Solution composition for testing grafting rate of maleic anhydride as well as preparation method and application of solution composition

By using a specific solution composition to dissolve polyolefins at high temperatures and constructing a stable reaction environment, the problems of acid volatilization, polyolefin precipitation, and entanglement in traditional methods are solved, achieving efficient and accurate grafting rate testing and overcoming the shortcomings of traditional methods.

CN121521569APending Publication Date: 2026-02-13JIANGSU KINGFA SCI & TECH ADVANCED MATERIALS CO LTD +1
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Patent Information

Application Number
CN202511687090.0
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-11-18
Publication Date
2026-02-13

AI Technical Summary

Technical Problem

Traditional methods for testing the grafting rate of maleic anhydride-grafted polyolefins suffer from problems such as acid volatilization due to high temperatures, polyolefin precipitation and entanglement due to low temperatures, as well as high energy consumption and long testing time, resulting in low testing efficiency and accuracy.

Method used

A solution composition comprising a main solvent, an auxiliary solvent, a surfactant, a solubilizer, and a detangling agent is used. By dissolving polyolefins at high temperature, a stable non-polar reaction environment is formed. The surfactant and auxiliary solvent are used to construct micelle channels to accelerate the diffusion of alkaline ions. The solubilizer captures free maleic anhydride, and the detangling agent destroys entanglement, ensuring titration accuracy.

Benefits of technology

It significantly improves the accuracy and efficiency of testing, avoids acid evaporation and polyolefin precipitation, simplifies the operation process, reduces energy consumption, and improves the reliability of grafting rate testing.

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Abstract

The invention provides a solution composition for testing the grafting rate of maleic anhydride, and belongs to the field of high polymer material detection. The solution composition for testing the maleic anhydride grafting rate is prepared from the following components in parts by weight: 80 to 90 parts of a main solvent, 5 to 10 parts of an auxiliary solvent, 3 to 5 parts of a surfactant, 2 to 5 parts of a solubilizer, 0.05 to 0.15 part of a disentangling agent and 0 to 0.15 part of water. The method comprehensively solves the four key problems of high-temperature volatilization / low-temperature precipitation, entanglement embedding, low titration efficiency and free anhydride interference in the traditional method which influence the test accuracy of the maleic anhydride grafting rate.
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Description

TECHNICAL FIELD

[0001] The present application relates to the field of high molecular material detection, in particular to a solution composition for testing maleic anhydride grafting rate, and a preparation method and application thereof. BACKGROUND

[0002] Since the maleic anhydride grafted polyolefin material was introduced in the 1960s, the introduction of polar maleic anhydride groups into the non-polar polyolefin chain through chemical grafting technology has significantly improved the compatibility and functionality of the material. In the early stage, it was mainly used to improve the interfacial bonding of polyolefin and polar polymer, filler, such as the AMPLIFY series of compatibilizers developed by Dow Chemical, which effectively solved the blending problem of polyethylene and nylon, EVOH. With the maturity of reactive extrusion technology, its application has been extended to the fields of automotive lightweight parts, electronic and electrical packaging, and high-performance composite materials. In the future, driven by the 5G communication and new energy vehicle industries, the material will develop towards high grafting rate and low crystallinity, and gradually penetrate into the environmental protection field such as degradable plastics and bio-based materials. It is expected that the global market size will continue to expand at a compound annual growth rate of 4.2%, becoming a key technology carrier in the field of polymer modification.

[0003] However, the determination scheme of grafting rate, an important parameter for using maleic anhydride grafted polyolefin in industry, has always been unsatisfactory. The traditional test scheme is acid-base titration, but this scheme has many obvious unreasonable aspects. In the acid liquid back titration step of the traditional scheme, in the process of determining the grafting rate of maleic anhydride grafted polyolefin by conventional acid-base titration method, the boiling point of hydrochloric acid is 110°C. In fact, hydrochloric acid volatilizes to some extent at room temperature. Xylene melts polyolefin often needs a temperature of more than 125°C. Even if the titration is cooled to 80-90°C, there is still a problem of hydrochloric acid volatilization. The traditional acid-base titration method inevitably has the problem of inaccurate measurement caused by acid volatilization. And it is difficult to choose low temperature measurement because polyolefin is easy to precipitate from xylene, which makes it difficult to accurately quantify the grafting rate.

