A method for evaluating the compatibility of a combination polyol

Abstract

This invention provides a method for evaluating the compatibility of two components in a composite polyol, comprising the steps of: 1) measuring the surface tension σ of the two components using a contact angle meter. L1 , σ L2 1) The contact angles θ1 and θ2 of the two components on the PTFE plate; 2) Calculate the dispersion force components σ of the two components according to Equations 1 to 4 respectively. L1 D and σ L2 D and polar force component σ L1 P and σ L2 P And the interfacial tension σ generated during mixing is calculated according to Equation 5. LL 3) Compatibility is judged based on the following criteria: a) σ LL When <1mN / m, the compatibility is excellent; b) when 1mN / m≤σ LL When ≤2mN / m, the compatibility is relatively good; c) When 2mN / m<σ LL When ≤3mN / m, the compatibility is relatively poor; d) when σ LL When the N / m value is greater than 3 mN / m, the compatibility is very poor. This method can optimize the reaction process and save costs.

Description

Technical Field

[0001] This invention belongs to the field of analytical chemistry, and in particular to a method for evaluating the compatibility between any two components in a composite polyol. Background Technology

[0002] Polyurethane, abbreviated as PU, is a general term for macromolecular compounds containing repeating urethane groups (-NHCOO-) on their main chain. Polyurethane materials are a very important and widely used polymer material, primarily prepared by the reaction of isocyanates and polyols. Depending on the number of functional groups in the raw materials, linear or three-dimensional polymer structures can be produced. By selecting different polyisocyanates, different types and molecular weights of polyols, and various functional additives, polyurethane materials with excellent elasticity, adhesion, foamability, wear resistance, low-temperature resistance, and many other properties can be obtained under appropriate conditions. These materials are widely used in foam plastics, elastomers, coatings, adhesives, synthetic leather, and fibers, among many other fields. Polyols are one of the two-component raw materials for synthesizing polyurethane materials. Polyols consist of various components, including polyether polyols, polyester polyols, polymer polyols, vegetable oil polyols, and other polyols, as well as surfactants, catalysts, foaming agents, stabilizers, crosslinking agents, and other additives.

[0003] Currently, in the field of polyurethane and polyol blends, the moisture content, hydroxyl value, molecular weight and molecular weight distribution of polyols in polyol blends are usually determined. The testing methods used include chemical titration, infrared spectroscopy, nuclear magnetic resonance, and high performance liquid chromatography.

[0004] In the application synthesis of polyols, understanding their compatibility is crucial. Polyols have complex compositions, requiring high compatibility between their components. In practical scientific research and industrial production, the compatibility of polyols is a vital indicator, significantly impacting their storage stability. Poorly compatible polyols are prone to stratification, severely affecting product quality. Failure to understand polyol compatibility can cause unnecessary trouble or serious losses in production. Currently, there is no rapid and effective method for evaluating the compatibility of polyols.

[0005] Chinese patent application CN201910756241.1 discloses a method for evaluating the compatibility of asphalt and SBS based on molecular dynamics simulation. This technical solution uses molecular dynamics simulation software to construct a unit cell model of a single asphalt system, a molecular structure model of an SBS block copolymer, and a model of an SBS-modified asphalt blend system, and performs molecular dynamics simulations on them respectively. The solubility parameters and interaction energies are then calculated and used as indicators to characterize and evaluate the compatibility of SBS and asphalt. However, the process is complex and cumbersome, and it is not suitable for situations involving a large number of compounds.

[0006] In his article "Research Progress on the Compatibility of Polymer Blends," published in the 5th issue of *Modern Chemical Industry* in 1994, Du Shiguo mentioned that the glass transition temperature (Tg) can be used to evaluate the compatibility of blends by measuring the glass transition temperature (Tg) using differential scanning calorimetry. When the system is completely compatible, there is only one Tg, which lies between the Tg values ​​of the two components. A completely immiscible system will exhibit two Tg values ​​corresponding to the pure components. If the two compounds are partially compatible, the two Tg values ​​of the blend will approach each other due to the mutual diffusion between the components. However, when the difference in Tg between the two components is less than 20°C, it is difficult to distinguish between them, and their compatibility cannot be determined.

[0007] Zhang Qun'an et al. published "Study on the Compatibility of Two Polyols" in Volume 4, Issue 6 of the Journal of Nanyang Institute of Technology in 2012. They disclosed the use of the co-solvent method to study the compatibility between hydroxyl-terminated polyethylene terephthalate and biomass-based polyol castor oil. However, the co-solvent method is very difficult and cumbersome in terms of solvent selection, and is especially unsuitable for situations where there are many types of compounds involved in the combined polyol.

