A process for removing impurities from a crystallized metal sulfate, including contacting crystallized metal sulfate with a liquor rich in metal sulfate. The metal may be cobalt, nickel, or manganese, and the impurities may be magnesium or calcium. The liquor rich in metal sulfate may be an overflow liquor from crystallization of the metal sulfate, and said overflow liquor may be subject to one or more impurities removal steps prior to contacting the crystallized metal sulfate, such that the overflow liquor contains lower levels of impurities than the crystallized metal sulfate to be contacted. A counter-current wash circuit may be used to remove impurities from a crystallized metal sulfate, whereby a plurality of washing tanks are configured to receive crystallized metal sulfate in a sequence, and washing liquor in reverse of said sequence.

The present invention relates to means and methods for producing crystals or crystalline substances in a contained vessel. In particular, crystals or crystalline substances, which are useful as pharmaceutical ingredients, can be manufactured.

A method of making CBD concentrate or CBD Isolate comprises (a) milling a raw material; (b) contacting the milled raw material with an extraction solvent and separating a solid waste material to form a filtered extract; (c) concentrating the filtered extract; (d) washing the concentrated extract to form an organic phase and an aqueous phase; (e) separating the aqueous phase from the organic phase to form a washed extract; (f) removing an organic solvent from the washed extract to form a concentrated washed extract; (g) decarboxylating the concentrated washed extract; (h) vacuum distilling the decarboxylated extract to form a distillate; (i) dewaxing the distillate to form a post-dewax filtrate; (j) applying a vacuum to the post-dewax filtrate to form a post-dewax concentrate; (k) degassing the post-dewax concentrate; and (l) vacuum distilling the degassed concentrate to form a CBD concentrate.

A method of isomerizing Δ9-tetrahydrocannabinol (“Δ9-THC”) to Δ10-tetrahydrocannabinol (“Δ10-THC”). The method includes the steps of: extracting Δ9-THC from cannabis biomass, which optionally contains one or more of the components found in fire retardant such as PHOS-CHEK®; dewaxing of crude extracts by winterization; pH-adjusting extracts by washing the extracts in heptane solution with aqueous solutions of: citric acid, sodium bicarbonate, and brine; isomerizing Δ9-THC to Δ10-THC by exposure to suitable conditions and in the presence of a catalyst based on the components of fire retardant; vacuum distillation of Δ10-THC at a predetermined temperature range and vacuum level; collecting the distillate and redistilling it up to three times to acquire distillate containing less than 60% Δ10-THC; and purification of the MO-THC to a purity of 99% or greater by crystallization from n-pentane solution.

The present invention describes a process for the production of (−)-cannabidiol (CBD) from industrial hemp by means of an extraction followed by two alternative working processes: a process A which provides extraction with solvents first to an alkaline pH and then to acidic pH to isolate the carboxyl form of the CBD which is then subjected to decarboxylation and a process B which provides the elimination of waxes and pitches and then purification by chromatography. At the end of both alternative working processes the CBD is crystallized obtained in high purity crystalline form.

The invention provides a process for the production of crystalline ammonium sulfate, wherein the process comprises performing a Beckmann rearrangement reaction, neutralizing the Beckmann rearrangement reaction mixture, separating a first aqueous ammonium sulfate phase and an aqueous ε-caprolactam phase, charging the first ammonium sulfate phase to a first evaporative type crystallization section wherein crystalline ammonium sulfate is obtained, discharging from the first evaporative type crystallization section mother liquor enriched in organic components, extracting the aqueous ε-caprolactam phase to obtain an extracted ε-caprolactam phase and a second aqueous ammonium sulfate phase, discharging the mother liquor that is discharged from the first evaporative type crystallization section and/or the second aqueous ammonium sulfate phase to a second evaporative type crystallization section wherein evaporative type crystallization is performed so that a three-phase system occurs. At least a liquid oily phase is recovered from the three-phase system. The invention further provides a plant suitable to carry out the process of the invention, crystalline ammonium sulfate and a liquid oily phase obtained by the process of the invention.

An object of the present invention is to provide a method for producing a bis(fluorosulfonyl)amide alkali metal salt powder having high purity while suppressing reduction in yield due to thermal decomposition, etc. The method for producing a bis(fluorosulfonyl)amide alkali metal salt powder according to the present invention comprises precipitating a bis(fluorosulfonyl)amide alkali metal salt by conducting distillation using a thin-film evaporator while adding a poor solvent for the bis(fluorosulfonyl)amide alkali metal salt such as an aromatic hydrocarbon solvent and a linear or branched aliphatic hydrocarbon solvent to a solution formed by dissolving the bis(fluorosulfonyl)amide alkali metal salt in a good solvent for the bis(fluorosulfonyl)amide alkali metal salt such as an ester solvent and nitrile solvent.

Disclosed are methods for separating, recovering, and purifying cannabidiolic acid (CBDA) salts from an organic solvent solution comprising a mixture of cannabinoids. The methods comprise solubilizing the mixture of cannabinoids in C5-C7 hydrocarbon solvents, adding thereto a selected amine to thereby precipitate a CBDA-amine salt therefrom, dissolving the recovered CBDA-amine salt in a selected solvent and then adding thereto a selected antisolvent to thereby recrystallize a purified CBDA-amine salt therefrom. The recrystallized CBDA-amine salt may be decarboxylated to form a mixture of cannabidiol (CBD) and amine. The CBD amine mixture may be acidified to separate the amine from CBD. Also disclosed are CBDA-amine salts produced with certain amines selected from groups of secondary amines, tertiary amines, diamines, amino alcohols, amino ethers, and highly basic amines.

A process for purification of phytosterols, said process comprising, a. providing a liquid mixture comprising a phytosterol, lower alcohol, wherein the lower alcohol is present in an amount of from 25 to 800% by weight, based on the amount of phytosterol; b. cooling the mixture to form phytosterol crystals, wherein the crystals are formed at a temperature of from of from 10° C. to 75° C., preferably 15° C. to 50° C., more preferably 20° C. to 45° C., even more preferably 25° C. to 35° C. c. separating the phytosterol crystals from the remainder of the mixture by filtration; d. subjecting the phytosterol crystals to washing with a solvent system comprising at least one polar aprotic solvent to obtain purified phytosterol; e. optionally repeating step (d); f. drying the washed phytosterol crystals; g. optionally melting and drying in molted state to remove traces of remaining solvent; and h. optionally subjecting to a particle-forming process to obtain solid sterol particles.

Compositions and methods are provided for producing crystalline forms of organic acids or salts or lactones thereof from an aqueous solution. More specifically, methods are provided for producing a crystalline form of a salt of mevalonic acid (also referred to as X-MVA) from an aqueous solution, comprising subjecting the aqueous solution comprising said X-MVA to a purification step to produce a purified solution and crystallizing said X-MVA from said purified solution by water solvent crystallization. Methods are also provided for producing mevalonolactone from an aqueous solution comprising X-MVA, comprising subjecting the aqueous solution comprising said X-MVA to cation exchange thereby converting said aqueous solution comprising X-MVA to an aqueous solution comprising mevalonolactone (MVL). Methods are also provided for producing mevalonolactone monohydrate crystals.