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US 10,954,256 B2Granted
Process for recovering a mixture comprising a (thio)phosphoric acid derivative
AssigneeBASF SE
InventorsTobias Lang, Karl-Heinrich Schneider, Zoltan Baan, Philip Muelheims, Steffen Tschirschwitz, Sascha Shuxia Zhu
Life of this patent
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Abstract
Provided herein is a use of a high-boiling solvent in a mixture comprising a (thio)phosphoric acid derivative and a process including the addition of a high-boiling solvent to a mixture comprising a (thio)phosphoric acid derivative to recover the (thio)phosphoric acid from the mixture by an evaporation process.
Claims6
A method of using at least one high-boiling solvent having a boiling point of at least 130° C., in a mixture comprising at least one (thio)phosphoric acid derivative and at least one volatile component, for preventing decomposition or solids formation of the at least one (thio)phosphoric acid derivative in an evaporation process, wherein said evaporation process comprises:
- separating the at least one (thio)phosphoric acid derivative from the at least one volatile component, wherein the at least one volatile component is selected from the group consisting of liquid paraffinic, cycloparaffinic, and/or aromatic hydrocarbons, liquid halocarbons and halohydrocarbons, ethers, and esters;
- and
- recovering as a bottom product a first mixture (1) comprising components:
- (1a) the at least one (thio)phosphoric acid derivative;
- and
- (1b) the at least one high-boiling solvent, wherein the at least one (thio)phosphoric acid derivative is selected from the group consisting of:
- (thio)phosphoric acid triamides according to general formula (I) and (thio)phosphoric acid ester amides according to general formula (IIa) or (IIb);
- wherein general formula (I) is
- wherein
- X1 is O or S;
- R1 is C1-C20-alkyl, C3-C20-cycloalkyl, C6-C20-aryl, C6-C20-aryl-C1-C4-alkyl, or C1-C6-(di)alkylaminocarbonyl;
- R2 is H, C1-C20-alkyl, C3-C20-cycloalkyl, C6-C20-aryl, C6-C20-aryl-C1-C4-alkyl, or C1-C6-(di)alkylaminocarbonyl;
- or
- R1 and R2 together with the nitrogen atom linking them define a 5- or 6-membered saturated or unsaturated heterocyclic radical, which optionally comprises 1 or 2 further heteroatoms selected from the group consisting of N, O, and S;
- and
- R3, R4, R5, and R6 are independently of each other selected from the group consisting of H and C1-C4-alkyl;
- and wherein general formula (IIa) is
- wherein
- X2 is O or S;
- R7 is C1-C20-alkyl, C3-C20-cycloalkyl, C6-C20-aryl, C6-C20-aryl-C1-C4-alkyl, or C1-C6-(di)alkylaminocarbonyl;
- and
- R8, R9, R10, and R11 are independently of each other selected from the group consisting of H and C1-C4-alkyl;
- and wherein general formula (IIb) is
- wherein
- X3 is O or S;
- R12 is C1-C20-alkyl, C3-C20-cycloalkyl, C6-C20-aryl, C6-C20-aryl-C1-C4-alkyl, or C1-C6-(di)alkylaminocarbonyl;
- R15 is C1-C20-alkyl, C3-C20-cycloalkyl, C6-C20-aryl, C6-C20-aryl-C1-C4-alkyl, or C1-C6-(di)alkylaminocarbonyl;
- and
- R13 and R14 are independently of each other selected from the group consisting of H and C1-C4-alkyl, and
- wherein the at least one high-boiling solvent is hydrophilic.
27 more elements
A process for recovering at least one (thio)phosphoric acid derivative from a first mixture comprising the at least one (thio)phosphoric acid derivative and at least one solvent, wherein the process comprises:
- adding at least one high-boiling solvent having a boiling point of at least 130° C. to the first mixture so as to form a second mixture (2) comprising components:
- (2a) the at least one (thio)phosphoric acid derivative;
- (2b) the at least one high-boiling solvent;
- and
- (2c) the at least one solvent, the at least one solvent having a boiling point that is at least 30° C. lower than the boiling point of the at least one high-boiling solvent to be and is selected from liquid paraffinic, cycloparaffinic, and/or aromatic hydrocarbons, liquid halocarbons and halohydrocarbons, ethers, and esters;
- and
- and separating a third mixture (1) from said second mixture (2), wherein said third mixture (1) comprises components:
- (1a) the at least one (thio)phosphoric acid derivative;
- and
- (1b) the at least one high-boiling solvent;
- by evaporating the at least one solvent component (2c) of the second mixture (2) and collecting the third mixture (1) as a bottom product, wherein the at least one (thio)phosphoric acid derivative is selected from the group consisting of:
- (thio)phosphoric acid triamides according to general formula (I) and (thio)phosphoric acid ester amides according to general formula (IIa) or (IIb);
- wherein general formula (I) is
- wherein
- X1 is O or S;
- R1 is C1-C20-alkyl, C3-C20-cycloalkyl, C6-C20-aryl, C6-C20-aryl-C1-C4-alkyl, or C1-C6-(di)alkylaminocarbonyl;
- R2 is H, C3-C20-cycloalkyl, C6-C20-aryl, C6-C20-aryl-C1-C4-alkyl, or C1-C6-(di)alkylaminocarbonyl;
- or
- R1 and R2 together with the nitrogen atom linking them define a 5- or 6-membered saturated or unsaturated heterocyclic radical, which optionally comprises 1 or 2 further heteroatoms selected from the group consisting of N, O, and S;
- and
- R3, R4, R5, and R6 are independently of each other selected from the group consisting of H and C1-C4-alkyl;
- and wherein general formula (IIa) is
- wherein
- X2 is O or S;
- R7 is C1-C20-alkyl, C3-C20-cycloalkyl, C6-C20-aryl, C6-C20-aryl-C1-C4-alkyl, or C1-C6-(di)alkylaminocarbonyl;
- and
- R8, R9, R10, and R11 are independently of each other selected from the group consisting of H and C1-C4-alkyl;
- and wherein general formula (IIb) is
- wherein
- X3 is O or S;
- R12 is C1-C20-alkyl, C3-C20-cycloalkyl, C6-C20-aryl, C6-C20-aryl-C1-C4-alkyl, or C1-C6-(di)alkylaminocarbonyl;
- R15 is C1-C20-alkyl, C3-C20-cycloalkyl, C6-C20-aryl, C6-C20-aryl-C1-C4-alkyl, or C1-C6-(di)alkylaminocarbonyl;
- and
- R13 and R14 are independently of each other selected from the group consisting of H and C1-C4-alkyl, and
- wherein the at least one high-boiling solvent is hydrophilic.
32 more elements
Dependencies are inferred from the claim text.