[0008] Therefore, there is a need for a method that can more conveniently, quickly, and precisely evaluate the compatibility between any two components in a composite polyol. Summary of the Invention

[0009] This invention provides a method for evaluating the compatibility of two components in a composite polyol. The method evaluates the compatibility between any two components in a composite polyol, and is simple to operate, quantitative, rapid, efficient, and highly accurate. It can provide more accurate experimental or process parameter guidance for scientific research or industrial production using composite polyols, reduce unnecessary process steps, optimize reaction processes, and save costs.

[0010] According to the present invention, a method for evaluating the compatibility of two components in a composite polyol is provided, comprising the following steps:

[0011] 1) The surface tension σ of the first component to be evaluated for compatibility in the combined polyol was measured using a contact angle meter. L1 The surface tension σ of the second componentL2 , and the contact angle θ1 of the first component on the PTFE plate and the contact angle θ2 of the second component on the PTFE plate;

[0012] 2) Calculate the dispersion force component σ of the first component to be evaluated in the combined polyol according to Equations 1 to 4. L1 D The dispersion force component σ of the second component L2 D and the polar force component σ of the first component L1 P The polar force component σ of the second component L2 P And, according to Equation 5, the interfacial tension σ generated when the first and second components to be evaluated for compatibility in the combined polyol are mixed. LL ;

[0013] σ L1 D =[σ L1 2 (1+cosθ1) 2 ] / (4σ S Formula 1

[0014] σ L2 D =[σ L2 2 (1+cosθ2) 2 ] / (4σ S Equation 2

[0015] σ L1 P =σ L1 -σ L1 D Formula 3

[0016] σ L2 P =σ L2 -σ L2 D Formula 4

[0017] σ LL =σ L1 +σ L2 -2(σ L1 D +σ L2 D ) 1 / 2 -2(σ L1 P +σ L2 P ) 1 / 2 Formula 5

[0018] Where, σ S It is the surface energy of the PTFE sheet. The unit of surface tension is mN / m, the unit of contact angle is degrees, and the unit of interfacial tension is mN / m.

[0019] 3) The compatibility of the first and second components is judged based on the following criteria:

[0020] a) The interfacial tension σ generated when the first and second components of the combined polyol are mixed. LL When the ratio is less than 1 mN / m, the compatibility of the two components of the combined polyol is excellent;

[0021] b) The interfacial tension σ generated when the first and second components of the combined polyol are mixed. LL When the ratio is greater than or equal to 1 mN / m and less than or equal to 2 mN / m, the compatibility of the two components of the combined polyol is relatively good.

[0022] c) The interfacial tension σ generated when the first and second components of the combined polyol are mixed. LL When the ratio is greater than 2 mN / m and less than or equal to 3 mN / m, the compatibility of the two components of the combined polyol is relatively poor.

[0023] d) The interfacial tension σ generated when the first and second components of the combined polyol are mixed. LL When the ratio is greater than 3mN / m, the compatibility of the two components of the combined polyol is very poor.

[0024] Preferably, the combined polyol is a mixture of two or more polyols, or a mixture of at least one polyol with one or more selected from different polyols, surfactants, catalysts and auxiliaries, and the combined polyol is selected from polyether polyols and polyester polyols.

[0025] Preferably, the first component and the second component can each be a single component, or a mixture of two or more components that are well compatible with each other.

[0026] Preferably, the polyether polyol refers to an oligomer containing hydroxyl groups at the molecular ends or side groups, with the main molecular chain composed of ether chains (-RO-R'-), and a functionality of 2 to 8. Examples include, but are not limited to, polypropylene glycol, polypropylene triol, polymer polyols, and vegetable oil polyols.

[0027] Preferably, the polyester polyol refers to an oligomer containing hydroxyl groups at the molecular ends or side groups, whose main molecular chain is composed of ester chains (-C(O)-O-), and whose functionality is 2 to 3. Examples include, but are not limited to, adipic acid-based polyester diols, aromatic polyester diols, dimer polyester diols, polycaprolactone polyols, and polycarbonate diols.

[0028] Preferably, the surfactant is a polyether-modified silicone surfactant widely used in the polyurethane foam industry. Examples include, but are not limited to, a polysiloxane-olefin block copolymer as its main structure.

[0029] Preferably, the catalyst is a compound that has catalytic activity towards isocyanates and active hydrogen atoms, and examples include, but are not limited to, amine catalysts and organometallic catalysts.