[0004] In the past decade, researchers have generally improved this scheme, but all face the following problems: (1) high temperature leads to acid volatilization and polyolefin precipitation; (2) entanglement of polyethylene after grafting leads to embedding phenomenon; (3) high energy consumption and long time consumption in alkali titration step; (4) a large amount of free maleic anhydride in the system. The above reasons obviously slow down the test rate and reduce the accuracy, which ultimately limits the rapid development of the field of maleic anhydride grafted polyolefin.

[0005] Therefore, it is an urgent problem in the field to develop a method that can fundamentally solve the problems of affecting the test efficiency and accuracy in the traditional test of maleic anhydride grafted polyolefin grafting rate. SUMMARY

[0006] To overcome the shortcomings of the prior art, the present invention aims to provide a solution for testing the grafting rate of maleic anhydride-grafted polyolefins and its application, thereby solving the problems of low testing efficiency and accuracy in the prior art.

[0007] This invention is achieved through the following technical solution: In a first aspect, the present invention provides a solution for testing the grafting rate of maleic anhydride-grafted polyolefins, comprising, by weight, the following components: 80-90 parts of main solvent; 5-10 parts of auxiliary solvent; 3-5 parts surfactant; 2-5 parts of solubilizer; 0.05-0.15 parts of untangling agent; Water 0-0.15 parts.

[0008] Preferably, the main solvent of the present invention is selected from at least one of alkyl-substituted aromatic hydrocarbons or saturated fused cyclic aliphatic hydrocarbons.

[0009] More preferably, the main solvent is selected from alkyl-substituted aromatic hydrocarbons.

[0010] More preferably, the alkyl group in the alkyl-substituted aromatic hydrocarbon has 1-16 carbon atoms.

[0011] The alkyl-substituted aromatic hydrocarbon solvent of the present invention has a benzene ring structure, and the benzene ring is connected to an alkyl group (straight chain or branched chain, such as methyl or ethyl) or an ester group; the saturated fused-ring aliphatic hydrocarbon solvent of the present invention has a structure containing at least two fused six-membered rings and no double bonds or polar functional groups.

[0012] Specifically, the alkyl-substituted aromatic hydrocarbon can be selected from at least one of xylene, toluene, DBP, or DOP.

[0013] Specifically, the saturated fused cyclic aliphatic hydrocarbon can be selected from decahydronaphthalene.

[0014] More preferably, the alkyl-substituted aromatic hydrocarbon is selected from xylene, toluene, or a mixture of xylene and toluene.

[0015] More preferably, the mass ratio of the xylene to toluene mixture is (0.2-5):1.

[0016] More preferably, the mass ratio of the xylene to toluene mixture is (0.5-3):1.

[0017] More preferably, the mass ratio of the xylene to toluene mixture is 1:1.

[0018] The decahydronaphthalene can be selected from at least one of cis-decahydronaphthalene and trans-decahydronaphthalene.

[0019] The DBP is dibutyl phthalate.

[0020] The DOP is dioctyl phthalate.

[0021] The main solvent described in this invention not only serves to completely and uniformly dissolve the nonpolar backbone of maleic anhydride-grafted polyolefins, but also provides a high-temperature stable nonpolar reaction environment.

[0022] Specifically, the solubility parameters of the main solvent are matched with the polyolefin chain, which reduces the resistance to chain segment movement and prevents polyolefin precipitation at 120-130℃. At the same time, the high boiling point of the main solvent ensures thermal stability at the operating temperature, reduces solution viscosity, and promotes chain de-entanglement.

[0023] As the continuous phase of the composition, the main solvent works synergistically with other components: the main solvent forms micellar channels with the surfactant, accelerating the diffusion of alkali ions; it constructs a polar-nonpolar interface with the auxiliary solvent, reducing the cage effect; and it works with the solubilizer and deentanglement agent to capture free maleic anhydride and expose embedded groups, thereby improving titration accuracy and efficiency.

