CN110865146A - Method for measuring double bond content of ethyleneoxy polyoxyethylene ether - Google Patents
Method for measuring double bond content of ethyleneoxy polyoxyethylene ether Download PDFInfo
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- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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Abstract
The invention provides a method for measuring the double bond content of ethyleneoxy polyoxyethylene ether, which comprises the steps of measuring the double bond content through the reaction of the ethyleneoxy polyoxyethylene ether, methanol and iodine simple substances; wherein the structural formula of the ethyleneoxy polyoxyethylene ether is CH2＝CH‑O‑R‑(OCH2CH2)nOH, R is selected from C1～C18A linear alkylene group of (a). The method provided by the embodiment of the invention has higher accuracy in determination of the double bond content of the ethyleneoxy polyoxyethylene ether, and provides a quality basis for preparation of the high-performance water reducing agent.
Description
Technical Field
The invention relates to ethyleneoxy polyoxyethylene ether, in particular to a method for measuring the double bond content of ethyleneoxy polyoxyethylene ether.
Background
The ethylene-oxy-polyoxyethylene ether is an important raw material of a new-generation polycarboxylate superplasticizer, the polycarboxylate superplasticizer prepared by taking the ethylene-oxy-polyoxyethylene ether as a monomer has obvious performance advantages, good slump retaining performance, good dispersing and dispersion maintaining capabilities, wider application range and stronger adaptability, and can be applied to important fields of commercial mixing stations, water conservancy, railways, highways, airports, hydraulic engineering and the like.
Based on this, the quality of the ethyleneoxy polyoxyethylene ether is directly related to the performance of the water reducing agent after polymerization. The double key value is an important quality index for inspecting the ethyleneoxy polyoxyethylene ether, the higher the double key value is, the higher the degree of unsaturation is, and the higher the activity of the product is, so that the accurate determination of the double key value of the product is particularly important. At present, no report is found about a method for measuring the double-key value of the ethyleneoxy polyoxyethylene ether.
Disclosure of Invention
The invention mainly aims to provide a method for measuring the double bond content of ethyleneoxy polyoxyethylene ether, which comprises the steps of measuring the double bond content by the reaction of the ethyleneoxy polyoxyethylene ether, methanol and iodine simple substances; wherein the structural formula of the ethyleneoxy polyoxyethylene ether is CH2＝CH-O-R-(OCH2CH2)nOH, R is selected from C1～C18A linear alkylene group of (a).
The method provided by the embodiment of the invention has higher accuracy in determination of the double bond content of the ethyleneoxy polyoxyethylene ether, and provides a quality basis for preparation of the high-performance water reducing agent.
Detailed Description
Exemplary embodiments that embody features and advantages of the invention are described in detail below. It is to be understood that the invention is capable of other and different embodiments and its several details are capable of modification without departing from the scope of the invention, and that the description is intended to be illustrative in nature and not to be construed as limiting the invention.
The invention provides a method for measuring the double bond content of ethyleneoxy polyoxyethylene ether, which comprises the steps of measuring the double bond content by the reaction of the ethyleneoxy polyoxyethylene ether, methanol and iodine simple substances; wherein the structural formula of the ethyleneoxy polyoxyethylene ether is CH2＝CH-O-R-(OCH2CH2)nOH, R is selected from C1～C18N represents the average number of ethoxy groups.
In one embodiment, n may be 5 to 180, such as 5, 8, 10, 15, 20, 30, 40, 50, 60, 65, 70, 80, 90, 100, 105, 110, 150, 175, 180, etc.
In one embodiment, the number of carbon atoms in R may be 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, or 18.
In one embodiment, R may be a linear C1～C18Alkylene of, e.g. -CH2-、-CH2CH2-、-CH2CH2CH2-、-CH2CH2CH2CH2-、-(CH2)18-。
In one embodiment, the method for determining the double bond content of ethyleneoxy polyoxyethylene ether comprises:
providing a first mixture comprising a mass m of ethyleneoxy polyoxyethylene ether and a volume V of methanol;
providing a second mixture comprising a mass m2Iodine and volume of V2Ethanol of (2);
mixing the first mixture and the second mixture, and fully reacting to obtain a third mixture;
titrating the third mixture with a molar concentration C of aqueous sodium thiosulfate solution; and
through the total amount of elementary iodine species participating in the reaction, the amount CV of species used for titrating the sodium thiosulfate consumed by the third mixture1And calculating the mass m of the ethyleneoxy polyoxyethylene ether to obtain the double bond content of the ethyleneoxy polyoxyethylene ether.