[0030] Preferably, in step 1), the surface tension σ of the first component is tested using the pendant drop method mode in a contact angle measuring instrument. L1 The surface tension σ of the second component L2 The contact angles θ1 of the first component and θ2 of the second component on a PTFE plate were measured using a contact angle measuring instrument in the seat drop mode.

[0031] The suspended drop method refers to recording images of a droplet extruded and suspended at a needle tip using an optical imaging system. When the surface tension and gravity of the droplet reach equilibrium, the surface tension σ of the sample is measured. L The aforementioned droplet-seat method refers to recording an image of a droplet in a stable state on a PTFE plate using an optical imaging system, and then measuring the contact angle θ.

[0032] Preferably, step 1) is performed under constant temperature conditions, with the test temperature controlled at 25℃±0.2℃. The surface tension of polyols changes with temperature, and the parameters used in theoretical calculations are those at 25℃. Controlling the test temperature at 25℃±0.2℃ ensures the accuracy of the test.

[0033] Preferably, the viscosity of the combined polyol and the first and second components at 25°C is less than 5000 mPa·s.

[0034] Step 1) uses the pendant drop method to test the surface tension of the droplet. The pendant drop method requires the droplet to be in static equilibrium between surface tension and gravity, and to be symmetrical about its central axis. If the viscosity is too high, the droplet cannot form the required shape, affecting the accuracy of the test. Furthermore, if the viscosity is too high, the equilibration time required when testing the contact angle is too long, resulting in high time costs. The viscosity range specified in this invention ensures that the method is accurate and efficient.

[0035] The PTFE sheet can be a commercially available PTFE sheet, which requires a smooth surface. Before use, the surface energy of the cleaned PTFE sheet must be tested and verified to ensure that the surface energy is 18±1N / m.

[0036] The contact angle measuring instrument can be a commonly used instrument in the field, and commercial equipment providers such as Klüz Instruments Ltd., Betop Scientific Instruments Ltd., and Inno Precision Instruments Ltd. can be used.

[0037] In a preferred embodiment, the parameters of the contact angle measuring instrument are: viewing angle +2°, optical zoom of 3x for the pendant drop method, B shape factor of 0.4 to 0.7, optical zoom of 1.5x for the seated drop method, and droplet volume of 3.0 μl.

[0038] The result obtained in step 2) of the method is presented in a quantitative numerical form, specifically by measuring the surface tension σ of the components in the combined polyol. L And the contact angle θ on the PTFE plate, and then calculate the dispersion force component σ according to the derivation formula of OWRK and Young's equation. L D Polar force component σ L P It is the difference between the total surface tension and the dispersion force component.

[0039] The OWRK equation is expressed as follows:

[0040] σ SL =σ S +σ L -2[(σ S D +σ L D ) 1 / 2 +(σ S P +σ L P ) 1 / 2 ]

[0041] Where σ SL It is the interfacial tension between the solid and liquid interfaces, σ S It is the surface energy of the solid substrate, σ L It is the surface tension of the liquid, σ S D and σ L D These are the dispersion force components of the surface energy of the solid substrate and the surface tension of the liquid sample, respectively, σ S P and σ L P These are the dispersion force components of the surface energy of the solid substrate and the surface tension of the liquid sample, respectively.

[0042] Young's equation is expressed as follows:

[0043] σ S =σ SL +σ L cosθ

[0044] Where θ is the contact angle of the liquid sample on the PTFE plate.

[0045] Based on OWRK and Young's equations, we can derive:

[0046] σ L D =[σ L 2 (1+cosθ) 2 ] / (4σ S )

[0047] Based on the above testing and calculation process, the methods used at solid-liquid interfaces can also be applied to liquid-liquid interfaces to obtain the surface tension σ of any component in a composite polyol. L， Dispersion force component σ L D and polar force component σ L P The interfacial tension σ between the two components in the combined polyol can then be calculated using the OWRK equation. LL , σ LL =σ L1 +σ L2 -2(σ L1 D +σ L1 D ) 1 / 2 -2(σ L1 P +σ L2 P ) 1 / 2 The calculated interfacial tension value is used as an indicator to determine the compatibility of any two components in a composite polyol. The interfacial tension value σ LL The larger the size, the worse the compatibility.

[0048] The compatibility definition in the described method is verified using a commonly used accelerated separation method. This accelerated separation method involves mixing the two components to be evaluated uniformly, storing them at a high temperature of 80°C, and then measuring the stratification of the mixture. Compatibility is judged by the time it takes for stratification to begin: a stratification time of less than 2 hours indicates very poor compatibility; a stratification time between 2 and 8 hours indicates relatively poor compatibility; a stratification time between 8 and 24 hours indicates relatively good compatibility; and a stratification time greater than 24 hours indicates very good compatibility.

