CN112683728A - Si-H content detection device and Si-H content detection method - Google Patents
Si-H content detection device and Si-H content detection method Download PDFInfo
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- CN112683728A CN112683728A CN202011513637.2A CN202011513637A CN112683728A CN 112683728 A CN112683728 A CN 112683728A CN 202011513637 A CN202011513637 A CN 202011513637A CN 112683728 A CN112683728 A CN 112683728A
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- 238000001514 detection method Methods 0.000 title claims abstract description 26
- 230000007246 mechanism Effects 0.000 claims abstract description 51
- 238000006243 chemical reaction Methods 0.000 claims abstract description 46
- 238000004321 preservation Methods 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000007789 sealing Methods 0.000 claims abstract description 9
- 239000007789 gas Substances 0.000 claims description 84
- 239000007788 liquid Substances 0.000 claims description 45
- 229910052739 hydrogen Inorganic materials 0.000 claims description 24
- 239000001257 hydrogen Substances 0.000 claims description 23
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical group [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- -1 polysiloxane Polymers 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 229920001296 polysiloxane Polymers 0.000 claims description 11
- 239000000126 substance Substances 0.000 claims description 11
- 239000003513 alkali Substances 0.000 claims description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 229920001577 copolymer Polymers 0.000 claims description 6
- 238000006459 hydrosilylation reaction Methods 0.000 claims description 5
- 239000012491 analyte Substances 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 2
- 239000002585 base Substances 0.000 claims 1
- 238000005259 measurement Methods 0.000 abstract description 9
- 239000003921 oil Substances 0.000 description 10
- 235000019198 oils Nutrition 0.000 description 10
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 7
- 239000004721 Polyphenylene oxide Substances 0.000 description 6
- 229920000570 polyether Polymers 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 101100298225 Caenorhabditis elegans pot-2 gene Proteins 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 1
- 239000004264 Petrolatum Substances 0.000 description 1
- 229920005830 Polyurethane Foam Polymers 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229940066842 petrolatum Drugs 0.000 description 1
- 235000019271 petrolatum Nutrition 0.000 description 1
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Abstract
The invention provides a device and a method for detecting Si-H content, and relates to the technical field of gas content analysis. The device comprises a reaction mechanism, a metering mechanism and a heat preservation device, wherein the metering mechanism comprises a shell, and a gas storage device and a gas metering device which are arranged in the shell, the gas storage device is communicated with the gas metering device, the gas storage device is provided with one end extending out of the shell and is in sealing connection with a gas outlet of the reaction mechanism, the gas metering device is provided with scale marks, and a space for containing a heat preservation medium is arranged in the shell. The detection device for the Si-H content provided by the invention has the advantages that the gas storage device and the gas metering device are communicated and designed into a whole, the device is simplified, the measurement is more convenient, the analysis time is reduced, the analysis accuracy is greatly improved, and the repeatability is better.
Description
Technical Field
The invention relates to the technical field of gas content analysis, in particular to a device and a method for detecting Si-H content.
Background
The polyether modified siloxane is a high-efficiency surfactant, takes hydrophobic low-hydrogen polysiloxane and hydrophilic allyl polyether as raw materials, and prepares polysiloxane with polyether at a side chain or two ends through hydrosilylation reaction, so that the polysiloxane has good stability, can effectively improve the compatibility of a polyurethane foaming system, and further improves the cell structure of polyurethane foam. Wherein the amount of Si-H remaining after the low-hydrogen polysiloxane participates in the hydrosilylation reaction has an important influence on monitoring the degree of reaction progress and the application properties of the synthesized sample.
Patent CN203191275U discloses a device for measuring and analyzing hydrogen content in hydrogen-containing silicone oil, which is formed by connecting a sample injection mechanism, a reaction mechanism, a gas storage mechanism and a metering structure with scales and an open top. This patent changes traditional stirring reaction mechanism into automatic stirring by manual rocking, and the reading design is hydraulic balance reading mode simultaneously, has improved the accuracy of analysis to a very big extent. However, the problems that the device for measuring and analyzing the hydrogen content is complex, the requirement of a plurality of structures for air tightness is high, and the like exist, so that the analysis error is large, and the data repeatability is poor.
