CN-121975098-A - Polyethylene sebacate resin and preparation method and application thereof
Abstract
The invention relates to a polyethylene sebacate resin, a preparation method and application thereof, belonging to the technical field of organic high polymer compounds. The preparation method of the polyethylene sebacate resin comprises the following steps of S1, mixing sebacic acid, ethylene glycol, a catalyst and an inhibitor for esterification reaction to obtain an esterified substance, S2, carrying out low-compression polymerization on the esterified substance obtained in the S1 to obtain the polyethylene sebacate resin, wherein the inhibitor is ethylene carbonate, and the chromatographic purity of the ethylene glycol is based on the GB/T14571.2-2018 standard, wherein the chromatographic peak area of the inhibitor is 0.1% -0.9% of the sum of the chromatographic peak areas of the inhibitor and the ethylene glycol in the mixture of the ethylene glycol and the inhibitor. The preparation method provided by the invention can effectively reduce the content of acetaldehyde in the esterified water.
Inventors
- GUO ZHILONG
- CHEN PINGXU
- OUYANG CHUNPING
- ZENG XIANGBIN
- HUANG XIANBO
Assignees
- 珠海金发生物材料有限公司
- 金发科技股份有限公司
Dates
- Publication Date
- 20260505
- Application Date
- 20260210
Claims (10)
- 1. The preparation method of the polyethylene sebacate resin is characterized by comprising the following steps of: s1, mixing sebacic acid, glycol, a catalyst and an inhibitor to perform esterification reaction to obtain an esterified substance; S2, carrying out low-compression polymerization on the esterified substance obtained in the step S1 to obtain the polyethylene sebacate resin; The inhibitor is ethylene carbonate, and the chromatographic peak area of the inhibitor in the mixture of the ethylene glycol and the inhibitor is 0.1% -0.9% of the sum of the chromatographic peak areas of the inhibitor and the ethylene glycol according to the GB/T14571.2-2018 standard.
- 2. The method for preparing polyethylene sebacate resin according to claim 1, wherein the chromatographic peak area of the inhibitor is 0.4% -0.7% of the sum of the chromatographic peak areas of the inhibitor and the ethylene glycol.
- 3. The method for preparing polyethylene sebacate resin according to claim 2, wherein the chromatographic peak area of the inhibitor is 0.5% -0.6% of the sum of the chromatographic peak areas of the inhibitor and the ethylene glycol.
- 4. The preparation method of the polyethylene sebacate resin according to claim 1, wherein the esterification reaction in the step S1 is to heat the mixed components to 180-200 ℃ in nitrogen atmosphere, and react for 2.5-4.5 h.
- 5. The preparation method of the polyethylene sebacate resin according to claim 1, wherein the low-compression polymerization reaction in the step S2 is carried out under the pressure of less than or equal to 60Pa until the intrinsic viscosity of a system reaches 1.2 dL/g-1.4 dL/g, nitrogen is filled, and the polyethylene sebacate resin is obtained through extrusion granulation.
- 6. The method for preparing polyethylene sebacate resin according to claim 5, wherein the reaction temperature in the step S2 is 225-240 ℃ and the reaction time is 3-4.5 h.
- 7. The method for preparing polyethylene sebacate resin according to claim 1, wherein the catalyst in the step S1 comprises at least one of tetrabutyl orthotitanate and tetraisopropyl orthotitanate.
- 8. The polyethylene sebacate resin produced by the production method of the polyethylene sebacate resin of any one of claims 1 to 7.
- 9. Use of the polyethylene sebacate resin of claim 8 for the preparation of films, foamed materials or injection molded articles.
- 10. A polyethylene sebacate resin article comprising the polyethylene sebacate resin of claim 8.
