CN112798372A - Analysis method of polyether polyol structure in polyurethane and application thereof - Google Patents

Analysis method of polyether polyol structure in polyurethane and application thereof Download PDF

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CN112798372A
CN112798372A CN202011610235.4A CN202011610235A CN112798372A CN 112798372 A CN112798372 A CN 112798372A CN 202011610235 A CN202011610235 A CN 202011610235A CN 112798372 A CN112798372 A CN 112798372A
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polyurethane
polyether polyol
analyzing
hydrolysis
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吴杰
耿遥杰
刘涛
李再永
申晓青
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Shanghai Microspectrum Chemical Technology Service Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode

Abstract

The invention relates to the field of chemical analysis, and particularly provides an analysis method for a polyether polyol structure in polyurethane and application thereof. The first aspect of the present invention provides a method for analyzing a structure of polyether polyol in polyurethane, comprising the steps of: (1) freezing and grinding: freezing and grinding a polyurethane sample; (2) hydrolysis: hydrolyzing the polyurethane sample obtained in the step (1) in an alkaline solution; (3) and (3) detection: and (3) carrying out MS and MALDI-TOF tests on the polyurethane sample obtained in the step (2).

Description

Analysis method of polyether polyol structure in polyurethane and application thereof
Technical Field
The invention relates to the field of chemical analysis, and particularly provides an analysis method for a polyether polyol structure in polyurethane and application thereof.
Background
Polyurethane is an important polymer material, and is widely applied to many fields such as automobile manufacturing, refrigerator manufacturing, transportation, civil engineering and construction, shoes, synthetic leather, textiles, electromechanics, petrochemical industry, mining machinery, aviation, medical treatment, agriculture and the like due to excellent performance of polyurethane. At present, polyurethane foam plastics are widely applied. The soft foam plastic is mainly used for various cushion materials, sound insulation materials and the like of furniture and vehicles; the hard foamed plastic is mainly used for heat insulating layers of household appliances, heat insulating waterproof spray foam of wall surfaces of houses, heat insulating materials of pipelines, building boards, heat insulating materials of refrigerated trucks and refrigerated storages, and the like; semi-rigid foams are used in automobile dashboards, steering wheels, and the like. The foam plastic composite material (bi-component premix) with various specifications and applications is mainly used for (cold curing) high-resilience foam plastic, semi-rigid foam plastic, casting and spraying rigid foam plastic and the like. Polyether polyols are one of the most important raw materials for polyurethanes and are widely used in products such as polyurethane adhesives, foams, elastomers, and the like.
The influence of the type of polyether polyol on the performance of polyurethane is large, so that the profiling of polyether polyol in unknown polyurethane samples is important for the research and development of the samples.
Disclosure of Invention
In order to solve the technical problems, the invention provides an analysis method of a polyether polyol structure in polyurethane, which comprises the following steps:
(1) freezing and grinding: freezing and grinding a polyurethane sample;
(2) hydrolysis: hydrolyzing the polyurethane sample obtained in the step (1) in an alkaline solution;
(3) and (3) detection: and (3) carrying out MS and MALDI-TOF tests on the polyurethane sample obtained in the step (2).
As a preferable technical scheme of the invention, the temperature of the freeze grinding in the step (1) is-180 to-230 ℃.
As a preferred technical scheme of the invention, the polyurethane sample is frozen and ground and then sieved by a 500-600-mesh sieve.
As a preferable technical scheme of the invention, the mass concentration of the alkali solution in the step (2) is 10-16%.
As a preferable technical scheme of the invention, the mass concentration of the alkali solution in the step (2) is 11-15%.
In a preferred embodiment of the present invention, in the step (2), the alkali solution is selected from any one of a potassium hydroxide solution, a sodium hydroxide solution, an ammonia water solution, and a tetramethylammonium hydroxide solution.
As a preferable technical scheme of the invention, in the step (2), the hydrolysis temperature is 140-180 ℃, and the hydrolysis time is 40-51 h.
As a preferable technical scheme of the invention, in the step (2), the hydrolysis temperature is 150-170 ℃, and the hydrolysis time is 45-50 h.