CN108490110A and CN207439856U disclose an analytical device capable of accurately detecting Si — H, in which the analytical device is simplified, connection of a plurality of mechanisms is avoided, and airtightness of the device is improved. However, the problems of large analysis error ratio and poor data repeatability still exist.
In view of this, the invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a device and a method for detecting Si-H content.
In order to solve the problems of large detection and analysis errors and poor repeatability, the invention provides a novel detection device for the content of Si-H, the device is designed to communicate a gas storage device with a gas metering device, namely the gas storage device and the gas metering device are designed into a whole, so that the connection of a plurality of mechanisms is avoided, and the integral gas tightness of the detection device is improved.
The invention is realized by the following steps:
a detection device for Si-H content comprises a reaction mechanism, a metering mechanism and a heat preservation device, wherein the metering mechanism comprises a shell, and a gas storage device and a gas metering device which are arranged in the shell;
the heat preservation device is arranged at the bottom of the reaction mechanism.
The gas storage device and the gas metering device are communicated to be integrated, so that the gas storage device and the gas metering device are improved in airtightness. Meanwhile, the gas storage device and the gas metering device are arranged in a shell, and a heat preservation medium is introduced into the shell, so that the gas storage device and the gas metering device are in a constant temperature environment.
The bottom of the reaction mechanism is provided with a heat preservation device to preserve heat of the whole reaction process so as to improve the accuracy of analysis. Hydrogen generated by the reaction directly enters the gas storage device, certain air pressure is given to the metering liquid in the gas metering device, so that the liquid level of the metering liquid is raised under the action of generated gas, the volume of the gas generated by the reaction can be obtained according to the difference value of the liquid levels before and after the reaction, and the Si-H content is calculated according to a calculation formula of the Si-H content.
The arrangement of the heat insulation medium, the shell and the heat insulation device avoids the influence of the external temperature on the reaction degree of the materials on one hand, and ensures the identity of the reaction degree; on the other hand, the influence of the external temperature on the gas volume is effectively avoided, and the accuracy of the detection result is ensured.
The heat preservation medium can be selected from water, steam, water gas and other heat preservation media. In other embodiments, the heat insulating medium may be adaptively adjusted as needed, and is not limited to the range of the heat insulating medium provided by the present invention.
The graduation mark of the gas metering device can be selected to be a division value of 0.02ml, and can also be selected to be a division value of 0.5ml, 0.1ml or 1ml as long as the gas metering can be satisfied.
The scale marks can also be provided with the lowest scale marks according to requirements.
The volume of the gas metering device can be any one of 10-100ml, and in practical implementation, the gas metering device can be adaptively adjusted according to needs.
In a preferred embodiment of the present invention, an accommodating device for accommodating the metering liquid is disposed at an end of the gas metering device away from the gas storage device.
The metering liquid is a liquid which does not react with hydrogen, such as water, ethanol, milk and oil substances. The oil substance can be selected from soybean oil, oleum Sesami, oleum Arachidis Hypogaeae, and oleum Rapae. In other embodiments, the metering liquid may be adaptively selected according to the requirement, and is not limited to the types of metering liquids defined above in the present invention.
In a preferred embodiment of the present invention, the gas storage device is a gas connection pipe, and the gas metering device is a liquid metering pipe.
In another embodiment, the gas storage device and the gas metering device are not limited to tubular shapes, and may have other shapes.
In a preferred embodiment of the present invention, one end of the gas connecting tube is fixedly connected or detachably connected to one end of the liquid metering tube. Before use, the two parts are assembled and kept in sealing connection.
Preferably, the gas storage device and the gas metering device are both U-shaped pipes, and the gas storage device is hermetically connected with one end of the gas metering device;
preferably, the gas storage means and the gas metering means are integrally formed.
In a preferred embodiment of the present invention, the accommodating device extends to the outside of the housing, and an end of the accommodating device away from the liquid outlet is open.
