CN107915581A - 一种2,2,3,3,3‑五氟丙醇的制备方法 - Google Patents

一种2,2,3,3,3‑五氟丙醇的制备方法 Download PDF

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CN107915581A
CN107915581A CN201711297031.8A CN201711297031A CN107915581A CN 107915581 A CN107915581 A CN 107915581A CN 201711297031 A CN201711297031 A CN 201711297031A CN 107915581 A CN107915581 A CN 107915581A
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catalyst
propyl alcohol
preparation
fluorine propyl
noble metal
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吕剑
唐晓博
杨志强
韩升
张伟
赵波
亢建平
郝志军
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Xian Modern Chemistry Research Institute
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Abstract

本发明公开了一种2,2,3,3,3‑五氟丙醇的制备方法，在负载型贵金属复合催化剂、溶剂和氧化剂存在的条件下，一步法催化氧化1,1,1,2,2‑五氟丙烷制备2,2,3,3,3‑五氟丙醇，其中，1,1,1,2,2‑五氟丙烷：催化剂：溶剂：氧化剂质量比为1：0.01～0.1：0.5～2：0.05～0.5，本发明的制备2,2,3,3,3‑五氟丙醇的方法具有反应步骤少、操作简单、原料廉价易得、收率高、反应条件温和的优点。