[0049] It should be noted that the data obtained by this method can be used in the formulation of various products, and can be evaluated efficiently and quickly through quantitative values ​​when any components are mixed.

[0050] It should also be noted that this method not only qualitatively assesses the compatibility of any two components, but also, within the same compatibility definition range, the magnitude of interfacial tension is significant; that is, the greater the interfacial tension, the worse the compatibility. This method can compare the compatibility of two formulations within the same compatibility definition range.

[0051] The method described above can be used to evaluate the compatibility of combined polyols, providing more accurate experimental or process parameter guidance for scientific research or industrial production using combined polyols, reducing unnecessary process steps, optimizing reaction processes, and saving costs.

[0052] For example, in the development of seat foam formulations, it is necessary to introduce a new type of polyether polyol. The method described in this invention can be used to test and calculate the original polyol composition and the newly introduced polyether polyol in the seat foam formulation. This can quickly assess the compatibility of the newly introduced polyether polyol with the original components, so as to ensure the stability and quality of the product formulation design. Detailed Implementation

[0053] To better illustrate the content of this invention, some embodiments and comparative examples are listed below. The experimental equipment for the embodiments and comparative examples is as follows:

[0054] Contact angle measuring instrument: DSA 25S, Krüger Scientific Instruments Co., Ltd.

[0055] Differential Scanning Calorimeter: DSC 822 e Mettler Technology Ltd.

[0056] High-temperature chamber: GPV-22, ESPEC Ltd.

[0057] Mixer: Talboys, Shanghai Anpu Co., Ltd.

[0058] Optical microscope: H5608T, Shenzhen Microsun Technology Co., Ltd.

[0059] The raw materials used in the examples and comparative examples are as follows:

[0060] Polyether polyol, C2020, viscosity at 25℃ is 300 mPa·s, Wanhua Chemical Group Co., Ltd.

[0061] Polyether polyol, F3135, viscosity at 25℃ is 900 mPa·s, Wanhua Chemical Group Co., Ltd.

[0062] Polyether polyol, TMN7000, viscosity at 25℃ is 400 mPa·s, Tianjin No.3 Petrochemical Plant;

[0063] Polyether polyol, BPM001, viscosity at 25℃ is 300 mPa·s, Jiangsu Zhongshan Chemical Co., Ltd.

[0064] Polyester polyol, 2000PM, viscosity at 25℃ is 4499mPa·s, Asahikawa Chemical (Suzhou) Co., Ltd.

[0065] Surfactant, DC6070, viscosity at 25°C is 100 mPa·s, Gas Chemical Company, USA;

[0066] Seat assembly material #1, containing polyether polyol, water, surfactant, catalyst and other components, with a viscosity of 1500 mPa·s at 25℃, Wanhua Chemical (Beijing) Co., Ltd.

[0067] Polyether polyol A, viscosity at 25°C is 300 mPa·s, Wanhua Chemical Group Co., Ltd.

[0068] Polyether polyol B, viscosity at 25°C is 300 mPa·s, Wanhua Chemical Group Co., Ltd.

[0069] The method for measuring interfacial tension in the embodiment is as follows: (1) Test the surface tension of one component using a contact angle measuring instrument; (2) Test the contact angle of the component on the PTFE plate; (3) Calculate the dispersion force component and polar force component of the component; (4) Test the surface tension of the other component using a contact angle measuring instrument; (5) Test the contact angle of the component on the PTFE plate; (6) Calculate the dispersion force component and polar force component of the component; (7) Calculate the interfacial tension of the two components, and determine the compatibility based on the magnitude of the interfacial tension.

[0070] The compatibility assessment method for the examples and comparative examples can be combined with the accelerated separation method. This accelerated separation method involves mixing the two components to be evaluated uniformly, storing them at a high temperature of 80°C, and then measuring the stratification of the mixture. Compatibility is determined by the time it takes for stratification to begin. A stratification time of less than 2 hours indicates very poor compatibility. A stratification time between 2 and 8 hours indicates relatively poor compatibility. A stratification time between 8 and 24 hours indicates relatively good compatibility. A stratification time greater than 24 hours indicates excellent compatibility.

[0071] Example 1

[0072] The compatibility between polyether polyol C2020 and polyether polyol F3135 was evaluated.

[0073] The parameters of the contact angle measuring instrument used were: viewing angle +2°, optical zoom of 3x for the pendant drop method, B shape factor of 0.4 to 0.7, optical zoom of 1.5x for the seated drop method, and droplet volume of 3.0 μl.