The containing device can be selected to contain a bottle, the top end of the containing bottle is open, and the bottom end of the containing bottle is communicated with the gas metering device. The containing device has the functions of: after the reaction takes place, certain atmospheric pressure is given to the measurement liquid to hydrogen for the liquid level of measurement liquid risees gradually, sets up accommodate device in order to prevent that measurement liquid from dashing out gaseous metering device.
In a preferred embodiment of the present invention, the outer wall of the casing is provided with an insulating medium inlet and an insulating medium outlet.
In a preferred embodiment of the present invention, the reaction mechanism is a flask. In another embodiment, the reaction mechanism may be a reaction cup, a reaction tube, or the like, and is not limited to the above-described structure provided by the present invention.
In a preferred embodiment of the present invention, the heat-insulating device is a constant-temperature water bath, a constant-temperature oil bath, or a constant-temperature oil bath.
In a preferred embodiment of the present invention, a stirring mechanism is further disposed at the bottom of the heat preservation device; preferably, the stirring mechanism is a magnetic stirrer.
A method for detecting Si-H content by using a Si-H content detection device comprises the following steps: placing the object to be measured and alkali liquor into a reaction mechanism, introducing metering liquid into a gas metering device, then hermetically connecting a gas storage device of the metering mechanism with a gas outlet of the reaction mechanism, obtaining the volume V of hydrogen generated by reaction according to the liquid level change of the gas metering device before and after the reaction, and obtaining the content of Si-H according to the formula (1):
formula (1):
v is the volume (ml) of hydrogen generated by the reaction, m is the mass (g) of the substance to be measured, and t is the holding temperature (DEG C) of the holding device.
The liquid level of the metering liquid is not lower than the lowest scale of the gas metering mechanism, and the metering liquid is used for sealing and marking, so that hydrogen leakage is avoided.
In a preferred embodiment of the present invention, the analyte is polyether-modified siloxane or hydrogen-containing polysiloxane, and the alkali solution is strong alkali; preferably, the alkali liquor is potassium hydroxide or sodium hydroxide.
In the detection method, the substance to be detected and the alkaline solution in the reaction mechanism are added in sequence. The adding mass ratio of the substance to be detected to the alkali liquor is 1 (1-50).
Preferably, the analyte is hydrogen-containing polysiloxane and a copolymer prepared from the hydrogen-containing polysiloxane through hydrosilylation.
Compared with the prior art, the invention has the beneficial effects that:
the detection device for the content of Si-H provided by the invention has the advantages that the gas storage device and the gas metering device are communicated and designed into a whole, the device is simplified, the measurement is more convenient, the analysis time is reduced, the analysis accuracy is greatly improved, and the repeatability is better. The detection device provided by the invention enables the whole detection system and the reaction mechanism to be in a constant temperature environment, so that on one hand, the influence of the external temperature on the reaction degree of the materials is avoided, and the identity of the reaction degree is ensured; on the other hand, the influence of the external temperature on the gas volume is effectively avoided, and the accuracy of the detection result is ensured. The detection device and the detection method can accurately measure the Si-H content in the hydrogenous polysiloxane and the copolymer prepared from the hydrogenous polysiloxane through hydrosilylation, avoid hydrogen leakage and improve the hydrogen collection accuracy.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a schematic structural diagram of a device for detecting Si-H content.
Icon: 1-a stirring mechanism; 2-constant temperature water/oil bath pan; 3-a magnetic rotor; 4-a reaction mechanism; 5-a gas storage device; 6-metering liquid; 7-a gas metering device; 8-a buffer device.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", "clockwise", "counterclockwise", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings or orientations or positional relationships that the products of the present invention usually place when in use, and are used only for convenience of describing the present invention and simplifying the description, but do not indicate or imply that the devices or elements referred to must have specific orientations, be constructed in specific orientations, and be operated, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," "third," and the like are used solely to distinguish one from another and are not to be construed as indicating or implying relative importance.
Furthermore, the terms "horizontal", "vertical", "overhang" and the like do not imply that the components are required to be absolutely horizontal or overhang, but may be slightly inclined. For example, "horizontal" merely means that the direction is more horizontal than "vertical" and does not mean that the structure must be perfectly horizontal, but may be slightly inclined.