As a preferable technical scheme of the invention, the mass concentration of the polyurethane sample in the step (2) is 7-12%.
The second aspect of the invention provides an application of the method for analyzing the structure of polyether polyol in polyurethane, which is applied to structural analysis of polyether polyol in unknown polyurethane samples.
Has the advantages that: the invention provides an analysis method of a polyether polyol structure in polyurethane, which comprises the steps of breaking a urethane bond in a sample by a special hydrolysis method, fully hydrolyzing to reduce polyether polyol to a state before reaction, further performing MS and MALDI-TOF tests, and analyzing test results to obtain the molecular weight of common polyether, a synthetic monomer and an initiator of most polyether; the analysis method can effectively analyze the hard bubble polyether with the content of more than 5 percent, and has the advantages of stability, reliability and high accuracy of analysis results.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a sample of the polyurethane tested;
FIG. 2 is a sample of polyurethane after hydrolysis;
FIG. 3 is a spectrum of a polyurethane sample subjected to MS testing;
FIG. 4 is a spectrum of a polyurethane sample subjected to MS testing;
FIG. 5 spectrum of MALDI-TOF test of polyurethane sample.
Detailed Description
The disclosure may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.
The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.
When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.
In addition, the indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the number clearly indicates the singular.
In order to solve the technical problems, the invention provides an analysis method of a polyether polyol structure in polyurethane, which comprises the following steps:
(1) freezing and grinding: freezing and grinding a polyurethane sample;
(2) hydrolysis: hydrolyzing the polyurethane sample obtained in the step (1) in an alkaline solution;
(3) and (3) detection: and (3) carrying out MS and MALDI-TOF tests on the polyurethane sample obtained in the step (2).
In a preferred embodiment, the method for analyzing the structure of polyether polyol in polyurethane comprises the following steps:
(1) freezing and grinding: freezing and grinding a polyurethane sample;
(2) hydrolysis: placing the polyurethane sample obtained in the step (1) in a hydrothermal reaction kettle, and hydrolyzing in an alkaline solution;
(3) and (3) detection: and (3) carrying out MS and MALDI-TOF tests on the polyurethane sample obtained in the step (2).
<Step (1)>
The temperature of the freeze grinding in the step (1) is-180 to-230 ℃.
In a preferred embodiment, the temperature of the freeze-milling in step (1) is-196 ℃.
In one embodiment, the polyurethane sample is frozen and ground and then sieved with a 500-600 mesh sieve.
In a preferred embodiment, the polyurethane sample is cryogenically ground and passed through a 550 mesh screen.
The freeze grinding is to freeze the tough and hard-to-crush matter below the embrittlement point and grind the matter in tissue grinder to required fineness without destroying the original components. In the experimental process, the applicant finds that the polyurethane sample is subjected to freeze grinding at-196 ℃, and then is sieved by a 500-600-mesh sieve, so that the prepared sample is easy to disperse in alkali liquor, sufficient hydrolysis is facilitated, and the structural analysis of polyether polyol in the sample is more accurate.
<Step (2)>
The mass concentration of the alkali solution in the step (2) is 10-16%.
In a more preferred embodiment, the concentration of the alkali solution in the step (2) is 11-15% by mass.
In a more preferred embodiment, the concentration of the alkali solution in the step (2) is 13% by mass.
In the experimental process, the applicant finds that when the mass concentration of the alkali solution is controlled to be 10-16%, particularly 11-15%, the polyurethane can be hydrolyzed sufficiently, and the structural analysis of polyether polyol in the polyurethane is more accurate. When the concentration of the alkali solution is too low, the polyurethane is not hydrolyzed sufficiently, and when the concentration of the alkali solution is too high, the concentration of the polyether polyol contained therein is low, which affects the analysis result.
In one embodiment, the alkali solution in the step (2) is selected from any one of a potassium hydroxide solution, a sodium hydroxide solution, an aqueous ammonia solution, and a tetramethylammonium hydroxide solution.
In a preferred embodiment, the alkali solution is a sodium hydroxide solution.
In one embodiment, the hydrolysis temperature in the step (2) is 140 to 180 ℃, and the hydrolysis time is 40 to 51 hours.