[0074] The specific steps include:

[0075] (1) Test the surface tension of polyether polyol C2020

[0076] Take 0.5 ml of C2020 into a disposable 1 ml plastic syringe and manually remove any air bubbles from the syringe. Accurately measure the outer diameter of the stainless steel needle using a micrometer. After attaching the needle, mount the syringe on a contact angle measuring instrument for testing. Five test points were used throughout the experiment, and the final result was the average of the five values. Specific data are shown in Table 1.

[0077] Table 1: Surface tension of C2020

[0078] Number of tests Surface tension (mN / m) 1 33.51 2 33.45 3 33.50 4 33.51 5 33.50 average value 33.49

[0079] (2) Test the contact angle of polyether polyol C2020 on PTFE plate.

[0080] Place the prepared PTFE plate under the syringe and gently drop the liquid onto the PTFE plate, controlling the volume of each droplet to be 3.0 ± 0.2 μl. After the droplets stabilize, record the contact angle. Five test points were used throughout the experiment, and the final result was the average of the five values. See Table 2 for specific data.

[0081] Table 2: Contact Angle of C2020 on PTFE Plate

[0082] Number of tests Contact angle (°) 1 67.03 2 66.05 3 66.40 4 66.09 5 66.03 average value 66.32

[0083] (3) Calculate the dispersion force component and polar force component of polyether polyol C2020.

[0084] Based on the surface tension of polyether polyol C2010 and its contact angle on the PTFE plate obtained from the above tests, the dispersion force component and polar force component of C2010 can be calculated according to Young's equation and OWRK equation. The calculation results are shown in Table 3.

[0085] Table 3: Surface tension, dispersion force, and polar force of C2020

[0086] Surface tension (mN / m) Dispersion force component (mN / m) Polar force component (mN / m) 33.49 30.60 2.89

[0087] (4) Test the surface tension of polyether polyol F3135

[0088] Take 0.5 ml of F3135 into a disposable 1 ml plastic syringe, and manually remove any air bubbles from the syringe. Accurately measure the outer diameter of the stainless steel needle using a micrometer. After attaching the needle, mount the syringe on a contact angle measuring instrument for testing. Five test points were used throughout the experiment, and the final result was the average of the five values. See Table 4 for detailed data.

[0089] Table 4: Surface tension of F3135

[0090] Number of tests Surface tension (mN / m) 1 33.06 2 33.23 3 33.52 4 32.34 5 33.26 average value 33.08

[0091] (5) Test the contact angle of polyether polyol F3135 on PTFE plate.

[0092] Place the prepared PTFE plate under the syringe and gently drop the liquid onto the PTFE plate, controlling the volume of each droplet to be 3.0 ± 0.2 μl. After the droplets stabilize, record the contact angle. Five test points were used throughout the experiment, and the final result was the average of the five values. See Table 5 for specific data.

[0093] Table 5: Contact Angle of F3135 on PTFE Sheet

[0094] Number of tests Contact angle (°) 1 67.98 2 68.80 3 68.56 4 67.49 5 67.41 average value 68.05

[0095] (6) Calculate the dispersion force component and polar force component of polyether polyol F3135.

[0096] The surface tension of polyether polyol F3135 and its contact angle on the PTFE plate obtained from the above tests can be used to calculate the dispersion force component and polar force component of F3135 according to Young's equation and OWRK equation.

[0097] Table 6: Surface tension, dispersion force, and polar force of F3135

[0098] Surface tension (mN / m) Dispersion force component (mN / m) Polar force component (mN / m) 33.08 28.68 4.40

[0099] (7) Evaluate the compatibility of polyether polyol C2020 and polyether polyol F3135.

[0100] The surface tension, dispersion force component, and polar force component of C2020, and the surface tension, dispersion force component, and polar force component of F3135 obtained from the above tests and calculations are used to calculate according to Equation 5. The interfacial tension between C2020 and F3135 is 0.19 mN / m, indicating that C2020 and F3135 have good compatibility.

[0101] Using an accelerated separation method, C2020 and F3135 were mixed evenly and stored in a high-temperature chamber at 80°C for one month, and no stratification occurred.

[0102] Example 2

[0103] The compatibility between polyether polyol C2020 and polyester polyol 2000PM was evaluated.

[0104] The parameters of the contact angle measuring instrument used were: viewing angle +2°, optical zoom of 3x for the pendant drop method, B shape factor of 0.4 to 0.7, optical zoom of 1.5x for the seated drop method, and droplet volume of 3.0 μl.