[0024] In this invention, the mass percentage content of the main solvent is 75-95%, for example, it can be 75%, 76%, 77%, 78%, 79%, 80%, 80.5%, 81%, 82%, 84%, 86%, 88%, 89.5%, 90%, 91%, 92%, 93%, 94%, 95% or any range formed by the above values.

[0025] The range of the mass percentage of the main solvent can maintain the homogeneity of the solution and prevent phase separation caused by imbalance of component ratios.

[0026] The auxiliary solvent described in this invention is selected from at least one of substituted amides, cyclic ethers, C2-C3 short-chain alcohols, or C2-C3 polyols.

[0027] Specifically, the substituted amide can be selected from N,N-dimethylformamide, dimethylacetamide, etc.; the cyclic ether can be selected from tetrahydrofuran, etc.; the C2-C3 short-chain alcohol can be selected from ethanol, isopropanol, etc.; and the C2-C3 polyol can be selected from ethylene glycol, glycerol, etc.

[0028] Preferably, the auxiliary solvent is selected from at least one of N,N-dimethylformamide, tetrahydrofuran or ethanol, a mixture of N,N-dimethylformamide and tetrahydrofuran, and a mixture of N,N-dimethylformamide, tetrahydrofuran and ethanol.

[0029] Preferably, the mass ratio of the mixture of N,N-dimethylformamide and tetrahydrofuran is 1:(0.2-5); the mass ratio of the mixture of N,N-dimethylformamide, tetrahydrofuran and ethanol is 1:(0.2-5):(0.2-5).

[0030] More preferably, the mass ratio of the mixture of N,N-dimethylformamide and tetrahydrofuran is 1:(0.5-3); the mass ratio of the mixture of N,N-dimethylformamide, tetrahydrofuran and ethanol is 1:(0.5-3):(0.5-3).

[0031] More preferably, the mass ratio of the mixture of N,N-dimethylformamide and tetrahydrofuran is 1:1; and the mass ratio of the mixture of N,N-dimethylformamide, tetrahydrofuran, and ethanol is 1:1:1.

[0032] The mass percentage content of the auxiliary solvent is 4%-12%, for example, it can be 4%, 4.5%, 5%, 5.5%, 6%, 7%, 8%, 9%, 9.5%, 10%, 11%, 11.5%, 12% or any range formed by the above values.

[0033] The auxiliary solvent achieves the following function through its polar functional groups: Enhanced reactivity: The amide group (-CONR2) and ether bond (-O-) provide lone pair electrons, forming d-pπ conjugation with the carbonyl group (C=O) of maleic anhydride, lowering the neutralization reaction energy barrier; the hydroxyl group (-OH) stabilizes the transition state through hydrogen bonding, accelerating the K+ reaction. + Ion nucleophilic attack increases the reaction rate constant.

[0034] Entanglement network disruption: Small molecular structures (such as ethanol and THF) penetrate the gaps between polyolefin chains, disrupting van der Waals forces and increasing the exposure rate of embedded MAHs; polyols (such as glycerol) anchor entanglement points through polyhydroxyl groups, forcibly separating polyolefin chains and increasing the intermolecular distance.

[0035] Phase stability assurance: Formation of hydrogen bond networks (such as DMF-xylene) or dipole interactions (such as THF-DOP) with the main solvent to prevent phase separation at high temperatures.

[0036] The auxiliary solvent can achieve complete miscibility with the main solvent in any ratio. The main solvent provides a non-polar dissolution environment, while the auxiliary solvent constructs a polar micro-reaction field, which significantly promotes the full contact and reaction process between maleic anhydride groups and base ions. The two achieve the integration of "dissolution-reaction" of MAH through interfacial mass transfer, thereby effectively eliminating potential detection blind spots and avoiding the cage effect, and ultimately ensuring the accuracy and reliability of titration analysis results.

[0037] The surfactant described in this invention is selected from at least one of the following: fluorinated surfactants, silicone surfactants, anionic surfactants, nonionic surfactants, cationic surfactants, and amphoteric surfactants.

[0038] Preferably, the surfactant is selected from at least one of fluorinated surfactants and silicone surfactants.