Description
Polyethylene sebacate resin and preparation method and application thereof Technical Field The invention relates to the technical field of organic high molecular compounds, in particular to polyethylene sebacate resin, a preparation method and application thereof. Background The polyethylene sebacate resin is one of the very active degradation materials in the current biodegradable plastic research, and has ultrahigh flexibility and unique mechanical properties. The polyethylene sebacate resin is generally prepared by polymerizing sebacic acid and ethylene glycol through a high-temperature esterification reaction, however, in the high-temperature esterification reaction, ethylene Glycol (EG) can undergo side reactions such as oxidation and the like to generate Acetaldehyde (ACE) and water, after the high-temperature esterification reaction is finished and the polyethylene sebacate resin is collected, the mixture containing EG, ACE, water and other gases can be discharged after being subjected to subsequent EG purification and other treatments, and in the purification process, the higher the content of Acetaldehyde (ACE), the higher the purification difficulty, the higher the energy consumption, so that the reduction of the acetaldehyde output in the esterification process has important significance. Disclosure of Invention The invention aims to overcome the defects of the prior art and provide a polyethylene sebacate resin, a preparation method and application thereof. In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: in a first aspect, the invention provides a method for preparing polyethylene sebacate resin, comprising the following steps: s1, mixing sebacic acid, glycol, a catalyst and an inhibitor to perform esterification reaction to obtain an esterified substance; S2, carrying out low-compression polymerization on the esterified substance obtained in the step S1 to obtain the polyethylene sebacate resin; The inhibitor is ethylene carbonate (CAS number: 96-49-1), and the chromatographic peak area of the inhibitor in the mixture of the ethylene glycol and the inhibitor is 0.1% -0.9% of the sum of the chromatographic peak areas of the inhibitor and the ethylene glycol based on the chromatographic purity of the ethylene glycol according to the GB/T14571.2-2018 standard. According to the preparation method of the polyethylene sebacate resin, provided by the invention, ethylene carbonate is used as an inhibitor, so that the generation of acetaldehyde which is a byproduct in the high-temperature esterification reaction process of sebacic acid and ethylene glycol can be inhibited, the content of acetaldehyde is reduced, and the difficulty in separating and purifying ethylene glycol in the subsequent waste liquid can be effectively reduced. The source of the inhibitor ethylene carbonate is not particularly limited, and may be an impurity present in ethylene glycol or directly added ethylene carbonate, and the present inventors have found that the range defined in the present invention is satisfied by the chromatographic peak area of the inhibitor ethylene carbonate/(the chromatographic peak area of the inhibitor ethylene carbonate+the chromatographic peak area of ethylene glycol). Alternatively, the chromatographic peak area of the inhibitor/(the chromatographic peak area of the inhibitor+the chromatographic peak area of ethylene glycol) may specifically be a range value of any one or any two of 0.1%, 0.15%, 0.2%, 0.25%, 0.3%, 0.35%, 0.4%, 0.45%, 0.5%, 0.55%, 0.6%, 0.65%, 0.7%, 0.75%, 0.8%, 0.85%, 0.9%. The chromatographic peak area can be obtained by calculation through a chromatograph, and the specific test method of the chromatographic peak area comprises the steps of dissolving the inhibitor raw material in the ethylene glycol raw material and mixing before the S1 esterification reaction, and obtaining the integral area of the chromatographic peak by test calculation through the gas chromatograph according to the GB/T14571.2-2018 standard. Wherein, the chromatographic peak area of the inhibitor and the percentage of the inhibitor to the sum of the chromatographic peak areas of the glycol can be regulated and controlled by controlling the adding amount of the inhibitor. As a preferred embodiment of the preparation method of the polyethylene sebacate resin, the chromatographic peak area of the inhibitor is 0.4% -0.7% of the sum of the chromatographic peak areas of the inhibitor and the ethylene glycol. As a preferred embodiment of the preparation method of the polyethylene sebacate resin, the chromatographic peak area of the inhibitor is 0.5% -0.6% of the sum of the chromatographic peak areas of the inhibitor and the ethylene glycol. As a preferred implementation mode of the preparation method of the polyethylene sebacate resin, according to GB/T14571.2-2018 standard, the retention time of ethylene glycol is 10.3-10.7 min, and the retention time of the inhibi