[0105] The surface tension, dispersion force component, and polar force component data of polyether polyol C2020 can be directly obtained from the test in Example 1 and do not need to be repeated. The specific test procedure for polyester polyol 2000PM is the same as that in Example 1. The surface tension, dispersion force component, and polar force component of 2000PM obtained from the test are shown in Table 7.

[0106] Table 7: Surface tension, dispersion force components, and polar force components at 2000 PM

[0107] Surface tension (mN / m) Dispersion force component (mN / m) Polar force component (mN / m) 42.81 34.29 8.52

[0108] The surface tension, dispersion force component, and polar force component of C2020 and 2000PM obtained from the above tests and calculations are used to calculate the interfacial tension between C2020 and 2000PM according to Equation 5. The result is that the interfacial tension between C2020 and 2000PM is 1.59 mN / m, indicating that C2020 and 2000PM have good compatibility.

[0109] Using an accelerated separation method, C2020 and 2000PM were mixed evenly and stored in a high-temperature chamber at 80°C for about 20 hours, at which point stratification began to occur.

[0110] Example 3

[0111] The compatibility between polyether polyol BPM001 and polyether polyol TMN700 was evaluated.

[0112] The parameters of the contact angle measuring instrument used were: viewing angle +2°, optical zoom of 3x for the pendant drop method, B shape factor of 0.4 to 0.7, optical zoom of 1.5x for the seated drop method, and droplet volume of 3.0 μl.

[0113] The specific testing procedures for polyether polyols BPM001 and TMN700 are the same as those in Example 1. The surface tension, dispersion force component, and polar force component of BPM001 and TMN700 obtained from the tests are shown in Table 8 below.

[0114] Table 8: Surface tension, dispersion force components, and polar force components of BPM001

[0115] Surface tension (mN / m) Dispersion force component (mN / m) Polar force component (mN / m) 48.29 32.80 15.29

[0116] Table 9: Surface tension, dispersion force components, and polar force components of TMN700

[0117] Surface tension (mN / m) Dispersion force component (mN / m) Polar force component (mN / m) 33.46 27.76 5.70

[0118] The surface tension, dispersion force component, and polar force component of BPM001, obtained from the above tests and calculations, and the surface tension, dispersion force component, and polar force component of TMN700, were calculated according to Equation 5. The interfacial tension between BPM001 and TMN700 was found to be 2.73 mN / m, indicating that the compatibility between BPM001 and TMN700 is relatively poor.

[0119] Using an accelerated separation method, BPM001 and TMN700 were mixed evenly and stored in a high-temperature chamber at 80°C for about 6 hours, at which point stratification began to occur.

[0120] Example 4

[0121] The compatibility between polyester polyol 2000PM and surfactant DC6070 was evaluated.

[0122] The parameters of the contact angle measuring instrument used were: viewing angle +2°, optical zoom of 3x for the pendant drop method, B shape factor of 0.4 to 0.7, optical zoom of 1.5x for the seated drop method, and droplet volume of 3.0 μl.

[0123] The surface tension, dispersion force component, and polar force component data of the polyester polyol at 2000 PM can be directly obtained from the test in Example 2 and do not need to be repeated. The specific test steps for surfactant DC6070 are the same as those in Example 1. The surface tension, dispersion force component, and polar force component of DC6070 obtained from the test are shown in Table 10.

[0124] Table 10: Surface tension, dispersion force components, and polar force components of DC6070

[0125] Surface tension (mN / m) Dispersion force component (mN / m) Polar force component (mN / m) 22.58 19.82 2.76

[0126] The surface tension, dispersion force component, and polar force component of 2000PM and DC6070 obtained from the above tests and calculations are used to calculate the interfacial tension between 2000PM and DC6070 according to Equation 5. The interfacial tension value is relatively large, indicating that the compatibility between 2000PM and DC6070 is very poor.

[0127] Using an accelerated separation method, 2000PM and DC6070 were mixed evenly and stored in a high-temperature chamber at 80℃ for about 30 minutes, resulting in stratification.

[0128] Example 5

[0129] The method of this invention is used to rapidly evaluate the stability of newly developed seat assembly formulations. Based on seat assembly formulation #1, a new component needs to be introduced to improve tensile properties. Both polyether polyol A and polyether polyol B possess the same functionality and can meet the target requirements. To further ensure the quality and stability of the new formulation, it is necessary to know the compatibility of the newly introduced polyether polyol A and polyether polyol B with the base formulation to ensure that the new formulation does not delaminate after long-term storage and can still stably meet the product's performance requirements.