[0039] Preferably, the fluorinated surfactant has a fluorine content of 40-80 wt%; and the silicone surfactant has a silicon content of 5-30 wt%.

[0040] Specifically, the surfactant may be selected from at least one of perfluorooctanoic acid, perfluorooctane sulfonic acid, polyether-modified siloxane, sodium alkylbenzene sulfonate, sodium fatty alcohol polyoxyethylene ether sulfate, alkylphenol polyoxyethylene ether, and fatty acid polyoxyethylene ester.

[0041] The core functions and synergistic mechanisms of surfactants: Nanochannel construction: Rigid perfluorinated chains of fluorocarbons form reverse micelles in a nonpolar host solvent, and alkali ions migrate directionally to MAH reaction sites through the hydrophilic cavities within the micelles; Flexible siloxane skeletons of siloxanes interpenetrate the gaps between polyolefin chains, disrupting interchain entanglement.

[0042] Interfacial energy regulation: Hydrophobic groups anchor the polyolefin phase, while hydrophilic groups extend into the auxiliary solvent phase, reducing interfacial tension.

[0043] Critical operating temperature matching: The cloud point of fluorocarbon surfactants is consistent with the operating temperature to ensure the stability of micelle structure at high temperatures.

[0044] Synergistic main solvent and auxiliary solvent: Forms complex micelles with the main solvent through hydrophobic interactions, preventing MAH from being embedded; constructs ion channels with the auxiliary solvent through dipole-ion interactions, accelerating K+ ion exchange. + transmission.

[0045] The surfactant has a mass percentage content of 2%-7%, for example, it can be 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, 6%, 6.5%, 7% or any range between the above proportions.

[0046] The solubilizer described in this invention is selected from lactam polymers.

[0047] Specifically, the lactam polymer may be selected from polyvinylpyrrolidone.

[0048] The mass percentage content of the solubilizer is 1%-6%, for example, it can be 1%, 15%, 2%, 2.5%, 3%, 4%, 4.5%, 5%, 5.5%, 6% or any range between the above proportions.

[0049] The core functions and synergistic mechanisms of solubilizers: Molecular capture of free maleic anhydride (MAH): The amide carbonyl group of PVP forms a bidentate hydrogen bond with the carboxyl group of MAH, encapsulating the free MAH into the hydrophobic cavity of pyrrolidone; the pinene double bond of turpentine oil undergoes Diels-Alder pre-complexation with the C=O of MAH, reducing its reactivity. Synergistic effect: When PVP and turpentine are combined, the MAH capture rate is improved.

[0050] Polyolefin chain entanglement inhibition: The diamino group of ethylenediamine is embedded between polyolefin chains, and the hydrogen bonds between chains are broken through proton transfer, reducing the number of entanglement points; the oleic acid chain of Tween 80 anchors the polyolefin phase, and the polyoxyethylene chain extends into the auxiliary solvent phase to form a "molecular bridge" to inhibit re-entanglement.

[0051] In synergy with the main solvent and auxiliary solvent, the hydrophobic framework of the main solvent PVP stacks with xylene π-π to form a homogeneous "dissolution cage"; and the amino group of the auxiliary solvent ethylenediamine forms a donor-acceptor complex with the carbonyl group of DMF, accelerating MAH transfer.

[0052] The combination of water and solubilizer can dissolve free unreacted maleic anhydride in the system, improving the accuracy of grafting results.

[0053] The untangling agent described in this invention is selected from at least one of halogenated hydrocarbons, polyols, and thermosetting resin solutions.

[0054] Specifically, the untangling agent of the present invention may be selected from at least one of dichloromethane, trichloromethane, 1,2-dichloroethane, pentaerythritol, sorbitol, glycerol, aqueous solution of phenolic resin, and aqueous solution of urea-formaldehyde resin.

[0055] The detangling agent breaks the interchain van der Waals forces by embedding itself into the polyolefin molecular entanglement network, thereby increasing the exposure rate of the embedded MAH groups, effectively removing the shielding of active sites caused by steric hindrance, and improving the accuracy of detection.

[0056] In this invention, the mass percentage content of the untangling agent is 0.03%-0.3%, for example, it can be 0.03%, 0.05%, 0.08%, 0.1%, 0.12%, 0.15%, 0.2%, 0.25%, 0.3% or any of the above proportions.

