CN1324956A - Prepn. of lactulose - Google Patents
Prepn. of lactulose Download PDFInfo
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- CN1324956A CN1324956A CN 01113315 CN01113315A CN1324956A CN 1324956 A CN1324956 A CN 1324956A CN 01113315 CN01113315 CN 01113315 CN 01113315 A CN01113315 A CN 01113315A CN 1324956 A CN1324956 A CN 1324956A
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- lactulose
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Abstract
The preparation method of lactulose is characterized by that it uses easily available whey as raw material, utilizes catalytic reaction to isomerize the glucosyl group of lactose molecular interior in the whey into fructose so as to synthesize a lactulose with health-care action, and its purity is up to above 94%. It contains no artificial synthetic matter, can be used for preparing health-care products, such as health-care milk powder, sweets and beverage with good taste. Said invention is moderate in technological condition, and is easy to implement scale-production.
Description
Technical field
The present invention relates to a kind of preparation method of lactulose.
Background technology
Lactulose has another name called isomerizing lactose, is that a kind of proterties is faint yellow, and heavy-gravity liquid is soluble in water.Its molecular formula is C
11H
22O
11, molecular weight is 342.30.
Lactulose is a kind of disaccharide, and the glucose in the lactose molecule is replaced by fructose, is lactulose, and its sugariness is a little more than lactose.There is not lactulose in occurring in nature, and it belongs to the disaccharide of synthetic, but all contains a spot of lactulose in milk that boils and condensed milk.
Lactulose is not only a kind of good sweeting agent, is good for the stomach, ease constipation, physiological function such as prevents from just to secrete but also have, and also can be used as the functional additive of dairy products, beverage, baby and old people food, also can be made into health promoting beverage for directly taking.In addition, lactulose has obvious curative effects to treatment hepatic diseases and encephalopathy, therefore this is a kind ofly to have medicinal and health care is worth, and the healthcare products of new generation of great economic benefit are arranged again simultaneously, for its preparation research and the Application and Development focus that become people's research.
Along with fast development of social economy, the improving constantly of standard of living, people's health care consciousness strengthens gradually, therefore, researchs and develops the preparation method of new lactulose, to satisfy the needs of people's daily life, will have crucial meaning.
Summary of the invention
The purpose of this invention is to provide a kind of is raw material with the whey that is easy to get, by catalyzed reaction glucosyl group isomery in the lactose molecule in the whey is become fructose, thereby the preparation method of synthetic a kind of lactulose with health role is to satisfy the needs of people's daily life.
Design of the present invention is such:
With the pair material whey of milk after refining deep processing is raw material, and the lactose under weak basic condition in the isoversion whey becomes lactulose, again through concentrate, crystallization, separation and make lactulose.
Said whey is meant the colloidal particle process cohesion in the animals and plants milk, and removes the clear liquid that is obtained behind the colloidal particle of cohesion.The said whey of the present invention refers to the junket unit isolated clear liquid after cohesion and press filtration in the milk, yellow-green colour slightly, solid content is 5～7%, mainly is lactose, and contain certain protein, minerals and vitamins, be the pair material of milk after refining deep processing.
Lactose in the pair material whey of milk after refining deep processing is dissolved in the hot water, slowly drips alkaline solution then, keep boiling state to carry out isomerization reaction.When reaction finishes postcooling also with the pH value of sour conditioned reaction liquid, use decolorizing with activated carbon then, destainer is crossed anion-cation exchange resin and is carried out desalination, gets the effluent liquid of certain pH value.Then effluent liquid is carried out vacuum concentration, cooling, crystallization, separate lactulose.
The concrete method of the present invention in turn includes the following steps:
(1) preparation raw material liquid: getting whey, to be mixed with the lactose concentration expressed in percentage by weight be 3～7% solution A, and concentration is the alkaline solution B of 0.1～1.0mol/L, and is stand-by;
Said alkali is a kind of and composition thereof in sodium hydroxide, potassium hydroxide, yellow soda ash, salt of wormwood, sodium bicarbonate or the saleratus;
(2) isomerization of lactose: lactose is dissolved fully the heating of A solution, preferably boiled 10～60 minutes, slowly drip B solution then, the pH value of reaction solution is controlled between 9.5～12.0, keep boiling state that reaction is transformed fully;
(3) reaction product decolouring: reaction solution is cooled to 65-75 ℃,, uses decolorizing with activated carbon then with pH to 4～5 of acid solution conditioned reaction liquid;
According to optimized technical scheme of the present invention, can decolour with powdered activated carbon earlier, and then use the granule activated carbon secondary decolourization;
Said acid is a kind of and composition thereof in hydrochloric acid, sulfuric acid or the phosphoric acid;
(4) destainer desalination: destainer is carried out desalination by anion and cation exchange resin, can pass through Zeo-karb earlier, get the pH value less than 4.0 effluent liquid, this effluent liquid is again through anionite-exchange resin, gets the pH value greater than 6.0 effluent liquid;
Said Zeo-karb can preferably adopt a kind of in 732 type Zeo-karbs, strongly acidic styrene's Zeo-karb, SA-149 carboxyl type cation exchange resin or the huge legendary turtle mould assembly amine carboxyl Zeo-karb, said anionite-exchange resin can preferably adopt a kind of in 717 type anionite-exchange resin, D202 strong basicity quaternary ammonium II type anionite-exchange resin, weakly basic styrene type anion exchange resin or the weakly alkaline epoxy type anion exchange resin;
(5) demineralised liquid concentrates: adopt conventional method that above-mentioned demineralised liquid is concentrated post crystallization, can obtain the said lactulose of the present invention.