[0130] The compatibility of polyether polyol A with compound 1# and the compatibility of polyether polyol B with compound 1# were evaluated.

[0131] The parameters of the contact angle measuring instrument used were: viewing angle +2°, optical zoom of 3x for the pendant drop method, B shape factor of 0.4 to 0.7, optical zoom of 1.5x for the seated drop method, and droplet volume of 3.0 μl.

[0132] The specific testing steps for polyether polyol A, polyether polyol B, and composite material 1# are the same as those in Example 1.

[0133] Table 11: Surface tension, dispersion force component, and polar force component of composite material #1

[0134] Surface tension (mN / m) Dispersion force component (mN / m) Polar force component (mN / m) 33.2 28.38 4.82

[0135] Table 12: Surface tension, dispersion force component, and polar force component of polyether polyol A

[0136] Surface tension (mN / m) Dispersion force component (mN / m) Polar force component (mN / m) 34.84 28.24 6.6

[0137] Table 13: Surface tension, dispersion force component, and polar force component of polyether polyol B

[0138] Surface tension (mN / m) Dispersion force component (mN / m) Polar force component (mN / m) 45.95 31.44 14.51

[0139] The surface tension, dispersion force component, and polar force component of polyether polyol A, polyether polyol B, and composite material 1# obtained from the above tests and calculations are used to calculate the interfacial tension between the newly introduced polyether polyol A and composite material 1# according to Equation 5. The results show that the interfacial tension between the newly introduced polyether polyol A and composite material 1# is 0.14 mN / m, and the interfacial tension between the newly introduced polyether polyol B and composite material 1# is 2.68 mN / m. Based on the test and calculation results, polyether polyol A can be quickly selected as the material to be introduced.

[0140] Using an accelerated separation method, polyether polyol A was mixed evenly with composite material 1# and stored in a high-temperature chamber at 80°C for one month without any stratification. However, after mixing polyether polyol B with composite material 1# and storing it in a high-temperature chamber at 80°C for approximately 6 hours, stratification began to occur.

[0141] Meanwhile, after storing the blends containing polyether polyol A and the blends containing polyether polyol B for one month, foaming experiments were conducted. It was found that the foam produced by the blend containing polyether polyol B showed a significant deviation in tensile strength and elongation at break compared to the initial state, as shown in Table 14.

[0142] Table 14: Relevant experimental data from Example 5

[0143]

[0144] The comparison of the various embodiments is summarized in Table 15.

[0145] Table 15: Comparison of Examples

[0146]

[0147] Comparative Example 1

[0148] The compatibility of polyether polyol C2020 and polyester polyol 2000PM was evaluated.

[0149] The differential scanning calorimeter used was operated under the following conditions: 120℃, held for 5 min, then cooled to -80℃ at a rate of 10℃ / min, held for 3 min, and then heated to 200℃ at a rate of 10℃ / min.

[0150] The specific steps include:

[0151] (1) Test the glass transition temperature of polyether polyol C2020

[0152] Weigh 10±2 mg of C2020 into a crucible and test it according to the set conditions.

[0153] (2) Test the glass transition temperature of polyester polyol 2000PM

[0154] Weigh 10±2 mg of 2000 PM into a crucible and test it according to the set conditions.

[0155] (3) Test the glass transition temperature of the mixture of polyether polyol C2020 and polyester polyol 2000PM.

[0156] Weigh 5.0 g of C2020 into a 20 ml sealed glass bottle, add 5.0 g of 2000 PM, and mix thoroughly. Weigh 10 ± 2 mg of the mixed sample into a crucible and test according to the set conditions.

[0157] Differential scanning calorimetry (DSC) is used to test the glass transition temperature (Tg) of a mixture. When the system is completely compatible, there is only one Tg, which lies between the Tg values ​​of the two components. A completely immiscible system exhibits two Tg values ​​corresponding to the pure components. If the two compounds are partially compatible, the two Tg values ​​of the blend will approach each other due to interdiffusion. However, when the difference in Tg between the two components is less than 20°C, it is difficult to distinguish between them, making it impossible to determine their compatibility. The glass transition temperatures of C2020 and 2000PM differ by 10°C, and their mixture exhibits two Tg values, but it is difficult to distinguish the difference between these Tg values ​​and the pure components, making it impossible to determine their compatibility.

[0158] Comparative Example 2

[0159] The compatibility of polyether polyol C2020 and polyester polyol 2000PM was evaluated using the interaction parameter method. According to thermodynamic analysis, if the interaction parameter χ ≤ 0 between C2020 and 2000PM, then the two compounds are a compatible system. However, currently there is no suitable method to directly test the interaction parameter of these two compounds, making it difficult to evaluate the compatibility of polyether polyol C2020 and polyester polyol 2000PM using the interaction parameter method.