[0057] The water content in this invention is 0%-0.2% by mass, for example, it can be 0%, 0.05%, 0.08%, 0.1%, 0.12%, 0.15%, 0.18%, 0.2% or any of the above proportions.

[0058] Secondly, the present invention also provides a method for preparing the above-mentioned solution composition for testing the grafting rate of maleic anhydride, wherein all components are mixed evenly.

[0059] Thirdly, the present invention also provides the application of the above-mentioned solution composition for testing the grafting rate of maleic anhydride, for testing the grafting rate of maleic anhydride-grafted polyolefins.

[0060] Fourthly, the present invention also provides a method for testing the grafting rate of maleic anhydride, the operation steps of which are as follows: The components of the above-mentioned solution composition for testing the grafting rate of maleic anhydride are mixed evenly according to the specified ratio, heated, and then maleic anhydride-grafted polyolefin is added. After the maleic anhydride-grafted polyolefin dissolves, phenolphthalein is added, and the solution is immediately titrated with potassium hydroxide-ethanol solution while hot.

[0061] Preferably, the concentration of the potassium hydroxide-ethanol solution is 0.01-0.05 mol / L.

[0062] Preferably, the temperature after heating is 120-130℃.

[0063] The maleic anhydride-grafted polyolefins described in this invention can be selected from maleic anhydride-grafted polypropylene, maleic anhydride-grafted polyethylene, maleic anhydride-grafted POE, maleic anhydride-grafted EVA, and maleic anhydride-grafted SEBS. The types of maleic anhydride-grafted polyolefins used for detection in this invention are not limited to the above.

[0064] The grafting rate of the maleic anhydride-grafted polyolefin described in this invention is 0.6%-8%.

[0065] The melt index of the maleic anhydride-grafted polyolefin described in this invention is 1-250 g / 10min.

[0066] Preferably, the melt index of the maleic anhydride-grafted polyolefin of the present invention is 15-200 g / 10 min. The melt flow index test conditions for maleic anhydride-grafted polypropylene are 230°C / 2.16kg; the melt flow index test conditions for maleic anhydride-grafted polyethylene, maleic anhydride-grafted POE, and maleic anhydride-grafted EVA are 190°C / 2.16kg; and the melt flow index test conditions for maleic anhydride-grafted SEBS are 190°C / 5kg.

[0067] Compared with the prior art, the present invention has the following beneficial effects: The solution composition for testing the grafting rate of maleic anhydride provided by this invention and its application fundamentally solve the problem of inaccurate quantification caused by acid evaporation at high temperatures or polyolefin precipitation from xylene solvent at low temperatures in traditional acid-base titration schemes, ensuring the stability and homogeneity of the reaction system. Simultaneously, it effectively overcomes the embedding phenomenon caused by molecular chain entanglement and the interference of free maleic anhydride in the system, significantly improving the accuracy of the test. Furthermore, by optimizing the reaction system, the test cycle is greatly shortened and the operation procedure is simplified, significantly improving the test efficiency and effectively solving the drawbacks of high energy consumption and long time consumption in traditional alkali titration steps.

[0068] This invention employs a high-temperature approach, eliminating the use of acid and thus avoiding acid volatilization issues. Furthermore, through the coordinated use of its components, it comprehensively addresses four key shortcomings of traditional methods: high-temperature volatilization / low-temperature precipitation, entanglement and embedding, low titration efficiency, and interference from free anhydride. This represents a substantial breakthrough in grafting rate testing, providing an efficient, accurate, and reliable testing method. It resolves a long-standing technical bottleneck hindering the development of maleic anhydride-grafted polyolefins, offering solid technical support for product quality control, process optimization, and new material research and development. Detailed Implementation

[0069] The present invention will now be described in detail with reference to specific embodiments. These embodiments will help those skilled in the art to further understand the present invention, but do not limit the invention in any way. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention. These all fall within the scope of protection of the present invention.

[0070] Unless otherwise specified, all materials used in this invention can be purchased commercially or prepared using conventional methods.