In a more preferable embodiment, the hydrolysis temperature in the step (2) is 150 to 170 ℃, and the hydrolysis time is 45 to 50 hours.
In a more preferred embodiment, the hydrolysis temperature in step (2) is 160 ℃ and the hydrolysis time is 48 h.
In the experimental process, the applicant finds that when the hydrolysis temperature is controlled to be 140-180 ℃, the hydrolysis time is 40-51 h, particularly the hydrolysis temperature is controlled to be 150-170 ℃, and the hydrolysis time is 45-50 h, the hydrolysis is most sufficient, and the structural analysis of polyether polyol in the polyether polyol is more accurate.
In one embodiment, the mass concentration of the polyurethane sample in the step (2) is 7-12%.
In a more preferred embodiment, the mass concentration of the polyurethane sample in the step (2) is 8-11%.
In a more preferred embodiment, the mass concentration of the polyurethane sample in the step (2) is 10%.
The applicant finds that when the mass concentration of a polyurethane sample is controlled to be 8-11%, hydrolysis is sufficient under the action of an alkali solution, the structural analysis of polyether polyol in the polyurethane sample is more accurate, when the concentration of the polyurethane sample is too low, the accuracy of a detection result is reduced, and when the concentration of the polyurethane sample is too high, hydrolysis is insufficient, and the analysis result is influenced.
According to the invention, by regulating and controlling various conditions in the processes of freeze grinding and hydrolysis, the solidified polyurethane hard foam with high crosslinking density can be hydrolyzed sufficiently, the hard foam polyether with the content of more than 5% can be effectively analyzed, and the analysis method is stable and reliable and has high accuracy of analysis results.
<Step (3)>
The MS condition in the step (3) of the invention is as follows: ESI source, ion source temperature 150 ℃, measurement mode: SCAN, SCAN range: 50-2000, spray voltage 3.5kV, spray gas flow rate: 800L/h, spray gas temperature: 400 degrees.
In a preferred embodiment, the polyurethane sample is diluted 180 to 220 times with methanol before the MS test in step (3).
In a more preferred embodiment, the polyurethane sample is diluted 200 times with methanol before the MS test in step (3).
Mass Spectrometry (MS) is a method of determining the molecular and fragment ion masses of a sample in a high vacuum system to determine the relative molecular masses and molecular structures of the sample. Wide application range, high sensitivity, less sample consumption and high molecular speed.
MALDI-TOF conditions in step (3) of the present invention: YAG laser with acceleration voltage of 20kV, and collecting data in positive ion reflection mode and automatic data acquisition mode in scanning range of 100-10000 Da.
In a preferred embodiment, the polyurethane sample is diluted 180-220 times with acetonitrile before the MALDI-TOF test in the step (3).
In a more preferred embodiment, the polyurethane sample is diluted 200-fold with acetonitrile before the MALDI-TOF test in step (3).
The matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF) comprises a matrix-assisted laser desorption ionization ion source (MALDI) and a time-of-flight mass analyzer (TOF), wherein the MALDI is based on the principle that laser irradiates a cocrystallized film formed by a sample and a matrix, the matrix absorbs energy from the laser and transfers the energy to biomolecules, and protons are transferred to the biomolecules or obtained from the biomolecules in the ionization process so as to ionize the biomolecules. Therefore, the method is a soft ionization technology and is suitable for measuring mixtures and biomacromolecules. The principle of TOF is that ions are accelerated to fly through a flight tube under the action of an electric field, and are detected according to different flight times of arriving at a detector, namely, the mass-to-charge ratio (M/Z) of the ions is measured to be in direct proportion to the flight time of the ions, and the ions are detected. Has the characteristics of high sensitivity, high accuracy, high resolution, anti-noise interference and the like, and can be widely applied to polymer molecular mass measurement.
Examples
In order to better understand the above technical solutions, the following detailed descriptions will be provided with reference to specific embodiments. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are still within the scope of the present invention. In addition, the starting materials used are all commercially available, unless otherwise specified.
