.
Embodiment 3：
Remaining silicon hydrogen content in long-chain alkyl-silicone oil is detected, is with octamethylcy-clotetrasiloxane (D4) it is solvent, first will
Dioxane (purity>99.8%, the ratio between proton number and molecular weight are 1/11) accurate with becoming 0.1wt%) internal standard compound it is molten
Liquid；Again by internal standard substance solution and long-chain alkyl-silicone oil with 1:0.9 ratio is made into solution to be measured；By 2.3 instruments in embodiment 1
Condition and 2.4 operating procedure measure.It is calibrated with dioxane proton peak chemical shift 3.47ppm.Long-chain is calculated by formula (1)
Residual silicon hydrogen content in alkyl-silicone oil, repeated experiment the results are shown in Table 3.
Embodiment 4：
Remaining silicon hydrogen content in polyether silicone oil is detected, is with decamethyl cyclosiloxane (D5) it is solvent, first by trimerization first
Aldehyde (purity>99.8%, the ratio between proton number and molecular weight are 1/15) accurate with becoming 0.01wt%) internal standard substance solution；Again
By internal standard substance solution and polyether silicone oil with 1:1 ratio is made into solution to be measured；By 2.3 instrument conditions and 2.4 in embodiment 1
Operating procedure measures.It is calibrated with metaformaldehyde chemical shift of proton 5.10ppm.Residual silicon in polyether silicone oil is calculated by formula (1)
Hydrogen content, repeated experiment the results are shown in Table 3.
Embodiment 5：
Remaining silicon hydrogen content in chain alkyl polyethers co-modified silicone oil is detected, is with octamethylcy-clotetrasiloxane (D4) be
Solvent, first by metaformaldehyde (purity>99.8%, the ratio between proton number and molecular weight are 1/15) accurate with as 0.05wt%)
Internal standard substance solution；Again by internal standard substance solution and sample with 1:1 ratio is made into sample to be tested；By 2.3 instruments in embodiment 1
Condition and 2.4 operating procedure measure.It is calibrated with metaformaldehyde chemical shift of proton 5.10ppm.Long alkane is calculated by formula (1)
Residual silicon hydrogen content in base polyethers co-modified silicone oil, repeated experiment the results are shown in Table 3.
Residual silicon hydrogen content repeated experiment result in table .3 organosilicon polymers
Pass through above-mentioned repeated experiment, it can be seen that the detection method of the application in detection organosilicon polymer for remaining
Silicon hydrogen content have well repeatability.
Each technical characteristic of embodiment described above can be combined arbitrarily, to keep description succinct, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, it is all considered to be the range of this specification record.
Several embodiments of the invention above described embodiment only expresses, the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection of the present invention
Range.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (4)
1. the detection method of silicon hydrogen content in a kind of organosilicon polymer, which is characterized in that include the following steps：
(1) internal standard substance solution is prepared
Internal standard compound is dissolved in non-deuterated solvent, internal standard substance solution is obtained；The internal standard compound is dioxane or metaformaldehyde；It is described
Non-deuterated solvent is selected from the dimethicone that octamethylcy-clotetrasiloxane, decamethylcyclopentaandoxane or viscosity are 50-100cst；
(2) sample to be tested
Internal standard substance solution and organosilicon polymer accurately are weighed, is stirred up to sample to be tested；The organosilicon polymer choosing
From elastomer silicone, long-chain alkyl-silicone oil, polyether silicone oil or chain alkyl polyether modified silicon oil；
(3) it measures
The sample to be tested is detected using Nuclear Magnetic Resonance, records the peak area of the proton peak of the internal standard compound and described
The peak area of the proton peak of organosilicon polymer, is calculated as follows to obtain the final product：
A in formulaMark：The peak area of internal standard compound proton peak；
ASample：The peak area of organosilicon polymer silicon proton peak；
mMark：The quality of internal standard substance solution, g；
mSample：The quality of organosilicon polymer, g；
MMark：The concentration of internal standard substance solution, wt%；
X：The ratio between proton number and molecular weight of internal standard compound.
2. detection method according to claim 1, which is characterized in that internal standard compound is a concentration of in the internal standard substance solution
0.01wt%-0.1wt%.
3. according to claim 1-2 any one of them detection methods, which is characterized in that the internal standard substance solution with it is described organic
The mass ratio of silicon polymer is 1:0.8-1.2.
4. according to claim 1-2 any one of them detection methods, which is characterized in that the Nuclear Magnetic Resonance is selected1H spectrums
Pulse train is measured.
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| CN110220931B (en) * | 2019-07-18 | 2022-04-26 | 东莞东阳光科研发有限公司 | Lithium salt solubility detection method |
| CN111879806A (en) * | 2020-07-23 | 2020-11-03 | 中蓝晨光成都检测技术有限公司 | Method for identifying alkane plasticizer-doped organic silicon product by nuclear magnetic resonance hydrogen spectrum |
| CN111812142B (en) * | 2020-07-24 | 2022-04-29 | 东莞东阳光科研发有限公司 | Method for detecting content of alkyl silicon compounds in lithium ion battery electrolyte |
| CN114113423A (en) * | 2021-12-07 | 2022-03-01 | 江西蓝星星火有机硅有限公司 | Device and method for quantitatively determining residual silicon hydrogen in organic silicon sample |
| CN115524412B (en) * | 2022-09-02 | 2024-05-28 | 江西蓝星星火有机硅有限公司 | Method for measuring content of terminal silicon hydrogen and chain silicon hydrogen in organic silicon |
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