In one embodiment, the reaction equation of ethyleneoxy polyoxyethylene ether with methanol and iodine is as follows:
CH2＝CH-O-R-(OCH2CH2)nOH+I2+CH3OH→CH2I–CH(OCH3)-O-R-(OCH2CH2)nOH+HI。
in one embodiment, the volume V of methanol may be 25-50 mL, for example, 30mL, 35mL, 40mL, 45mL, etc.
In one embodiment, the second mixture may be an iodine-ethanol solution with a concentration of 0.1-0.2 mol/L, for example, the concentration of the iodine-ethanol solution may be specifically 0.12mol/L, 0.14mol/L, 0.15mol/L, 0.16mol/L, 0.18mol/L, and the like.
In one embodiment, the volume of the second mixture can be 25-50 mL, such as 30mL, 35mL, 40mL, 45mL, etc.
In one embodiment, the first mixture and the second mixture are mixed and then left in the dark at room temperature for 5 to 30 minutes, so that the reaction between the methanol, the iodine and the double bond can be sufficiently performed, and specifically, the left time may be, for example, 8 minutes, 10 minutes, 15 minutes, 20 minutes, 25 minutes, and the like.
In one embodiment, the concentration of the aqueous sodium thiosulfate solution can be 0.1 mol/L.
In one embodiment, the process for preparing the aqueous solution of sodium thiosulfate comprises: weighing a certain amount (e.g. 26g) of sodium thiosulfate (Na)2S2O3·5H2O) or anhydrous sodium thiosulfate (e.g., 16g), anhydrous sodium carbonate (e.g., 0.2g) is dissolved in water (e.g., 1000mL), slowly boiled for 10 minutes, cooled, left for two weeks, and filtered.
In one embodiment, the iodine-ethanol solution is prepared by the following steps: weighing a certain amount (for example, 13-26 g) of iodine in a beaker, dissolving the iodine in ethanol, transferring the iodine into a 1000mL volumetric flask, diluting the iodine to a scale mark with ethanol, and shaking up to obtain an iodine-ethanol solution with the concentration of 0.1-0.2 mol/L (the molar concentration of iodine is 1/2I)2Representation).
In one embodiment, the method for determining the total amount of elemental iodine involved in the reaction (blank test) comprises: providing a fourth mixture, mixing the fourth mixture with V volume of methanol, titrating the mixed solution by using a sodium thiosulfate aqueous solution with a molar concentration of C, and consuming V0Volume of aqueous sodium thiosulfate solution, CV0I.e. the amount of the iodine elementary substance participating in the reaction.
In one embodiment, the components, and the content of each component, of the fourth mixture are the same as the second mixture.
In one embodiment, the double bond content X of the ethyleneoxy polyoxyethylene ether is calculated by the following formula:
wherein X represents the actually measured double key value of the sample of the ethyleneoxy polyoxyethylene ether, namely the double bond amount contained in each gram of the sample, and the unit is mol/kg;
V0represents the volume of sodium thiosulfate titration solution consumed for the blank test in milliliters (mL);
V1represents the volume of sodium thiosulfate titration solution consumed by the assay sample in milliliters (mL);
c represents the actual concentration of the sodium thiosulfate titration solution in units of moles per liter (mol/L);
the mass of the m samples is given in grams (g).
Hereinafter, a method for measuring a double bond content of an ethyleneoxy polyoxyethylene ether according to an embodiment of the present invention will be described in detail with reference to specific examples. Wherein, the reagents used are as follows: sodium thiosulfate: AR, national drug group chemical agents limited; methanol: AR, national drug group chemical agents limited; iodine, AR, national drug group chemical agents limited; ethanol: AR, tianjin, komiou chemical reagents ltd; anhydrous sodium carbonate, AR, Tianjin City photo-recovery fine chemical research institute.