In the description of the present invention, it should also be noted that, unless otherwise explicitly specified or limited, the terms "disposed," "mounted," "connected," and "connected" are to be construed broadly and may, for example, be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Example 1
Referring to fig. 1, the present embodiment provides an apparatus for analyzing Si — H content in a polyether-modified siloxane copolymer and a hydrogenpolysiloxane, comprising a reaction mechanism 4, a gas storage device 5, and a gas metering device 7. The top of the reaction mechanism 4 and the bottom of the gas storage device 5 are both ground bottle mouths and can be connected in a sealing manner after being butted. In other embodiments, a substance such as petrolatum may also be selected as needed to add sealing properties to the two.
In this embodiment, the gas storage device 5 and the gas metering device 7 are both glass tubes and are integrally formed.
In the present embodiment, the gas storage mechanism 5 and the gas metering device 7 are designed as a whole, wherein a certain amount of metering liquid 6 is contained between the gas storage mechanism 5 and the gas metering device 7, and the metering liquid 6 is also a metering liquid. In this embodiment, the metering liquid 6 is water.
The liquid level of the metering liquid 6 is not lower than the lowest scale of the gas metering device 7; the gas metering device 7 is a precision measuring tube capable of directly reading, the volume of the precision measuring tube is 10-100ml, the top of the precision measuring tube is provided with a buffer device 8, and the bottle opening of the buffer device 8 is directly connected with the atmosphere.
In this embodiment, the buffer device 8 is provided as a buffer bottle, and in other embodiments, the buffer device 8 functions as: after the reaction, hydrogen gives certain atmospheric pressure to the measurement liquid for the liquid level of measurement liquid risees gradually, sets up buffer 8 in order to prevent that measurement liquid from dashing out gaseous metering device.
And a shell is arranged on the peripheries of the gas storage mechanism 5 and the gas metering device 7, and a heat preservation medium inlet and a heat preservation medium outlet are uniformly distributed on the upper part and the lower part of the shell. In the present embodiment, the heat insulating medium is circulating water, and in other embodiments, the heat insulating medium may be a medium having a certain temperature, such as steam.
In the present example, the reaction means 4 is a round-bottomed flask, but in other embodiments, it may have other shapes, for example, a round-bottomed flask, a cup, and the like.
The bottom of the reaction mechanism 4 is provided with a constant-temperature water/oil bath pot 2, and a heat medium which can be water or oil with a certain temperature is arranged in the constant-temperature water/oil bath pot 2 so as to perform constant-temperature regulation on the reaction mechanism 4.
A stirring mechanism 1 is also arranged below the constant-temperature water/oil bath pot 2. A magnetic rotor 3 matched with the stirring mechanism 1 is arranged in the reaction mechanism 4. By electrifying the stirring mechanism 1, the magnetic rotor 3 is driven to rotate in the reaction mechanism 4, so that the reaction is fully carried out. In this embodiment, the stirring mechanism 1 is a magnetic stirrer.
When the detection device provided by the embodiment is used for analyzing the content of Si-H in the polyether modified siloxane copolymer, firstly, a certain proportion of the polyether modified siloxane copolymer and KOH solution are sequentially added into a single-neck flask, a magnetic rotor is added, then, the single-neck flask is connected with the detection device, and the single-neck flask is placed in a constant-temperature water/oil bath pot for heat preservation (25 +/-2 ℃, in other embodiments, the heat preservation temperature can be set to be 15-40 ℃, preferably 20-25 ℃), and the initial scale of the liquid level of the sealing liquid is read; and then starting stirring to enable the sample to be fully mixed and reacted with the KOH solution, observing the liquid level rising height of the sealing liquid at the gas volume measuring mechanism after reacting for a certain time, reading the scales of the sealing liquid after ensuring the liquid level to be stable, and measuring the liquid level difference value which is the hydrogen amount of the product for 3 times in parallel. And (4) calculating the Si-H content according to the calculation formula (1).
Wherein: v is the hydrogen volume (ml), m is the sample mass (g), and t is the water bath temperature (. degree.C.).
Experimental example 1
In this experimental example, the Si-H content of polyether-modified siloxane A was measured using the Si-H content analyzer of example 1.
