阅读说明：本技术 一种有机烷基钆水性分散体系的制备方法 (Preparation method of organic alkyl gadolinium aqueous dispersion system ) 是由 张伟禄 张专 赵恢强 张晓霞 于 2018-06-07 设计创作，主要内容包括：一种有机烷基钆水性分散体系的制备方法,所述方法为：称取一定量的表面活性剂混合物溶解于水中,然后投入烷基钆化合物,所述的表面活性剂混合物和烷基钆的质量比为1:10-1:1,室温下搅拌直至溶液变得澄清,即得到烷基钆水性分散体系；所述的表面活性剂混合物选自下列之一：质量比为1:10-1:1的磺丁基醚β-环糊精钠与脂肪醇聚氧乙烯醚类非离子表面活性剂的混合物,或质量比为1:10-1:1的磺丁基醚β-环糊精钠与水溶性高分子聚合物的混合物；其中脂肪醇聚氧乙烯醚类非离子表面活性剂的通式为RO(CH<Sub>2</Sub>CH<Sub>2</Sub>O)<Sub>m</Sub>H,其中R代表C<Sub>12</Sub>～C<Sub>18</Sub>的烷基,m＝20～25；磺丁基醚β-环糊精钠的通式为C<Sub>42</Sub>H<Sub>70-n</Sub>O<Sub>35</Sub>(C<Sub>4</Sub>H<Sub>8</Sub>O<Sub>3</Sub>SNa)<Sub>n</Sub>,n＝5-10；所述的水溶性高分子聚合物为聚乙二醇或聚乙烯醇。本发明显著提高了有机钆盐在水中的溶解度。(A method for preparing an aqueous dispersion of an organoalkyl gadolinium, said method comprising: weighing a certain amount of surfactant mixture, dissolving the surfactant mixture in water, then adding an alkyl gadolinium compound, wherein the mass ratio of the surfactant mixture to the alkyl gadolinium is 1:10-1:1, and stirring at room temperature until the solution becomes clear, thus obtaining an alkyl gadolinium aqueous dispersion system; the surfactant mixture is selected from one of the following: a mixture of sulfobutyl ether beta-cyclodextrin sodium and fatty alcohol polyoxyethylene ether nonionic surfactant in a mass ratio of 1:10-1:1, or a mixture of sulfobutyl ether beta-cyclodextrin sodium and water-soluble high molecular polymer in a mass ratio of 1:10-1: 1; wherein the fatty alcohol polyoxyethylene ether nonionic surfactant has a general formula of RO (CH) 2 CH 2 O) m H, wherein R represents C 12 ～C 18 M is 20 to 25; the general formula of sulfobutyl ether beta-cyclodextrin sodium is C 42 H 70‑n O 35 (C 4 H 8 O 3 SNa) n N is 5-10; the water solution isThe high molecular polymer is polyethylene glycol or polyvinyl alcohol. The invention obviously improves the solubility of the organic gadolinium salt in water.)

1. A method for preparing an aqueous dispersion of an organoalkyl gadolinium, said method comprising: weighing a certain amount of surfactant mixture, dissolving the surfactant mixture in water, then adding an alkyl gadolinium compound, wherein the mass ratio of the surfactant mixture to the alkyl gadolinium is 1:10-1:1, and stirring at room temperature until the solution becomes clear, thus obtaining an alkyl gadolinium aqueous dispersion system;

The surfactant mixture is selected from one of the following: a mixture of sulfobutyl ether beta-cyclodextrin sodium and fatty alcohol polyoxyethylene ether nonionic surfactant in a mass ratio of 1:10-1:1, or a mixture of sulfobutyl ether beta-cyclodextrin sodium and water-soluble high molecular polymer in a mass ratio of 1:10-1: 1; wherein the fatty alcohol polyoxyethylene ether nonionic surfactant has a general formula of RO (CH)₂CH₂O)_mH, wherein R represents C₁₂～C₁₈M is 20 to 25; the general formula of sulfobutyl ether beta-cyclodextrin sodium is C₄₂H_70-nO₃₅(C₄H₈O₃SNa)_nN is 5-10; the water-soluble high molecular polymer is polyethylene glycol or polyvinyl alcohol.

2. The method of claim 1, wherein: the alkyl gadolinium compound is gadolinium dodecyl benzene sulfonate or gadolinium monostearyl succinate sulfonate.

3. The method of claim 1, wherein: the molecular weight of the water-soluble high molecular polymer is 3000-20000 Da.

4. The method according to any one of claims 1 to 3, wherein: the mass ratio of the water to the surfactant mixture is 40:1-20: 1.

5. The method of claim 4, wherein: the stirring temperature is 20-30 ℃.

Technical Field

The invention relates to a preparation method of an organic gadolinium alkyl aqueous dispersion system, in particular to a preparation method of a gadolinium alkyl sulfonate aqueous dispersion system.