Polyether polyol 4110, polyether polyol 635S, polyether polyol ED-500, polyester polyol SKR-450C, ethylene glycol, triethanolamine, water and tertiary amine are uniformly mixed and then react with polymethylene polyphenyl polyisocyanate PAPI at 50 ℃ to prepare the obtained rigid polyurethane foam material, as shown in figure 1, the structure of the polyether polyol is analyzed according to the analysis method of the following example, wherein the raw material composition of the rigid polyurethane foam material is shown in Table 1, and the raw materials can be obtained by commercial purchase.
TABLE 1
Figure BDA0002873068090000061
Figure BDA0002873068090000071
Example 1
Embodiment 1 of the present invention provides a method for analyzing a structure of polyether polyol in polyurethane, including the steps of:
(1) freezing and grinding: freezing and grinding a polyurethane sample;
(2) hydrolysis: placing the polyurethane sample obtained in the step (1) in a hydrothermal reaction kettle, and hydrolyzing in an alkaline solution;
(3) and (3) detection: and (3) carrying out MS and MALDI-TOF tests on the polyurethane sample obtained in the step (2).
The temperature of the freeze grinding in the step (1) is-196 ℃.
And (3) freezing and grinding the polyurethane sample, and then sieving the polyurethane sample with a 550-mesh sieve.
The mass concentration of the alkali solution in the step (2) is 13%.
The alkali solution is sodium hydroxide solution.
The hydrolysis temperature in the step (2) is 160 ℃, and the hydrolysis time is 48 hours.
The mass concentration of the polyurethane sample in the step (2) is 10%.
The MS condition in the step (3): ESI source, ion source temperature 150 ℃, measurement mode: SCAN, SCAN range: 50-2000, spray voltage 3.5kV, spray gas flow rate: 800L/h, spray gas temperature: 400 degrees; before the MS test in the step (3), diluting a polyurethane sample by 200 times by using methanol; the test results are shown in fig. 3 and 4.
MALDI-TOF conditions in the step (3): YAG laser with acceleration voltage of 20kV, collecting data in positive ion reflection mode and automatic data acquisition mode, and scanning range of 100-10000 Da; before MALDI-TOF test in the step (3), diluting a polyurethane sample by 200 times by using acetonitrile; the test results are shown in fig. 5.
In FIGS. 3 to 5, the abscissa represents the peak value of the molecular ion, i.e., the molecular mass of the sample; the ordinate represents relative abundance, the size of the peak represents ion signal intensity, and it can be seen from the figure that 553, 611, 669, 727 and the like are behind the initial polyether peak + Na, the mass difference of each adjacent peak is 58, which is equivalent to the molecular mass of one propylene oxide, which is illustrated as propylene oxide homopolyether, and sorbitol (containing 6 hydroxyl groups and having a molecular weight of 182) is calculated as the initiator; the initial polyether peak + Na is 887, 945 and 1003, the mass difference of each adjacent peak is 58, which is equivalent to the molecular mass of one propylene oxide, namely propylene oxide homopolyether, the initial agent is sucrose (containing 8 hydroxyl groups and having the molecular weight of 342), the accuracy of the test result is 99%, and the repeatability is high.
Example 2
Embodiment 2 of the present invention provides a method for analyzing a structure of polyether polyol in polyurethane, including the steps of:
(1) freezing and grinding: freezing and grinding a polyurethane sample;
(2) hydrolysis: placing the polyurethane sample obtained in the step (1) in a hydrothermal reaction kettle, and hydrolyzing in an alkaline solution;
(3) and (3) detection: and (3) carrying out MS and MALDI-TOF tests on the polyurethane sample obtained in the step (2).
The temperature of the freeze grinding in the step (1) is-196 ℃.
And (3) freezing and grinding the polyurethane sample, and then sieving the polyurethane sample with a 600-mesh sieve.
The mass concentration of the alkali solution in the step (2) is 15%.
The alkali solution is sodium hydroxide solution.
The hydrolysis temperature in the step (2) is 170 ℃, and the hydrolysis time is 50 h.
The mass concentration of the polyurethane sample in the step (2) is 11%.
