Mingyang Hu, Hexiong Yang, Xiaojia Huo and Bin Lian
{"title":"半水合乙醇酸钾†的合成、结构、表征及降解","authors":"Mingyang Hu, Hexiong Yang, Xiaojia Huo and Bin Lian","doi":"10.1039/D5CE00182J","DOIUrl":null,"url":null,"abstract":"<p >The process of glycolate crystallization is well documented; however, research on the formation of potassium chelate with glycolate and the characteristics of the resulting crystals remains limited. In this study, a potassium glycolate hemihydrate (PGH) crystal, ideally K(C<small><sub>2</sub></small>H<small><sub>3</sub></small>O<small><sub>3</sub></small>)·0.5H<small><sub>2</sub></small>O, was obtained by freeze-drying, evaporation, and liquid phase diffusion. PGH was characterized by single-crystal X-ray diffraction, Fourier transform infrared spectroscopy, Raman spectroscopy, DFT calculation, thermogravimetric analysis, and powder X-ray diffraction refinement. A structurally similar compound, potassium glycolate glycolic acid [K(C<small><sub>2</sub></small>H<small><sub>3</sub></small>O<small><sub>3</sub></small>)(C<small><sub>2</sub></small>H<small><sub>4</sub></small>O<small><sub>3</sub></small>), PGGA], was synthesized for comparison. The results revealed that PGH is monoclinic with the space group <em>P</em>2<small><sub>1</sub></small>/<em>m</em> and unit cell parameters <em>a</em> = 5.8982(1), <em>b</em> = 7.2515(1), <em>c</em> = 11.0270(1) Å, <em>β</em> = 102.253(1)°, and <em>V</em> = 460.890(11) Å<small><sup>3</sup></small>. The infrared and Raman spectra of PGH and PGGA exhibit notable similarities and are highly consistent with the calculated infrared spectra calculated. Thermogravimetric analysis indicated that PGH dehydrated at approximately 60 °C; however, further experiments showed that PGH gradually transformed into PGGA at 30 °C. This study provides new insights into the bonding behavior of glycolate and the stability of its crystalline forms.</p>","PeriodicalId":70,"journal":{"name":"CrystEngComm","volume":" 28","pages":" 4816-4825"},"PeriodicalIF":2.6000,"publicationDate":"2025-05-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Synthesis, structures, characterization and deterioration of potassium glycolate hemihydrate†\",\"authors\":\"Mingyang Hu, Hexiong Yang, Xiaojia Huo and Bin Lian\",\"doi\":\"10.1039/D5CE00182J\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p >The process of glycolate crystallization is well documented; however, research on the formation of potassium chelate with glycolate and the characteristics of the resulting crystals remains limited. In this study, a potassium glycolate hemihydrate (PGH) crystal, ideally K(C<small><sub>2</sub></small>H<small><sub>3</sub></small>O<small><sub>3</sub></small>)·0.5H<small><sub>2</sub></small>O, was obtained by freeze-drying, evaporation, and liquid phase diffusion. PGH was characterized by single-crystal X-ray diffraction, Fourier transform infrared spectroscopy, Raman spectroscopy, DFT calculation, thermogravimetric analysis, and powder X-ray diffraction refinement. A structurally similar compound, potassium glycolate glycolic acid [K(C<small><sub>2</sub></small>H<small><sub>3</sub></small>O<small><sub>3</sub></small>)(C<small><sub>2</sub></small>H<small><sub>4</sub></small>O<small><sub>3</sub></small>), PGGA], was synthesized for comparison. The results revealed that PGH is monoclinic with