Concentration process preferably adopts following method: the reaction solution of above-mentioned collection is carried out vacuum concentration, it is 65～70% that effluent liquid is concentrated into lactulose concentration, concentrated solution is emitted while hot then, non-shock chilling is to room temperature, again with ice bath to 4-10 ℃, treat to carry out solid-liquid separation after lactulose forms crystallization, promptly get product lactulose of the present invention.
Full glycan analysis method with routine is analyzed above-mentioned lactulose, and its purity reaches more than 94%.
By above-mentioned disclosed technical scheme as seen, the lactulose that adopts method of the present invention to obtain, raw material are taken from crude substance fully, do not contain the material of synthetic, are used to prepare healthcare products, as health-care milk powder, candy and beverage, good mouthfeel.Processing condition gentleness of the present invention is easy to large-scale production.
Embodiment
By the following examples the concrete embodiment of the present invention is narrated, but embodiment does not limit protection scope of the present invention.
Embodiment 1
Preparation contain lactose concn be 4% whey solution 1000ml in the 2000ml beaker, the NaOH solution for standby of cofabrication 0.2mol/L.Under agitation lactose aqueous solution is slowly heated and make it dissolving fully, and boiled 30 minutes, slowly drip NaOH solution then, make the pH value of reaction solution be controlled at 11.5, and maintenance boiling state 90 minutes, catalytic conversion reaction finishes.Reaction solution is naturally cooled to about 70 ℃, and, with powdered activated carbon decolouring, use the granule activated carbon secondary decolourization more then with the pH to 4.0 of dilution heat of sulfuric acid conditioned reaction liquid.Destainer is crossed anion-cation exchange resin and is carried out desalination, and Zeo-karb is 732 types, gets the pH value less than 4.0 effluent liquid, and this effluent liquid is again through anionite-exchange resin 717 types, gets the pH value greater than 6.0 effluent liquid.Above-mentioned reaction solution is carried out vacuum concentration to the concentration of lactulose reach 69%.Concentrated solution is emitted while hot, naturally cools to room temperature, is cooled to about 5 ℃ with frozen water again, and then the lactulose crystallization is separated out, and carries out solid-liquid separation subsequently and gets lactulose 35 grams, and its purity is 95%.
Embodiment 2
Preparation contain lactose concn be 6% whey solution 1000ml in the 2000ml beaker, the KOH solution for standby of cofabrication 0.8mol/L.Under agitation lactose aqueous solution is slowly heated and make it dissolving fully, and boiled 45 minutes, slowly drip KOH solution then, make the pH value of reaction solution be controlled at 10.5, maintenance boiling state 120 minutes, catalytic conversion reaction finishes.Reaction solution is naturally cooled to about 65 ℃, and, with powdered activated carbon decolouring, use the granule activated carbon secondary decolourization more then with the pH to 4.0 of dilute hydrochloric acid solution conditioned reaction liquid.Destainer is crossed anion-cation exchange resin and is carried out desalination, and Zeo-karb is a SA-149 carboxyl type, gets the pH value less than 4.0 effluent liquid, and this effluent liquid is again through anionite-exchange resin D202 strong basicity quaternary ammonium II type, gets the pH value greater than 6.0 effluent liquid.Above-mentioned reaction solution is carried out vacuum concentration to the concentration of lactulose reach 65%.Concentrated solution is emitted while hot, naturally cools to room temperature, is cooled to about 5 ℃ with frozen water again, and then the lactulose crystallization is separated out, and carries out solid-liquid separation subsequently and gets lactulose 52 grams, and its purity is 95.3%.
Embodiment 3
Adopt the method identical with embodiment 1, replace NaOH with NaOH and the KOH mixing solutions (1: 1, weight ratio) of 0.2mol/L, can obtain lactulose 34.8 at last and restrain, its purity is 95.2%.
Claims (10)
1. the preparation method of a lactulose is characterized in that, this method comprises the steps:
(1) lactose is wherein dissolved the whey solution heating, add alkaline solution then, the pH value of reaction solution is controlled between 9.5～12.0, kept boiling state 80～120 minutes;
(2) reaction solution is cooled to 65-75 ℃,, uses decolorizing with activated carbon then with pH to 4～5 of acid solution conditioned reaction liquid;
(3) with destainer earlier through Zeo-karb, get the pH value less than 4.0 effluent liquid, this effluent liquid is again through anionite-exchange resin, gets the pH value greater than 6.0 effluent liquid;
(4) adopt conventional method that above-mentioned demineralised liquid is concentrated post crystallization, can obtain the said lactulose of the present invention.