The MS condition in the step (3): ESI source, ion source temperature 150 ℃, measurement mode: SCAN, SCAN range: 50-2000, spray voltage 3.5kV, spray gas flow rate: 800L/h, spray gas temperature: 400 degrees; before the MS test in step (3), the polyurethane sample is diluted 200 times with methanol.
MALDI-TOF conditions in the step (3): YAG laser with acceleration voltage of 20kV, collecting data in positive ion reflection mode and automatic data acquisition mode, and scanning range of 100-10000 Da; before MALDI-TOF testing in step (3), the polyurethane sample was diluted 200-fold with acetonitrile.
The accuracy of the test result is 99%, and the repeatability is high.
Example 3
Embodiment 3 of the present invention provides a method for analyzing a structure of polyether polyol in polyurethane, including the steps of:
(1) freezing and grinding: freezing and grinding a polyurethane sample;
(2) hydrolysis: placing the polyurethane sample obtained in the step (1) in a hydrothermal reaction kettle, and hydrolyzing in an alkaline solution;
(3) and (3) detection: and (3) carrying out MS and MALDI-TOF tests on the polyurethane sample obtained in the step (2).
The temperature of the freeze grinding in the step (1) is-196 ℃.
And (3) freezing and grinding the polyurethane sample, and then sieving the polyurethane sample with a 500-mesh sieve.
The mass concentration of the alkali solution in the step (2) is 11%.
The alkali solution is sodium hydroxide solution.
The hydrolysis temperature in the step (2) is 150 ℃, and the hydrolysis time is 45 h.
The mass concentration of the polyurethane sample in the step (2) is 8%.
The MS condition in the step (3): ESI source, ion source temperature 150 ℃, measurement mode: SCAN, SCAN range: 50-2000, spray voltage 3.5kV, spray gas flow rate: 800L/h, spray gas temperature: 400 degrees; before the MS test in step (3), the polyurethane sample is diluted 200 times with methanol.
MALDI-TOF conditions in the step (3): YAG laser with acceleration voltage of 20kV, collecting data in positive ion reflection mode and automatic data acquisition mode, and scanning range of 100-10000 Da; before MALDI-TOF testing in step (3), the polyurethane sample was diluted 200-fold with acetonitrile.
The accuracy of the test result is 99%, and the repeatability is high.
Example 4
Embodiment 4 of the present invention provides a method for analyzing a structure of polyether polyol in polyurethane, including the steps of:
(1) freezing and grinding: freezing and grinding a polyurethane sample;
(2) hydrolysis: placing the polyurethane sample obtained in the step (1) in a hydrothermal reaction kettle, and hydrolyzing in an alkaline solution;
(3) and (3) detection: and (3) carrying out MS and MALDI-TOF tests on the polyurethane sample obtained in the step (2).
The temperature of the freeze grinding in the step (1) is-196 ℃.
And (3) freezing and grinding the polyurethane sample, and then sieving the polyurethane sample with a 550-mesh sieve.
The mass concentration of the alkali solution in the step (2) is 10%.
The alkali solution is sodium hydroxide solution.
The hydrolysis temperature in the step (2) is 140 ℃, and the hydrolysis time is 40 h.
The mass concentration of the polyurethane sample in the step (2) is 7%.
The MS condition in the step (3): ESI source, ion source temperature 150 ℃, measurement mode: SCAN, SCAN range: 50-2000, spray voltage 3.5kV, spray gas flow rate: 800L/h, spray gas temperature: 400 degrees; before the MS test in step (3), the polyurethane sample is diluted 200 times with methanol.
MALDI-TOF conditions in the step (3): YAG laser with acceleration voltage of 20kV, collecting data in positive ion reflection mode and automatic data acquisition mode, and scanning range of 100-10000 Da; before MALDI-TOF testing in step (3), the polyurethane sample was diluted 200-fold with acetonitrile.
The accuracy of the test result is 89%.
Example 5
Embodiment 5 of the present invention provides a method for analyzing a structure of polyether polyol in polyurethane, including the steps of:
(1) freezing and grinding: freezing and grinding a polyurethane sample;
(2) hydrolysis: placing the polyurethane sample obtained in the step (1) in a hydrothermal reaction kettle, and hydrolyzing in an alkaline solution;
(3) and (3) detection: and (3) carrying out MS and MALDI-TOF tests on the polyurethane sample obtained in the step (2).