Example 1
Titration of the sample
(1) Preparation of standard titration solution: 26g of sodium thiosulfate (Na) are weighed2S2O3·5H2O), adding 0.2g of anhydrous sodium carbonate, dissolving in 1000mL of water, slowly boiling for 10 minutes, cooling, standing for two weeks, and filtering to prepare a 0.1mol/L sodium thiosulfate standard titration solution; the accurate concentration of the calibrated sodium thiosulfate standard titration solution is 0.1011 mol/L;
(2) preparation of iodine-ethanol solution: weighing 26g of iodine, placing the iodine in a beaker, dissolving the iodine in ethanol, transferring the iodine into a 1000mL volumetric flask, diluting the iodine with ethanol to a scale, and shaking up to prepare a 0.2mol/L iodine-ethanol solution;
(3) 3.1106 g of a sample of ethyleneoxy polyoxyethylene ether (CH) were weighed2＝CH-O-CH2CH2-(OCH2CH2)65OH), dissolved in 50mL of methanol;
(4) adding 25mL of iodine-ethanol solution prepared in the step (2) into the ethyleneoxy polyoxyethylene ether-methanol solution in the step (3), shaking uniformly, and standing in the dark for 30 minutes to obtain a mixed solution in a brownish red color;
(5) titrating the mixed solution obtained in the step (4) by using the sodium thiosulfate standard titration solution obtained in the step (1) until the mixed solution is colorless, wherein the volume V of the consumed sodium thiosulfate standard titration solution130.52 mL;
blank test
Adding 25mL of the iodine-ethanol solution prepared in the step (2) into 50mL of methanol to obtain a brownish red mixed solution, titrating the brownish red mixed solution by using the sodium thiosulfate standard titration solution in the step (1) until colorless is taken as an end point, and consuming the volume V of the sodium thiosulfate standard titration solution049.73 mL;
that is, in the blank test, the operations of the above steps (3), (4), and (5) were repeated except that no sample of ethyleneoxy polyoxyethylene ether was added.
According to C, V0、V1And m is calculated according to the following formula to obtain that the double bond content of the sample of the ethyleneoxy-polyoxyethylene ether is 0.312 mol/kg.
Example 2
The materials and procedures used in this example were substantially the same as those described in example 1, except that 0.5092 g of a sample of ethyleneoxy polyoxyethylene ether (CH) was weighed2＝CH-O-CH2CH2CH2CH2-(OCH2CH2)8OH), dissolved in 50mL of methanol, titrated with the standard sodium thiosulfate titration solution of step (1), and the volume V of the consumed standard sodium thiosulfate titration solution129.32 mL; the measured double bond content of the sample of ethyleneoxy polyoxyethylene ether was 2.026 mol/kg.
Example 3
The raw materials and procedures used in this example were substantially the same as those of example 1, except that 5.0779 g of a sample of ethyleneoxy polyoxyethylene ether (CH) was weighed2＝CH-O-CH2CH2-(OCH2CH2)105OH), dissolved in 50mL of methanol, titrated with the standard sodium thiosulfate titration solution of step (1), and the volume V of the consumed standard sodium thiosulfate titration solution130.03 mL; the double bond content of the sample of ethyleneoxy polyoxyethylene ether was measured to be 0.196 mol/kg.
Example 4
The raw materials and procedures used in this example were substantially the same as those of example 1, except that 9.3021 g of a sample of ethyleneoxy polyoxyethylene ether (CH) was weighed2＝CH-O-CH2CH2CH2CH2-(OCH2CH2)175OH), dissolved in 50mL of methanol, titrated with the standard sodium thiosulfate titration solution of step (1), and the volume V of the consumed standard sodium thiosulfate titration solution129.12 mL; the double bond content of the sample of ethyleneoxy polyoxyethylene ether was measured to be 0.112 mol/kg.
Comparative example 1
The samples used in examples 1, 2, 3, 4 were taken, respectively, according to the national standard "plastic polyether polyol part 6: determination of the degree of unsaturation the double bond content was determined by the method "determination of the degree of unsaturation", corresponding to the sample numbers 1#, 2#, 3#, 4# (1# corresponds to the sample of example 1, and so on), and the double bond content of the samples determined and the double bond content determined in examples 1 to 4 were compared and are shown in table 1.