the space group <em>P</em>2<small><sub>1</sub></small>/<em>m</em> and unit cell parameters <em>a</em> = 5.8982(1), <em>b</em> = 7.2515(1), <em>c</em> = 11.0270(1) Å, <em>β</em> = 102.253(1)°, and <em>V</em> = 460.890(11) Å<small><sup>3</sup></small>. The infrared and Raman spectra of PGH and PGGA exhibit notable similarities and are highly consistent with the calculated infrared spectra calculated. Thermogravimetric analysis indicated that PGH dehydrated at approximately 60 °C; however, further experiments showed that PGH gradually transformed into PGGA at 30 °C. This study provides new insights into the bonding behavior of glycolate and the stability of its crystalline forms.</p>\",\"PeriodicalId\":70,\"journal\":{\"name\":\"CrystEngComm\",\"volume\":\" 28\",\"pages\":\" 4816-4825\"},\"PeriodicalIF\":2.6000,\"publicationDate\":\"2025-05-29\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"CrystEngComm\",\"FirstCategoryId\":\"92\",\"ListUrlMain\":\"https://pubs.rsc.org/en/content/articlelanding/2025/ce/d5ce00182j\",\"RegionNum\":3,\"RegionCategory\":\"化学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q2\",\"JCRName\":\"CHEMISTRY, MULTIDISCIPLINARY\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"CrystEngComm","FirstCategoryId":"92","ListUrlMain":"https://pubs.rsc.org/en/content/articlelanding/2025/ce/d5ce00182j","RegionNum":3,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q2","JCRName":"CHEMISTRY, MULTIDISCIPLINARY","Score":null,"Total":0}
引用次数: 0
摘要
乙醇酸结晶的过程有很好的文献记载;然而,对乙醇酸盐与钾螯合物的形成及其晶体特性的研究仍然有限。本研究通过冷冻干燥、蒸发和液相扩散得到半水合乙醇酸钾(PGH)晶体,理想状态为K(C2H3O3)·0.5H2O。采用单晶x射线衍射、傅里叶变换红外光谱、拉曼光谱、DFT计算、热重分析和粉末x射线衍射细化等方法对PGH进行了表征。合成了结构相似的化合物乙醇酸钾乙醇酸[K(C2H3O3)(C2H4O3), PGGA]进行比较。结果表明,PGH呈单斜状,空间群为P21/m,胞参数a = 5.8982(1), b = 7.2515(1), c = 11.0270(1) Å, β = 102.253(1)°,V = 4600.890 (11) Å3。PGH和PGGA的红外光谱和拉曼光谱具有显著的相似性,与计算得到的红外光谱高度一致。热重分析表明,PGH在60℃左右脱水;然而,进一步的实验表明,在30°C时,PGH逐渐转化为PGGA。该研究为乙醇酸盐的键合行为及其结晶形式的稳定性提供了新的见解。
Synthesis, structures, characterization and deterioration of potassium glycolate hemihydrate†
The process of glycolate crystallization is well documented; however, research on the formation of potassium chelate with glycolate and the characteristics of the resulting crystals remains limited. In this study, a potassium glycolate hemihydrate (PGH) crystal, ideally K(C2H3O3)·0.5H2O, was obtained by freeze-drying, evaporation, and liquid phase diffusion. PGH was characterized by single-crystal X-ray diffraction, Fourier transform infrared spectroscopy, Raman spectroscopy, DFT calculation, thermogravimetric analysis, and powder X-ray diffraction refinement. A structurally similar compound, potassium glycolate glycolic acid [K(C2H3O3)(C2H4O3), PGGA], was synthesized for comparison. The results revealed that PGH is monoclinic with the space group P21/m and unit cell parameters a = 5.8982(1), b = 7.2515(1), c = 11.0270(1) Å, β = 102.253(1)°, and V = 460.890(11) Å3. The infrared and Raman spectra of PGH and PGGA exhibit notable similarities and are highly consistent with the calculated infrared spectra calculated. Thermogravimetric analysis indicated that PGH dehydrated at approximately 60 °C; however, further experiments showed that PGH gradually transformed into PGGA at 30 °C. This study provides new insights into the bonding behavior of glycolate and the stability of its crystalline forms.