Background

The organic gadolinium alkyl salt is not easily soluble in water and has low solubility even in an organic solvent, thereby greatly limiting its application in a liquid phase system. In order to expand the application range of the gadolinium alkyl, it is a feasible solution to disperse the gadolinium alkyl in water to form an aqueous solution dispersion system. Therefore, the preparation of an aqueous solution system of the alkyl gadolinium salt is of great significance for expanding the application of the organic alkyl gadolinium salt.

Disclosure of Invention

The invention aims to provide a preparation method of an aqueous dispersion system of organic gadolinium salt, which is used for remarkably improving the solubility of the organic gadolinium salt in water.

The technical problem to be solved by the invention is specifically realized by the following technical scheme.

A method for preparing an aqueous dispersion of an organoalkyl gadolinium, said method comprising: weighing a certain amount of surfactant mixture, dissolving the surfactant mixture in water, then adding a corresponding amount of alkyl gadolinium compound, wherein the mass ratio of the mixture to the alkyl gadolinium is 1:10-1:1, and stirring at room temperature (20-30 ℃) until the solution becomes clear, thus obtaining an alkyl gadolinium aqueous dispersion system;

The surfactant mixture is selected from one of the following: a mixture of sulfobutyl ether beta-cyclodextrin sodium and fatty alcohol polyoxyethylene ether nonionic surfactant in a mass ratio of 1:10-1:1, or a mixture of sulfobutyl ether beta-cyclodextrin sodium and water-soluble high molecular polymer in a mass ratio of 1:10-1: 1; wherein the fatty alcohol polyoxyethylene ether nonionic surfactant has a general formula of RO (CH)₂CH₂O)_mH, wherein R represents C₁₂～C₁₈M is 20 to 25; the general formula of sulfobutyl ether beta-cyclodextrin sodium is C₄₂H_70-nO₃₅(C₄H₈O₃SNa)_nN is 5-10; the water-soluble high molecular polymer is polyethylene glycol or polyvinyl alcohol.

Further, the gadolinium alkyl is gadolinium alkyl salts such as gadolinium dodecylbenzene sulfonate and gadolinium sulfosuccinate monostearyl amide sulfonate.

Further, the molecular weight of the water-soluble high molecular polymer is 3000-20000 Da.

Further, the mass ratio of the water to the surfactant mixture is 40:1-20: 1.

The invention selects a mixture of sulfobutyl ether beta-cyclodextrin sodium anionic surfactant and fatty alcohol polyoxyethylene ether nonionic surfactant or water-soluble high molecular polymer (molecular weight is 3000Da-20000Da) to solubilize organic gadolinium alkyl such as gadolinium dodecyl benzene sulfonate, gadolinium succinyl monostearate sulfonate and the like, and prepares an aqueous solution dispersion system of the gadolinium alkyl. The solubilization principle of the mixed solubilizer mainly lies in that: (1) the nonionic surfactant and the anionic surfactant are compatible and dissolved in water to form an oil-in-water mixed micelle, and the alkyl gadolinium is wrapped in the inner core of the micelle, so that the solubility of the organic alkyl gadolinium is improved; (2) the insoluble organic gadolinium salt can form an inclusion compound with sulfobutyl ether beta-cyclodextrin sodium, and the water solubility of the organic gadolinium salt is further improved. By these two means, gadolinium alkyls can be well dispersed in water.

The organic alkyl gadolinium aqueous dispersion system prepared by the method is expected to be used in the fields of nuclear magnetic resonance imaging radiography, fluorine-free refrigeration and the like.

Compared with the prior art, the invention has the beneficial effects that: by using a mixture of sulfobutyl ether beta-cyclodextrin sodium anionic surfactant and fatty alcohol polyoxyethylene ether nonionic surfactant or water-soluble high-molecular polymer as a solubilizer, the solubility of organic gadolinium alkyl such as gadolinium dodecyl benzene sulfonate, gadolinium succinyl monostearate amide sulfonate and the like in water is remarkably improved, and an alkyl gadolinium aqueous solution dispersion system with high solid content can be prepared. The solubilizing capacity is improved by more than 80 times compared with the solubilizing capacity of the conventional surfactant.

Detailed Description

The present invention will be described in detail with reference to examples, which are only preferred embodiments of the present invention and are not intended to limit the present invention.

The raw material components are commercially available, wherein sulfobutyl ether beta-cyclodextrin sodium is purchased from Zhiyuan Biotech limited, Shandong, Binshui, fatty alcohol-polyoxyethylene ether is purchased from Haian petrochemical plant of Jiangsu province, and polyethylene glycol is purchased from Haian petrochemical plant of Jiangsu province.