Specifically, the Si — H content of polyether-modified siloxane a was measured to be 0.0115% by a chemical method (refer to HG/T4804-2015) using conventional polyether-modified siloxane a as a standard sample, and the Si-H content of polyether-modified siloxane a measured by a Si-H content analyzer is shown in table 1:
table 1 detection of the Si-H content of polyether modified siloxane A.
As can be seen from the test results in Table 1, the test results of the Si-H content analysis device provided by the present invention are substantially consistent with the test results of the chemical method.
Experimental example 2
In this experimental example, the Si-H content of the hydrogenpolysiloxane B was measured by using the Si-H content analysis apparatus of example 1.
The Si-H content of the hydrogenpolysiloxane B was 0.1548% as measured by a chemical method (refer to HG/T4804-2015) using hydrogenpolysiloxane B as a standard sample, and the results of the Si-H content measurement of the hydrogenpolysiloxane B using a Si-H content analyzer are shown in Table 2:
table 2 detection of the content of hydrogenpolysiloxane B Si — H.
The detection data in table 2 show that the detection result of the Si-H content analysis device is substantially consistent with the detection result of the chemical method.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The detection device for the content of Si-H is characterized by comprising a reaction mechanism, a metering mechanism and a heat preservation device, wherein the metering mechanism comprises a shell, and a gas storage device and a gas metering device which are arranged in the shell;
the heat preservation device is arranged at the bottom of the reaction mechanism.
2. The apparatus for detecting the content of Si-H according to claim 1, wherein an end of the gas metering device away from the gas storage device is provided with a containing device for containing a metering liquid.
3. The device for detecting the content of Si-H according to claim 2, wherein the gas storage device is a gas connecting pipe, and the gas metering device is a liquid metering pipe;
preferably, one end of the gas connecting pipe is fixedly connected or detachably connected with one end of the liquid metering pipe;
preferably, the gas storage device and the gas metering device are both U-shaped pipes, and the gas storage device is connected with one end of the gas metering device in a sealing manner;
preferably, the gas storage means and the gas metering means are integrally formed.
4. The device for detecting the content of Si-H according to claim 2 or 3, wherein the accommodating device extends out of the housing, and an end of the accommodating device, which is far away from the liquid outlet, is open.
5. The device for detecting the content of Si-H according to claim 1, wherein the outer wall of the shell is provided with a heat preservation medium inlet and a heat preservation medium outlet.
6. The apparatus for detecting the content of Si — H according to claim 1, wherein the reaction mechanism is a flask.
7. The apparatus for detecting Si-H content according to claim 1, wherein said temperature keeping means is a constant temperature water bath, a constant temperature oil bath, or a constant temperature oil bath.
8. The device for detecting the content of Si-H according to claim 7, wherein a stirring mechanism is further arranged at the bottom of the heat preservation device; preferably, the stirring mechanism is a magnetic stirrer.
9. A method for detecting the Si-H content using the Si-H content detecting apparatus according to any one of claims 1 to 8, comprising: placing an object to be measured and alkali liquor into the reaction mechanism, introducing metering liquid into a gas metering device, then hermetically connecting a gas storage device of the metering mechanism with a gas outlet of the reaction mechanism, obtaining the volume V of hydrogen generated by reaction according to the liquid level change of the gas metering device before and after the reaction, and obtaining the content of Si-H according to the formula (1):
formula (1):
v is the volume of hydrogen generated by the reaction, m is the mass of the substance to be detected, and t is the heat preservation temperature of the heat preservation device.
10. The method according to claim 9, wherein the analyte is hydrogen-containing polysiloxane and a copolymer prepared from hydrogen-containing polysiloxane by hydrosilylation, and the alkali solution is a strong base; preferably, the alkali liquor is potassium hydroxide or sodium hydroxide.
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| CN215066419U (en) * | 2020-12-08 | 2021-12-07 | 泰安瑞泰纤维素有限公司 | Methoxy content measuring device |
| CN213779800U (en) * | 2020-12-18 | 2021-07-23 | 江苏美思德化学股份有限公司 | Detection apparatus for Si-H content |
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