Description

一种2,2,3,3,3-五氟丙醇的制备方法
技术领域
本发明属于氟化工领域，涉及一种2,2,3,3,3-五氟丙醇的制备方法。
背景技术
ODS清洗剂(ODS是“Ozone Depleting Substance”的缩写，意为“消耗臭氧层的物质”)是人类生活和工业普遍应用的一类重要物质，具有低毒、不燃、化学惰性等特点，因此被广泛地用作制冷剂、发泡剂、喷雾剂以及电子元件和精密零件的清洗剂，其使用范围遍及家庭和各行各业，成为现代化生活不可或缺的一类产品。
但是，ODS清洗剂对臭氧层有很强的破坏作用，同时会引起全球气温变暖。根据已生效的《关于消耗臭氧层物质的蒙特利尔议定书》和《中国清洗行业ODS整体淘汰计划》及其《关于中国清洗行业逐步淘汰消耗臭氧层物质(ODS)的协议》规定，我国已经逐步淘汰四氯化碳、1,1,2-三氟-1,2,2-三氯乙烷及1,1,1-三氯乙烷的生产和消费；氢氯氟烷烃(HCFC)计划在2030年完全淘汰。
氢氟醇作为清洗剂，其ODP为零、GWP低，且不燃、表面张力小、洗净能力强，对焊锡助焊剂、机械加工零件上的油脂以及清除粒子及离子污染物方面优于CFC-113、CFC-11，是理想的ODS替代品清洗剂。
2,2,3,3,3-五氟丙醇的沸点为80.7℃，密度为1.51g/cm-3，粘度为2.82mP.s，表面张力为19mN.m-1。2,2,3,3,3-五氟丙醇没有着火点，不易燃，表面张力小，可清洗细小部件；对聚乙二醇、酯油、水溶性焊剂有很好的清洗效果。因此，2,2,3,3,3-五氟丙醇作为清洗剂，其ODP为零、GWP较低，可以在我国淘汰ODS清洗剂的进程中发挥重要的作用，为开辟清洗行业新市场提供技术支撑。
现有合成2,2,3,3,3-五氟丙醇的方法主要为加成法和催化加氢法，均存在合成步骤多，操作复杂，所用试剂价格昂贵，收率低等问题。
发明内容
本发明要解决的技术问题是针对现有技术存在的缺陷与不足，提供一种合成步骤少、操作简单、原料廉价易得、收率高、反应温和的2,2,3,3,3-五氟丙醇的制备方法。
为了实现本发明的目的，本发明在催化剂、氧化剂、溶剂的存在下，以1,1,1,2,2-五氟丙烷为原料一步法催化氧化制备2,2,3,3,3-五氟丙醇，反应温度为50℃～100℃，反应时间为1h～8h；1,1,1,2,2-五氟丙烷：催化剂：溶剂：氧化剂质量比为1：0.01～0.1：0.5～2：0.05～0.5；所述催化剂为负载型贵金属复合催化剂，所述的负载型贵金属复合催化剂组成包括：活性贵金属、载体、助剂金属，所述活性贵金属的质量分数为0.1～10％，所述助剂金属的质量分数为0.05～5，余量为载体。所述活性贵金属为Au、Pt、Pd或Ru，所述载体为活性炭、纤维素、分子筛、沸石、水滑石、无机物氧化或无机氟化物，所述助剂金属为铁、钴、镍、铜、锌、铋、锰、铈、镁、钠、钾的氯化物或氧化物；所述溶剂为甲醇、乙腈、甲苯、异丙醇、二甲基甲酰胺、二甲基亚砜、N-甲基吡咯烷酮或1,4-二氧己烷；所述氧化剂为过氧化氢溶液、有机过氧化物、亚碘酰苯、间氯过苯甲酸或过硫酸钾。
本发明的负载型贵金属复合催化剂的方法，包括下述步骤：(1)贵金属胶体的制备：将无机碱的醇溶液缓慢加入到贵金属前驱体的醇溶液中，充分搅拌1～4h，得到的混合液在氩气保护下，50℃～100℃油浴中加入1～8h，得到贵金属胶体；所述无机碱为NaOH或KOH，所述醇为乙二醇、丙二醇或丁二醇，所述贵金属为H2PtCl6、H2PdCl4或H2AuCl4，所述无机碱的醇溶液浓度为1～20g/L，所述贵金属前驱体的醇溶液浓度为1～100g/L。(2)负载型贵金属复合催化剂的制备：将上述贵金属胶体、助剂金属盐和载体混合，搅拌1～4h，在置于50℃～100℃油浴中加入1～4h，得到的固体经洗涤、抽滤、干燥、压成40～60目的颗粒，在180～250℃下氧气处理1～4h，得到负载型贵金属符合催化剂。
本发明的2,2,3,3,3-五氟丙醇的制备方法是通过间歇法进行，1,1,1,2,2-五氟丙烷、催化剂、溶剂、氧化剂一次性加入至反应器，升至反应温度50℃～100℃，反应时间为1h～8h，反应压力为1.0～2.0MPa。1,1,1,2,2-五氟丙烷：催化剂：溶剂：氧化剂质量比为1：0.01～0.1：0.5～2：0.05～0.5。
本发明的有益效果：
(1)本发明以1,1,1,2,2-五氟丙烷为原料，一步法制备2,2,3,3,3-五氟丙醇，合成步骤少、操作简单、原料廉价易得、收率高、反应温和。
(2)本发明的负载型贵金属复合催化剂，制备简单，活性高、稳定性好。
具体实施方式
下列结合实施例对本发明进一步详述说明，但并不限制本发明的范围。
实施例1
间歇液相氟化反应在带搅拌的300mL不锈钢高压釜中进行。向反应釜中依次投入1g Pt-Fe3O4/C催化剂(其中Pt的质量百分含量为1，Fe的质量百分含量为0.5％)、100g异丙醇、5g过硫酸钾、80g 1,1,1,2,2-五氟丙烷，升温至80℃，反应2h后降温，气相色谱分析有机相，结果表明1,1,1,2,2-五氟丙烷转化率为85.3％，2,2,3,3,3-五氟丙醇的选择性为78.1％。
实施例2～4
实施例2～4制备2,2,3,3,3-五氟丙醇的方法与实施例1相同，所不同的是改变Pt的质量百分含量，反应结果如表1所示。
表1
实施例5～7
实施例5～7制备2,2,3,3,3-五氟丙醇的方法与实施例1相同，所不同的是改变Fe的质量百分含量，反应结果如表2所示。
表2
实施例8～11
实施例8～11制备2,2,3,3,3-五氟丙醇的方法与实施例1相同，所不同的是改变反应时间，反应结果如表3所示。
表3
实施例12～16
实施例12～16制备2,2,3,3,3-五氟丙醇的方法与实施例1相同，所不同的是改变反应温度，反应结果如表4所示。
表4
实施例17～23
实施例17～23制备2,2,3,3,3-五氟丙醇的方法与实施例1相同，所不同的是改变溶剂，反应结果如表5所示。
表5
实施例 溶剂 1,1,1,2,2-五氟丙烷/％ 2,2,3,3,3-五氟丙醇/％
17 甲醇 75.3 76.1
18 乙腈 75.9 77.2
19 甲苯 51.4 46.2
20 二甲基甲酰胺 67.1 73.5
21 二甲基亚砜 47.5 42.8
22 N-甲基吡咯烷酮 78.2 69.8
23 1,4-二氧己烷 74.1 66.4
实施例24～28
实施例24～28制备2,2,3,3,3-五氟丙醇的方法与实施例1相同，所不同的是改变氧化剂，反应结果如表6所示。
表6
实施例 氧化剂 1,1,1,2,2-五氟丙烷/％ 2,2,3,3,3-五氟丙醇/％
24 过氧化氢 71.4 72.3
25 叔丁基过氧化氢 82.4 74.3
26 亚碘酰苯(PhIO) 80.4 72.9
27 二甲基亚砜 68.7 67.4
28 间氯过苯甲酸 70.3 68.2
实施例29～45
实施例29～45制备2,2,3,3,3-五氟丙醇的方法与实施例1相同，所不同的是改变催化剂，反应结果如表7所示。
表7
实施例 催化剂 1,1,1,2,2-五氟丙烷/％ 2,2,3,3,3-五氟丙醇/％
29 Au/Fe3O4/C 82.3 77.7
30 Ru-Fe3O4/C 75.6 71.4
31 Pd-Fe3O4/C 80.7 72.6
32 Pt-Bi2O3/C 88.7 81.7
33 Pt-Al2O3/C 73.3 67.8
34 Pt-CeO2/C 78.4 68.9
35 Pt-CuO/C 74.3 65.2
36 Pt-NiO/C 69.4 65.4
37 Pt-Co2O3/C 76.2 76.7
38 Pt-MnO/C 77.4 70.2
39 Pt-ZnO/C 66.1 71.3
40 Pt-MgO/C 65.2 71.5
41 Pt-NaCl/C 66.1 74.7
42 Pt-KCl/C 65.9 75.2
43 Pt-Bi2O3/SBA-15 86.8 821
44 Pt-Bi2O3/沸石 87.3 80.4
45 Pt-Bi2O3/FeF3 90.1 83.3