[0071] The raw materials used in this invention are sourced from the following sources: Main solvent-1: Xylene, commercially available, from a Chinese pharmaceutical company.

[0072] Main solvent-2: Toluene, commercially available, from China National Pharmaceutical Group.

[0073] Main solvent-3: A mixture of xylene and toluene in a mass ratio of 1:1.

[0074] Auxiliary solvent-1: N,N-dimethylformamide, commercially available, Chinese medicine.

[0075] Auxiliary solvent-2: Tetrahydrofuran, commercially available, from a Chinese pharmaceutical company.

[0076] Auxiliary solvent-3: N,N-dimethylformamide and tetrahydrofuran are compounded in a mass ratio of 1:1.

[0077] Auxiliary flux-4: N,N-dimethylformamide, tetrahydrofuran and anhydrous ethanol are compounded in a mass ratio of 1:1:1.

[0078] Auxiliary solvent-5: Anhydrous ethanol and tetrahydrofuran are mixed in a mass ratio of 1:1.

[0079] Surfactant-1: Perfluorooctanoic acid (PFOA), commercially available, Chinese medicine.

[0080] Surfactant-2: Polyether modified siloxane, SILWET L-77, Momentive Advanced Materials Group.

[0081] Surfactant-3: Polyether-modified siloxane and alkylphenol polyoxyethylene ether are compounded in a mass ratio of 1:1.

[0082] Surfactant-4: Alkylphenol polyoxyethylene ether (APEO), commercially available, Chinese medicine.

[0083] Surfactant-5: Sodium alkylbenzene sulfonate (LAS), commercially available, Chinese medicine.

[0084] Surfactant-6: Perfluorooctanoic acid and sodium alkylbenzene sulfonate are compounded in a mass ratio of 1:1.

[0085] Solubilizer: Polyvinylpyrrolidone, commercially available, Chinese medicine.

[0086] Untangling agent-1: Hydrocarbon solvent, dichloromethane, commercially available, Chinese medicine.

[0087] Untangling agent-2: Pentaerythritol, commercially available, Chinese medicine.

[0088] Untangling agent-3: Pentaerythritol and a 30% phenolic resin ethanol solution are mixed in a mass ratio of 1:1, wherein the phenolic resin is purchased from Aladdin, product number P195710.

[0089] Maleic anhydride-grafted polypropylene 1: Grafting rate 0.85%, commercially available, Jia Yi Rong Polymer Shanghai Co., Ltd., CMG5701.

[0090] Maleic anhydride-grafted polypropylene 2: grafting rate 1.2%, Bynel 41E1057, DuPont.

[0091] Maleic anhydride-grafted polypropylene 3: grafting rate 7%, Licocene™ PP MA 7452, Clariant.

[0092] Maleic anhydride-grafted polyethylene 1: grafting rate 0.6%, MC226, Nengzhiguang.

[0093] Maleic anhydride-grafted polyethylene 2: grafting rate 0.85%, AR9020, Jia Yi Rong.

[0094] Maleic anhydride grafted onto SEBS: grafting rate 1.7%, FG1901GT, Kraton, USA.

[0095] Grafting rate test methods for Examples 1-8 and Comparative Examples 1-3: According to the formula, the components of the solution for testing the grafting rate of maleic anhydride-grafted polyolefin are mixed evenly, heated to 130°C, and maleic anhydride-grafted polyolefin is added; after the maleic anhydride-grafted polyolefin dissolves, phenolphthalein is added, and titration is immediately performed with potassium hydroxide-ethanol solution while hot.

[0096] The grafting rate test method for Comparative Examples 4-6 was the conventional acid-base titration method, and the specific operation is as follows: Take a sample of maleic anhydride-grafted polyolefin and place it in an Erlenmeyer flask equipped with a reflux condenser. Add boiling xylene and reflux mechanically in a 140°C oil bath for 2 hours under nitrogen protection until the sample is completely dissolved. After cooling to 80°C, add the solution to an acetone-water mixture at 80°C to form a homogeneous solution. Titrate visually with phenolphthalein indicator while hot.