[0160] Comparative Example 3

[0161] The compatibility of polyether polyol C2020 and polyester polyol 2000PM was evaluated using the optical transparency method. Generally, if two transparent amorphous polymers are compatible, the resulting blend will also be transparent; if they are incompatible, incident light will be scattered at the interface, making it opaque. This method is affected by the refractive index, and cannot accurately determine compatibility for samples with very small differences in refractive index.

[0162] After C2020 and 2000PM were mixed thoroughly, the transparency of the mixed sample was observed using an optical microscope, and it was found that the mixed sample was transparent. This method can only indicate that the mixture of C2020 and 2000PM is optically transparent, but it cannot determine the degree of compatibility.

[0163] As can be seen from the above examples and comparative results, within the scope of this invention, the examples are simple to operate, quick and efficient, and have high measurement accuracy. They can provide quantitative results for characterization, offering clear guidance for ensuring compatibility in the development of polyurethane compound systems, thus guaranteeing the stability and quality of product formulation design. The comparative examples, using different testing methods, are complex to operate and cannot accurately evaluate compatibility, showing a significant difference compared to the examples.

Claims

1. A method for evaluating the compatibility of two components in a composite polyol, comprising the following steps: 1) The surface tension σ of the first component to be evaluated for compatibility in the combined polyol was measured using a contact angle meter. L1 The surface tension σ of the second component L2 , and the contact angle θ1 of the first component on the PTFE plate and the contact angle θ2 of the second component on the PTFE plate; 2) Calculate the dispersion force component σ of the first component to be evaluated for compatibility in the combined polyol according to Equations 1 to 4. L1 D The dispersion force component σ of the second component L2 D and the polar force component σ of the first component L1 P The polar force component σ of the second component L2 P And, according to Equation 5, the interfacial tension σ generated when the first and second components to be evaluated for compatibility in the combined polyol are mixed. LL ; in, σ S It is the surface energy of the PTFE sheet. The unit of surface tension is mN / m, the unit of contact angle is degrees, and the unit of interfacial tension is mN / m. 3) The compatibility of the first and second components is judged based on the following criteria: a) The interfacial tension σ generated when the polyols are mixed LL When the ratio is less than 1 mN / m, the compatibility of the two components of the combined polyol is excellent; b) The interfacial tension σ generated when the polyols are mixed LL When the ratio is greater than or equal to 1 mN / m and less than or equal to 2 mN / m, the compatibility of the two components of the combined polyol is relatively good. c) The interfacial tension σ generated when the polyols are mixed LL When the ratio is greater than 2 mN / m and less than or equal to 3 mN / m, the compatibility of the two components of the combined polyol is relatively poor. d) The interfacial tension σ generated when the polyols are mixed LL When the ratio is greater than 3mN / m, the compatibility of the two components of the combined polyol is very poor.

2. The method according to claim 1, wherein, The combined polyol is a mixture of two or more polyols, or a mixture of at least one polyol with one or more selected from different polyols, surfactants, catalysts and auxiliaries.

3. The method according to claim 1, wherein, The first component and the second component are either single components or mixtures of two or more components that are well compatible with each other.

4. The method according to claim 2, wherein, The surfactant is selected from polysiloxane-olefin oxide block copolymers.

5. The method according to claim 2, wherein, The catalyst is an amine catalyst or an organometallic catalyst.

6. The method according to any one of claims 1 to 5, wherein, In step 1), the surface tension σ of the first component is tested using the pendant drop method mode in a contact angle measuring instrument. L1 The surface tension σ of the second component L2 The contact angles θ1 of the first component and θ2 of the second component on a PTFE plate were measured using a contact angle measuring instrument in the seat drop mode.

7. The method according to any one of claims 1 to 5, wherein, Step 1) is carried out under constant temperature conditions, with the test temperature controlled at 25℃±0.2℃.

8. The method according to any one of claims 1 to 5, wherein, The viscosity of the combined polyol, the first component, and the second component at 25°C is less than 5000 mPa•s.

9. The method according to any one of claims 1 to 5, wherein, In step 1), the parameters of the contact angle measuring instrument are: viewing angle +2°, optical zoom of 3x for the pendant drop method, B shape factor of 0.4~0.7, optical zoom of 1.5x for the seated drop method, and droplet volume of 3.0μl.

10. The method according to any one of claims 1 to 5, wherein, The functionality of the polyol is 2 to 8.

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