The temperature of the freeze grinding in the step (1) is-196 ℃.
And (3) freezing and grinding the polyurethane sample, and then sieving the polyurethane sample with a 550-mesh sieve.
The mass concentration of the alkali solution in the step (2) is 16%.
The alkali solution is sodium hydroxide solution.
The hydrolysis temperature in the step (2) is 180 ℃, and the hydrolysis time is 51 h.
The mass concentration of the polyurethane sample in the step (2) is 12%.
The MS condition in the step (3): ESI source, ion source temperature 150 ℃, measurement mode: SCAN, SCAN range: 50-2000, spray voltage 3.5kV, spray gas flow rate: 800L/h, spray gas temperature: 400 degrees; before the MS test in step (3), the polyurethane sample is diluted 200 times with methanol.
MALDI-TOF conditions in the step (3): YAG laser with acceleration voltage of 20kV, collecting data in positive ion reflection mode and automatic data acquisition mode, and scanning range of 100-10000 Da; before MALDI-TOF testing in step (3), the polyurethane sample was diluted 200-fold with acetonitrile.
The accuracy of the test result is 90%.
According to the invention, through regulating and controlling various conditions in the processes of freeze grinding and hydrolysis, the cured polyurethane hard foam with high crosslinking density can be hydrolyzed sufficiently, then MS and MALDI-TOF tests are further carried out, and the test result is analyzed, so that the molecular weight of common polyether, a synthetic monomer and most of polyether initiators are obtained, the hard foam polyether with the content of more than 5% can be effectively analyzed, the analysis method is stable and reliable, and the accuracy of the analysis result is high.
The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Also, where numerical ranges are used in the claims, subranges therein are included, and variations in these ranges are also to be construed as possible being covered by the appended claims.

Claims (10)

1. A method for analyzing the structure of polyether polyol in polyurethane is characterized by comprising the following steps:
(1) freezing and grinding: freezing and grinding a polyurethane sample;
(2) hydrolysis: hydrolyzing the polyurethane sample obtained in the step (1) in an alkaline solution;
(3) and (3) detection: and (3) carrying out MS and MALDI-TOF tests on the polyurethane sample obtained in the step (2).
2. The method for analyzing the structure of polyether polyol in polyurethane according to claim 1, wherein the temperature of the freeze-grinding in the step (1) is-180 to-230 ℃.
3. The method for analyzing the structure of polyether polyol in polyurethane according to claim 2, wherein the polyurethane sample is frozen and ground and then sieved with a 500-600 mesh sieve.
4. The method for analyzing the structure of polyether polyol in polyurethane according to claim 1 or 3, wherein the mass concentration of the alkali solution in the step (2) is 10-16%.
5. The method for analyzing the structure of polyether polyol in polyurethane according to claim 1 or 3, wherein the mass concentration of the alkali solution in the step (2) is 11 to 15%.
6. The method for analyzing the structure of polyether polyol in polyurethane according to claim 1, wherein the alkali solution in the step (2) is any one selected from potassium hydroxide solution, sodium hydroxide solution, ammonia water solution, and tetramethylammonium hydroxide solution.
7. The method for analyzing the structure of polyether polyol in polyurethane according to claim 1, wherein the hydrolysis temperature in the step (2) is 140-180 ℃ and the hydrolysis time is 40-51 h.
8. The method for analyzing the structure of polyether polyol in polyurethane according to claim 1, wherein the hydrolysis temperature in the step (2) is 150-170 ℃ and the hydrolysis time is 45-50 h.
9. The method for analyzing the structure of polyether polyol in polyurethane according to claim 1, wherein the mass concentration of the polyurethane sample in the step (2) is 7-12%.
10. Use of a method according to any one of claims 1 to 9 for the analysis of the structure of polyether polyols in polyurethanes, characterized in that it is used for the structural analysis of polyether polyols in unknown polyurethane samples.
CN202011610235.4A 2020-12-30 2020-12-30 Analysis method of polyether polyol structure in polyurethane and application thereof Pending CN112798372A (en)

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