[0097] Statistical calculation methods for test data: To quantify the accuracy and reproducibility of the test results, the following statistical formula is used: variance:

[0098] In the formula: σ 2 : Variance; n: Number of tests (n=5 in this example); xi: Grafting rate value of the i-th test (%); μ: Arithmetic mean of the grafting rates of the n tests.

[0099] Standard deviation:

[0100] Mean square error:

[0101] In the formula: x true : The nominal grafting rate of the sample.

[0102] Mean absolute error:

[0103] Table 1. Parts by weight of each component in the solution compositions used for testing maleic anhydride grafting rate in Examples 1-8

[0104] Table 2. Test results of the solution compositions used in Examples 1-8 for testing the grafting rate of maleic anhydride.

[0105] Table 3. Parts by weight of each component in the solution compositions used for testing maleic anhydride grafting rate in Comparative Examples 1-6

[0106] Table 4. Test results of the solution compositions used in Comparative Examples 1-6 for testing the grafting rate of maleic anhydride.

[0107] As can be seen from Examples 1-8, the average absolute error of the method for testing the grafting rate of maleic anhydride-grafted polyolefins provided by the present invention is less than 0.1, which has high accuracy.

[0108] As can be seen from Comparative Examples 1-6, the absence of any one of the components, such as surfactant, solubilizer, or detangling agent, will increase the mean absolute error. Comparative Examples 3-6 use traditional acid-base titration at a titration temperature of 80℃, which results in problems such as acid evaporation and polyolefin precipitation, thus leading to a higher mean absolute error and poorer accuracy.

Claims

1. A solution composition for testing the grafting rate of maleic anhydride, characterized in that, By weight, it contains the following components: 80-90 parts of main solvent; 5-10 parts of auxiliary solvent; 3-5 parts surfactant; 2-5 parts of solubilizer; 0.05-0.15 parts of untangling agent; Water 0-0.15 parts.

2. The solution composition for testing the grafting rate of maleic anhydride according to claim 1, characterized in that, The main solvent is selected from at least one of alkyl-substituted aromatic hydrocarbons or saturated condensed cyclic aliphatic hydrocarbons, preferably alkyl-substituted aromatic hydrocarbons.

3. The solution composition for testing the grafting rate of maleic anhydride according to claim 1, characterized in that, The auxiliary solvent is selected from at least one of substituted amides, cyclic ethers, C2-C3 short-chain alcohols or C2-C3 polyols, preferably at least one of substituted amides or cyclic ethers.

4. The solution composition for testing the grafting rate of maleic anhydride according to claim 1, characterized in that, The surfactant is selected from at least one of fluorinated surfactants, silicone surfactants, anionic surfactants, nonionic surfactants, cationic surfactants, and amphoteric surfactants, preferably at least one of fluorinated surfactants and silicone surfactants.

5. The solution composition for testing the grafting rate of maleic anhydride according to claim 1, characterized in that, The solubilizer is selected from lactam polymers, preferably from polyvinylpyrrolidone.

6. The solution composition for testing the grafting rate of maleic anhydride according to claim 1, characterized in that, The untangling agent is selected from at least one of halogenated hydrocarbon solvents, polyols, and thermosetting resin solutions.

7. The method for preparing the solution composition for testing the grafting rate of maleic anhydride according to any one of claims 1-6, characterized in that, Simply mix all the components thoroughly.

8. The application of the solution composition according to any one of claims 1-6 for testing the grafting rate of maleic anhydride, characterized in that, Used to test the grafting rate of maleic anhydride-grafted polyolefins.

9. A method for testing the grafting rate of maleic anhydride, characterized in that, The operation steps are as follows: The components of the solution composition for testing the grafting rate of maleic anhydride as described in claim 1 are mixed evenly according to the specified ratio, and then maleic anhydride-grafted polyolefin is added after heating. After the maleic anhydride-grafted polyolefin is dissolved, phenolphthalein is added, and the solution is immediately titrated with potassium hydroxide-ethanol solution while hot.

10. The method for testing the grafting rate of maleic anhydride according to claim 9, characterized in that, The concentration of the potassium hydroxide-ethanol solution is 0.01-0.05 mol / L, and the temperature after heating is 120-130℃.

Citation Information

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