TABLE 1 comparison analysis of unsaturation detection by the present invention and the national standard method
The data in Table 1 show that the double bond content determined using the examples of the invention compares favorably with the results of the "part 6 of the Plastic polyether polyol" of the national Standard: results of methods of measuring the unsaturation degree are basically consistent, feasibility of the measuring method is further verified, and meanwhile, good repeatability of the method is shown.
Comparative example 2
The above samples are measured according to GB/T13892-2012 & lt determination of iodine value of surfactant & gt, the Webster reagent cannot completely perform addition reaction with double bonds in the samples, and the double bond content of the product cannot be measured.
Unless otherwise defined, all terms used herein have the meanings commonly understood by those skilled in the art.
The described embodiments of the present invention are for illustrative purposes only and are not intended to limit the scope of the present invention, and those skilled in the art may make various other substitutions, alterations, and modifications within the scope of the present invention, and thus, the present invention is not limited to the above-described embodiments but only by the claims.
Claims (10)
1. A method for measuring the double bond content of ethyleneoxy polyoxyethylene ether comprises the steps of measuring the double bond content through the reaction of the ethyleneoxy polyoxyethylene ether, methanol and iodine simple substances; wherein the structural formula of the ethyleneoxy polyoxyethylene ether is CH2＝CH-O-R-(OCH2CH2)nOH, R is selected from C1～C18A linear alkylene group of (a).
2. The method of claim 1, comprising:
providing a first mixture comprising said ethyleneoxy polyoxyethylene ether in a mass m and methanol in a volume V;
providing a second mixture comprising a mass m2Iodine and volume of V2Ethanol of (2);
mixing the first mixture and the second mixture, and fully reacting to obtain a third mixture;
titrating the third mixture with an aqueous solution of sodium thiosulfate having a molar concentration of C; and
by passingThe total amount of elemental iodine involved in the reaction, the amount CV of the substance of sodium thiosulfate consumed for titrating the third mixture1And calculating the mass m of the ethyleneoxy polyoxyethylene ether to obtain the double bond content of the ethyleneoxy polyoxyethylene ether.
3. The method of claim 2, wherein the method for determining the total amount of elemental iodine participating in the reaction comprises:
providing a fourth mixture comprising a mass m2Iodine and volume of V2Ethanol of (2); and
mixing the fourth mixture with V volume of methanol, and titrating by using a sodium thiosulfate aqueous solution with a molar concentration of C to consume V0Volume of said aqueous sodium thiosulfate solution.
4. The method according to claim 3, wherein the double bond content X of the ethyleneoxy polyoxyethylene ether is calculated by the following formula:
5. the process according to claim 2, wherein the volume V of methanol is from 25 to 50 mL.
6. The method of claim 2, wherein the second mixture is an iodine-ethanol solution having a concentration of 0.1 to 0.2 mol/L.
7. The method of claim 2, wherein the volume of the second mixture is 25 to 50 mL.
8. The method according to any one of claims 2 to 7, comprising mixing the first mixture with the second mixture and then leaving the mixture in the dark at room temperature for 5 to 30 minutes.
9. The method of claim 1, wherein R is selected from-CH2-、-CH2CH2-、-CH2CH2CH2-or-CH2CH2CH2CH2-。
10. The method according to claim 1, wherein n is 5 to 180.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114184736A (en) * | 2021-11-29 | 2022-03-15 | 孙世兵 | Method for measuring unsaturation degree of macromonomer of polycarboxylate superplasticizer |
| CN114624311A (en) * | 2022-02-24 | 2022-06-14 | 浙江皇马科技股份有限公司 | Method for measuring triple bond content of acetylenic diol polyoxyethylene ether |
-
2019
- 2019-11-29 CN CN201911205516.9A patent/CN110865146A/en active Pending
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114184736A (en) * | 2021-11-29 | 2022-03-15 | 孙世兵 | Method for measuring unsaturation degree of macromonomer of polycarboxylate superplasticizer |
| CN114624311A (en) * | 2022-02-24 | 2022-06-14 | 浙江皇马科技股份有限公司 | Method for measuring triple bond content of acetylenic diol polyoxyethylene ether |
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