Claims (2)

1.一种2,2,3,3,3-五氟丙醇的制备方法，其特征在于在催化剂、氧化剂、溶剂的存在下，以1,1,1,2,2-五氟丙烷为原料一步法催化氧化制备2,2,3,3,3-五氟丙醇，反应温度为50℃～100℃，反应时间为1h～8h，1,1,1,2,2-五氟丙烷：催化剂：溶剂：氧化剂质量比为1：0.01～0.1：0.5～2：0.05～0.5；所述催化剂为负载型贵金属复合催化剂，所述的负载型贵金属复合催化剂组成包括：活性贵金属、载体、助剂金属；所述的活性贵金属的质量分数为0.1～10％，所述助剂金属的质量分数为0.05～5，余量为载体；所述活性贵金属为Au、Pt或Pd，所述载体为活性炭、纤维素、分子筛、沸石、水滑石、无机物氧化或无机氟化物，所述助剂金属为铁、钴、镍、铜、锌、铋、锰、铈、镁、钠、钾的氯化物或氧化物；所述溶剂为甲醇、乙腈、甲苯、异丙醇、二甲基甲酰胺、二甲基亚砜、N-甲基吡咯烷酮或1,4-二氧己烷；所述氧化剂为过氧化氢溶液、有机过氧化物、亚碘酰苯、间氯过苯甲酸或过硫酸钾。
2.根据权利要求1所述的2,2,3,3,3-五氟丙醇的制备方法，所述的负载型贵金属复合催化剂的制备方法，包括下述步骤：(1)贵金属胶体的制备：将无机碱的醇溶液缓慢加入到贵金属前驱体的醇溶液中，充分搅拌1～4h，得到的混合液在氩气保护下，50℃～100℃油浴中加入1～8h，得到贵金属胶体；所述无机碱为NaOH或KOH，所述醇为乙二醇、丙二醇或丁二醇，所述贵金属前驱体为H2PtCl6、H2PdCl4或H2AuCl4，所述无机碱的醇溶液浓度为1～20g/L，所述贵金属前驱体的醇溶液浓度为1～100g/L；
(2)负载型贵金属复合催化剂的制备：将上述贵金属胶体、助剂金属盐和载体混合，搅拌1～4h，在置于50℃～100℃油浴中加入1～4h，得到的固体经洗涤、抽滤、干燥、压成40～60目的颗粒，在180～250℃下氧气处理1～4h，得到负载型贵金属符合催化剂。
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109534953A (zh) * 2018-12-17 2019-03-29 西安近代化学研究所 一种制备2,2,3,3,3-五氟丙醇的方法
CN110981690A (zh) * 2019-12-12 2020-04-10 西安近代化学研究所 一种4,4,5,5,5-五氟戊醇的制备方法
CN111004091A (zh) * 2019-12-12 2020-04-14 西安近代化学研究所 一种制备4,4,5,5,5-五氟戊醇的方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5629458A (en) * 1996-07-26 1997-05-13 Alliedsignal Inc. Process for the preparation of 2 2 2 trifluoroethanol
CN1942422A (zh) * 2004-04-19 2007-04-04 大金工业株式会社 氟烷基酮的水合物的制造方法
CN102648172A (zh) * 2009-10-29 2012-08-22 卡迪夫大学学院顾问有限公司 使用非均相金催化剂进行的烃的选择性氧化
CN102741207A (zh) * 2009-10-29 2012-10-17 帝国科技及医学学院 C1-c3烷烃的选择性催化氧化

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5629458A (en) * 1996-07-26 1997-05-13 Alliedsignal Inc. Process for the preparation of 2 2 2 trifluoroethanol
CN1942422A (zh) * 2004-04-19 2007-04-04 大金工业株式会社 氟烷基酮的水合物的制造方法
CN102648172A (zh) * 2009-10-29 2012-08-22 卡迪夫大学学院顾问有限公司 使用非均相金催化剂进行的烃的选择性氧化
CN102741207A (zh) * 2009-10-29 2012-10-17 帝国科技及医学学院 C1-c3烷烃的选择性催化氧化

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109534953A (zh) * 2018-12-17 2019-03-29 西安近代化学研究所 一种制备2,2,3,3,3-五氟丙醇的方法
CN110981690A (zh) * 2019-12-12 2020-04-10 西安近代化学研究所 一种4,4,5,5,5-五氟戊醇的制备方法
CN111004091A (zh) * 2019-12-12 2020-04-14 西安近代化学研究所 一种制备4,4,5,5,5-五氟戊醇的方法

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