Systems and method for production of furfural comprising combining a xylose-containing solution with an extraction solution comprising water-insoluble boronic acid to provide a first combined solution comprising an aqueous phase and a non-aqueous phase, said non-aqueous phase comprising xylose-diboronate ester (BA.sub.2X); combining at least a portion of the non-aqueous phase with an ionic conversion solution having a pH of less than or equal to 4 and comprising one or more salts to form a second combined solution, wherein the ionic conversion solution has a calculated molar ionic strength of at least 1, heating the second combined solution to convert at least a portion of the xylose-diboronate ester into furfural; separating the second combined solution into a second aqueous phase comprising from a second non-aqueous phase and recovering furfural from the second non-aqueous phase.

This invention relates to a method for the conversion of lignocellulosic biomass into ethyl esters of carboxylic acids. Said method consists of treating the biomass material with an oxidizing agent that is incorporated in an solution comprising one or more acids, one or more alcohols and water, and subsequently performing a catalytic reaction at a higher temperature using the same acidic solution into which a larger volume of alcohol is added, in such a way that the catalytic conversion occurs in a medium with a much higher concentration of alcohol, i.e. with a much higher alcohol-to-water wt ratio. Such a method results in relatively high yields of ethyl esters, such as ethyl esters of formic, acetic, and levulinic acids, while producing a low yield of dialkyl ethers, which are unwanted by-products. The concentration of the oxidizing agent in the pre-treatment step is preferably higher than 6.0 wt %. The oxidizing agent is preferably a Fenton or Fenton-type reagent, and most preferably hydrogen peroxide activated by Fe (II), and/or Ti (IV) ions. The alcohol is preferably ethanol, and when ethanol is used, diethyl ether is formed as the unwanted dialkyl ether by-product. Preferably, the biomass material is pelleted before treatment.

The Notice states that an abstract of the technical disclosure is required. In response, Applicant submits herewith a Preliminary Amendment including an abstract in compliance with 37 CFR § 1.72(b). The abstract is based on that submitted in parent U.S. application Ser. No. 15/556,084 (issued as U.S. Pat. No. 11,193,106) and international application no. PCT/US2016/020621, of which U.S. application Ser. No. 15/556,084 is the US national stage application. The submitted abstract differs from the abstract of the parent application only by a correction of “may further comprising” to “may further comprise”. Thus, the abstract contains no new matter.

The Notice states that an abstract of the technical disclosure is required. In response, Applicant submits herewith a Preliminary Amendment including an abstract in compliance with 37 CFR § 1.72(b). The abstract is based on that submitted in parent U.S. application Ser. No. 15/556,084 (issued as U.S. Pat. No. 11,193,106) and international application no. PCT/US2016/020621, of which U.S. application Ser. No. 15/556,084 is the US national stage application. The submitted abstract differs from the abstract of the parent application only by a correction of “may further comprising” to “may further comprise”. Thus, the abstract contains no new matter.

Disclosed is a method for preparing a solid material including manganese, the method including the following steps: a. bringing into contact an aqueous effluent including manganese, for example at least 5 mg/L, typically at least 5 to 50 mg/L, and preferably 7 to 25 mg/L of manganese, with an oxidizing agent, manganese, preferably at a temperature between 10° C. and 50° C., and obtaining an oxidized aqueous solution; b. adding a base to the oxidized aqueous solution obtained at the end of step a) until a pH of between 8 and 12, preferably greater than 9, and preferably from 9 to 10.5, and obtaining a solution including a precipitate; c. filtration of the solution obtained at the end of step b); and d. obtaining a solid material including manganese, and especially manganese (IV) and/or Mn (III).

Disclosed is a method for preparing a solid material including manganese, the method including the following steps: a. bringing into contact an aqueous effluent including manganese, for example at least 5 mg/L, typically at least 5 to 50 mg/L, and preferably 7 to 25 mg/L of manganese, with an oxidizing agent, manganese, preferably at a temperature between 10° C. and 50° C., and obtaining an oxidized aqueous solution; b. adding a base to the oxidized aqueous solution obtained at the end of step a) until a pH of between 8 and 12, preferably greater than 9, and preferably from 9 to 10.5, and obtaining a solution including a precipitate; c. filtration of the solution obtained at the end of step b); and d. obtaining a solid material including manganese, and especially manganese (IV) and/or Mn (III).

This invention relates to a method for the conversion of lignocellulosic biomass into ethyl esters of carboxylic acids. Said method consists of treating the biomass material with an oxidizing agent that is incorporated in an solution comprising one or more acids, one or more alcohols and water, and subsequently performing a catalytic reaction at a higher temperature using the same acidic solution into which a larger volume of alcohol is added, in such a way that the catalytic conversion occurs in a medium with a much higher concentration of alcohol, i.e. with a much higher alcohol-to-water wt ratio. Such a method results in relatively high yields of ethyl esters, such as ethyl esters of formic, acetic, and levulinic acids, while producing a low yield of dialkyl ethers, which are unwanted by-products. The concentration of the oxidizing agent in the pre-treatment step is preferably higher than 6.0 wt %. The oxidizing agent is preferably a Fenton or Fenton-type reagent, and most preferably hydrogen peroxide activated by Fe (II), and/or Ti (IV) ions. The alcohol is preferably ethanol, and when ethanol is used, diethyl ether is formed as the unwanted dialkyl ether by-product. Preferably, the biomass material is pelleted before treatment.

A process for the production of furfural from a biphasic composition including furfural, an organic solvent and soluble organic debris. The said process includes subjecting the biphasic composition to a liquid-liquid separation step to provide an organic phase and an aqueous phase. The organic phase includes the organic solvent, a first portion of the furfural and a first portion of soluble organic debris. The aqueous phase includes a remainder portion of the furfural and a remainder portion of soluble organic debris. The organic phase is subjected to a distillation step to provide a furfural stream and an organic solvent stream including the organic solvent and the first portion of the soluble organic debris. The organic solvent stream is conveyed to an adsorption unit to adsorb a second portion of the soluble organic debris, forming an organic debris-depleted recycle stream.

A process for the production of furfural from a biphasic composition including furfural, an organic solvent and soluble organic debris. The said process includes subjecting the biphasic composition to a liquid-liquid separation step to provide an organic phase and an aqueous phase. The organic phase includes the organic solvent, a first portion of the furfural and a first portion of soluble organic debris. The aqueous phase includes a remainder portion of the furfural and a remainder portion of soluble organic debris. The organic phase is subjected to a distillation step to provide a furfural stream and an organic solvent stream including the organic solvent and the first portion of the soluble organic debris. The organic solvent stream is conveyed to an adsorption unit to adsorb a second portion of the soluble organic debris, forming an organic debris-depleted recycle stream.

A process for producing levulinic acid includes a step of catalytic conversion of a pentose (in particular xylose or arabinose) into furfural in an organic solvent having a boiling temperature from 60° C. to 220° C., followed by a step of reduction of furfural to furfuryl alcohol, in the presence of a Lewis acid as catalyst and a protic solvent. Eventually, furfuryl alcohol is converted into levulinic acid directly or indirectly, by preliminary conversion into a levulinic acid ester and its subsequent hydrolysis. This process has a reduced environmental impact and guarantees satisfactory process yields on an industrial scale. In particular, the process allows to reduce as much as possible the formation of humins, which require complex and costly purification processes and involve a considerable reduction in the levulinic acid yields.