Method for producing aqueous hydrogen peroxide solution

文档序号:957749 发布日期:2020-10-30 浏览:13次 中文

阅读说明:本技术 用于制造过氧化氢水溶液的方法 (Method for producing aqueous hydrogen peroxide solution ) 是由 J-T·卡利尔 P·杜内尔 K·洛伦特 于 2019-03-19 设计创作,主要内容包括:披露了一种用于制造过氧化氢水溶液的方法,该方法包括以下步骤:-氢化工作溶液,该工作溶液包含烷基蒽醌和/或四氢烷基蒽醌以及非极性有机溶剂和极性有机溶剂的混合物,其中所述混合物中的非极性有机溶剂的浓度等于或高于30wt%;-氧化该氢化的工作溶液以产生过氧化氢;以及-分离该过氧化氢,其中该极性有机溶剂是取代的环己烷腈。(Disclosed is a method for producing an aqueous hydrogen peroxide solution, comprising the steps of: -a hydrogenated working solution comprising alkylanthraquinones and/or tetrahydroalkylanthraquinones and a mixture of a non-polar organic solvent and a polar organic solvent, wherein the concentration of the non-polar organic solvent in said mixture is equal to or higher than 30 wt%; -oxidizing the hydrogenated working solution to produce hydrogen peroxide; and-separating the hydrogen peroxide, wherein the polar organic solvent is a substituted cyclohexanecarbonitrile.)

1. A method for producing an aqueous hydrogen peroxide solution, the method comprising the steps of:

-a hydrogenated working solution comprising alkylanthraquinones and/or tetrahydroalkylanthraquinones and a mixture of a non-polar organic solvent and a polar organic solvent, wherein the concentration of the non-polar organic solvent in said mixture is equal to or higher than 30 wt%;

-oxidizing the hydrogenated working solution to produce hydrogen peroxide; and

-separating the hydrogen peroxide from the aqueous solution,

wherein the polar organic solvent is a substituted cyclohexanecarbonitrile.

2. The process according to claim 1, which is a continuous process, wherein the working solution is circulated in a loop through the hydrogenation, oxidation and purification steps.

3. The process according to claim 1 or 2, wherein the alkylanthraquinone is selected from the group consisting of: ethylanthraquinones like 2-Ethylanthraquinone (EQ), 2-isopropylanthraquinone, 2-sec-and 2-tert-Butylanthraquinone (BQ), 1,3-, 2,3-, 1, 4-and 2, 7-dimethylanthraquinone, Amylanthraquinone (AQ) like 2-iso-and 2-tert-amylanthraquinone, and mixtures of these quinones.

4. The method according to claim 3, wherein the quinone is EQ, BQ or AQ, preferably EQ.

5. Process according to any one of the preceding claims, wherein the substituent(s) of the substituted cyclohexanecarbonitrile are one or more alkyl groups, preferably one or more methyl and/or ethyl groups.

6. Process according to claim 5, wherein the cyclohexanecarbonitrile is substituted with at least 2 methyl groups, preferably at least 3 methyl groups and more preferably at least 4 methyl groups.

7. Process according to any one of the preceding claims, in which the cyclohexanecarbonitrile has one or more substituents close to the nitrile function, preferably in the 1, 2 and/or 6 position.

8. Process according to any one of claims 1 to 6, wherein the substituted cyclohexanecarbonitrile is 3, 5-dimethylcyclohexane-1-carbonitrile.

9. Process according to any one of claims 1 to 6, wherein the substituted cyclohexanecarbonitrile is 2,2, 6-trimethyl-cyclohexane-carbonitrile or 1,3, 3-trimethyl-cyclohexane-carbonitrile.

10. Process according to the preceding claim, wherein the substituted cyclohexanecarbonitrile is 2,2, 6-trimethyl-cyclohexane-carbonitrile, which is synthesized starting from the corresponding acid (2,2, 6-trimethyl-cyclohexane-carboxylic acid), which is first converted into the corresponding carboxylic chloride using thionyl chloride, then into the corresponding amide using ammonia, and finally into the corresponding nitrile using phosphorus pentoxide.

11. The process according to claim 9, wherein the substituted cyclohexanecarbonitrile is 1,3, 3-trimethyl

-cyclohexane-carbonitrile synthesized by a process comprising the steps of:

-reacting diethylaluminum cyanide with isophorone;

-reduction of the keto group with sodium borohydride to obtain a mixture of diastereomers of 3-cyano-3, 5, 5-trimethylcyclohexanol;

-reacting the mixture with methanesulfonyl chloride;

-elimination of methanesulfonic acid and leaving a mixture of cyano-olefins;

hydrogenation of these resulting olefins in methanol over 10% Pd/C.

12. Process according to any one of claims 1 to 7, wherein the substituted cyclohexanecarbonitrile is synthesized in a 2-step reaction comprising: first reacting a conjugated diene with a dienophile bearing a nitrile group to obtain a substituted cyclohexenenitrile; and secondly hydrogenating the double bond of the substituted cyclohexenenitrile, wherein at least one of the conjugated diene or the dienophile is preferably substituted by at least one methyl group.

13. A process according to any one of the preceding claims, wherein no more than 80 wt%, preferably no more than 60 wt% of non-polar organic solvent is present in the organic solvent mixture.

14. The process according to any one of the preceding claims, wherein the non-polar organic solvent is an aromatic solvent or a mixture of aromatic solvents.

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