US4263052A — Production of fructose and useful by-products

Claim 1

Independent Claim 194 words

A process for obtaining solid fructose or aqueous fructose solutions of at least 85 weight-% fructose purity from a raw material containing a fructofuranoside-type compound, said fructofuranoside-type compound including glucose monomer, said process comprising the steps of: (a) hydrolyzing the fructofuranoside-type compound in said raw material to obtain an aqueous solution containing a hydrolyzate, said hydrolyzate comprising glucose and fructose monosaccharide hydrolysis products; (b) adding a calcium base to precipitate a mixture of calcium-sugar complexes, said mixture comprising at least about 85 weight-% calcium-fructose complex; (c) treating the calcium fructose complex obtained in step (b) with phosphoric acid in an aqueous reaction medium under temperature conditions sufficiently cool to avoid raising the temperature of said reaction medium, due to the reaction exotherm, above 40° C.; and maximizing the recovery of calcium phosphate precipitate by keeping the pH within the range of about 7 to about 9; (d) recovering from the reaction products of step (c) said calcium phosphate precipitate and an aqueous sugar solution, the solids of said solution comprising at least 85 weight-% fructose; (e) lowering the pH of said aqueous sugar solution to less than about 7 but greater than about 3.

Claim 2

Dependent Claim 194 words

A process for obtaining solid fructose or aqueous fructose solutions of at least 85 weight-% fructose purity from a raw material containing a fructofuranoside-type compound, said fructofuranoside-type compound including glucose monomer, said process comprising the steps of: (a) hydrolyzing the fructofuranoside-type compound in said raw material to obtain an aqueous solution containing a hydrolyzate, said hydrolyzate comprising glucose and fructose monosaccharide hydrolysis products; (b) adding a calcium base to precipitate a mixture of calcium-sugar complexes, said mixture comprising at least about 85 weight-% calcium-fructose complex; (c) treating the calcium fructose complex obtained in step (b) with phosphoric acid in an aqueous reaction medium under temperature conditions sufficiently cool to avoid raising the temperature of said reaction medium, due to the reaction exotherm, above 40° C.; and maximizing the recovery of calcium phosphate precipitate by keeping the pH within the range of about 7 to about 9; (d) recovering from the reaction products of step (c) said calcium phosphate precipitate and an aqueous sugar solution, the solids of said solution comprising at least 85 weight-% fructose; (e) lowering the pH of said aqueous sugar solution to less than about 7 but greater than about 3.

Claim 3

Dependent Claim 24 words

A process according to claim 1 wherein the calcium base is selected from the group consisting of aqueous calcium hydroxide and dry calcium oxide.

Claim 4

Dependent Claim 26 words

A process according to claim 1 wherein said step (e) is carried out by replacement of Ca ++ with H + with an ion exchange means.

Claim 5

Dependent Claim 18 words

A process according to claim 1 wherein the calcium phosphate precipitate comprises CaHPO 4 or a hydrate thereof.

Claim 6

Dependent Claim 31 words

A process according to claim 4 wherein the recovery of said precipitate is maximized by treating the calcium fructose complex with sufficient phosphoric acid to lower the pH to about 8.

Claim 7

Dependent Claim 23 words

A process according to claim 1 wherein said steps (b) and (c) are carried out at reaction medium temperatures below about 20° C.

Claim 8

Dependent Claim 12 words

A process according to claim 6 wherein said raw material comprises molasses.

Claim 9

Dependent Claim 22 words

A process according to claim 7 wherein said molasses contains raffinose which is also hydrolyzed to produce fructose in said step (a).

Claim 10

Dependent Claim 224 words

A process for obtaining solid fructose of at least about 90 weight-% purity from cane or beet molasses, comprising the steps of: (a) enzymatically hydrolyzing the sucrose in said molasses with invertase to obtain a treated molasses containing a hydrolyzate comprising at least one mole of fructose per mole of glucose; (b) adding an aqueous slurry comprising calcium hydroxide to said treated molasses to form a precipitated mixture of calcium-sugar complexes consisting essentially of at least about 90 weight-% calcium fructosate and less than about 10 weight-% calcium glucosate; (c) removing said precipitated mixture from the resulting fructose-depleted, glucose-enriched molasses to recover both said precipitated mixture and said fructose-depleted, glucose-enriched molasses; (d) blending said precipitated mixture with water to form an aqueous reaction medium; (e) adding sufficient phosphoric acid to said aqueous reaction medium to lower the pH thereof below 10 but above 7 and cooling said reaction medium to a temperature below about 20° C., thereby obtaining (1) a phosphate-containing precipitate comprising a calcium phosphate salt and entrapped color bodies and (2) an aqueous solution containing dissolved sugars comprising at least about 90 weight-% fructose and less than about 10 weight-% glucose; (f) separating said phosphate-containing precipitate from said aqueous solution containing dissolved sugars; and (g) further lowering the pH of said aqueous solution of dissolved sugars to below 7 but above 3.

Claim 11

Dependent Claim 224 words

A process for obtaining solid fructose of at least about 90 weight-% purity from cane or beet molasses, comprising the steps of: (a) enzymatically hydrolyzing the sucrose in said molasses with invertase to obtain a treated molasses containing a hydrolyzate comprising at least one mole of fructose per mole of glucose; (b) adding an aqueous slurry comprising calcium hydroxide to said treated molasses to form a precipitated mixture of calcium-sugar complexes consisting essentially of at least about 90 weight-% calcium fructosate and less than about 10 weight-% calcium glucosate; (c) removing said precipitated mixture from the resulting fructose-depleted, glucose-enriched molasses to recover both said precipitated mixture and said fructose-depleted, glucose-enriched molasses; (d) blending said precipitated mixture with water to form an aqueous reaction medium; (e) adding sufficient phosphoric acid to said aqueous reaction medium to lower the pH thereof below 10 but above 7 and cooling said reaction medium to a temperature below about 20° C., thereby obtaining (1) a phosphate-containing precipitate comprising a calcium phosphate salt and entrapped color bodies and (2) an aqueous solution containing dissolved sugars comprising at least about 90 weight-% fructose and less than about 10 weight-% glucose; (f) separating said phosphate-containing precipitate from said aqueous solution containing dissolved sugars; and (g) further lowering the pH of said aqueous solution of dissolved sugars to below 7 but above 3.

Claim 12

Dependent Claim 27 words

A process according to claim 9 comprising the additional step of recovering solid fructose of at least 90 weight-% purity from the aqueous solution of dissolved sugars.

Claim 13

Dependent Claim 17 words

A process according to claim 9 wherein said fructose-depleted, glucose-enriched molasses is acidified with a mineral acid.

Claim 14

Dependent Claim 33 words

A process according to claim 9 wherein said step (g) is carried out by replacement of Ca ++ with H + in said aqueous solution of dissolved sugars, using an ion exchange means.

Annuity Stage	Window Opens	Payment Deadline	Surcharge Period Until	Estimated Fee	Status
3.5 Years (Year 4)	1984-04-20	1984-10-20	1985-04-21	$2000.00	Window Closed / Lapsed
7.5 Years (Year 8)	1988-04-20	1988-10-20	1989-04-21	$3760.00	Window Closed / Lapsed
11.5 Years (Year 12)	1992-04-20	1992-10-20	1993-04-21	$7700.00	Window Closed / Lapsed

Production of fructose and useful by-products

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