2. the method for claim 1 is characterized in that, it is 3～7% solution that whey is mixed with the lactose concentration expressed in percentage by weight, and alkaline concentration is 0.1～1.0mol/L;
Said alkali is a kind of and composition thereof in sodium hydroxide, potassium hydroxide, yellow soda ash, salt of wormwood, sodium bicarbonate or the saleratus.
3. method as claimed in claim 1 or 2 is characterized in that, said acid is a kind of and composition thereof in hydrochloric acid, sulfuric acid or the phosphoric acid.
4. method as claimed in claim 1 or 2 is characterized in that, lactose is wherein dissolved the whey solution heating, boils 10～60 minutes again.
5. method as claimed in claim 1 or 2 is characterized in that, earlier with powdered activated carbon decolouring, and then uses the granule activated carbon secondary decolourization.
6. method as claimed in claim 1 or 2, it is characterized in that, said Zeo-karb is a kind of in 732 type Zeo-karbs, strongly acidic styrene's Zeo-karb, SA-149 carboxyl type cation exchange resin or the huge legendary turtle mould assembly amine carboxyl Zeo-karb, and said anionite-exchange resin is a kind of in 717 type anionite-exchange resin, D202 strong basicity quaternary ammonium II type anionite-exchange resin, weakly basic styrene type anion exchange resin or the weakly alkaline epoxy type anion exchange resin.
7. method as claimed in claim 1 or 2, it is characterized in that, concentration process adopts following method: the reaction solution of collecting is carried out vacuum concentration, it is 65～70% that effluent liquid is concentrated into lactulose concentration, concentrated solution is emitted while hot then, the cooling, again with ice bath to 4-10 ℃, solid-liquid separation promptly gets lactulose.
8. method as claimed in claim 4, it is characterized in that, concentration process adopts following method: the reaction solution of collecting is carried out vacuum concentration, it is 65～70% that effluent liquid is concentrated into lactulose concentration, concentrated solution is emitted while hot then, the cooling, again with ice bath to 4-10 ℃, solid-liquid separation promptly gets lactulose.
9. method as claimed in claim 5, it is characterized in that, concentration process adopts following method: the reaction solution of collecting is carried out vacuum concentration, it is 65～70% that effluent liquid is concentrated into lactulose concentration, concentrated solution is emitted while hot then, the cooling, again with ice bath to 4-10 ℃, solid-liquid separation promptly gets lactulose.
10. method as claimed in claim 6, it is characterized in that, concentration process adopts following method: the reaction solution of collecting is carried out vacuum concentration, it is 65～70% that effluent liquid is concentrated into lactulose concentration, concentrated solution is emitted while hot then, the cooling, again with ice bath to 4-10 ℃, solid-liquid separation promptly gets lactulose.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01113315 CN1324956A (en) | 2001-07-10 | 2001-07-10 | Prepn. of lactulose |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01113315 CN1324956A (en) | 2001-07-10 | 2001-07-10 | Prepn. of lactulose |
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| CN1324956A true CN1324956A (en) | 2001-12-05 |
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| CN 01113315 Pending CN1324956A (en) | 2001-07-10 | 2001-07-10 | Prepn. of lactulose |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101182563B (en) * | 2007-11-02 | 2011-06-22 | 江南大学 | Method for preparing lactulose by co-immobilized lactose enzyme and glucose isomerase |
| CN103540690A (en) * | 2013-09-29 | 2014-01-29 | 山东西王糖业有限公司 | PH regulation method in high fructose corn syrup production process |
| CN103842349A (en) * | 2011-09-29 | 2014-06-04 | 韩国生产技术研究院 | Method for producing 5- hydroxymethyl-2- furfural or alkyl ether derivatives thereof using an ion exchange resin in the presence of an organic solvent |
| CN108264528A (en) * | 2016-12-31 | 2018-07-10 | 烟台大学 | A kind of method that lactose is isolated and purified from whey |
| CN108260800A (en) * | 2016-12-31 | 2018-07-10 | 烟台大学 | The technique for preparing Lactulose liquid using whey |
-
2001
- 2001-07-10 CN CN 01113315 patent/CN1324956A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101182563B (en) * | 2007-11-02 | 2011-06-22 | 江南大学 | Method for preparing lactulose by co-immobilized lactose enzyme and glucose isomerase |
| CN103842349A (en) * | 2011-09-29 | 2014-06-04 | 韩国生产技术研究院 | Method for producing 5- hydroxymethyl-2- furfural or alkyl ether derivatives thereof using an ion exchange resin in the presence of an organic solvent |
| CN103842349B (en) * | 2011-09-29 | 2015-09-30 | 韩国生产技术研究院 | In presence of organic solvent, spent ion exchange resin is made to produce the method for 5-hydroxymethyl-furfural or its alkyl ether derivative |
| CN103540690A (en) * | 2013-09-29 | 2014-01-29 | 山东西王糖业有限公司 | PH regulation method in high fructose corn syrup production process |
| CN103540690B (en) * | 2013-09-29 | 2015-09-02 | 山东西王糖业有限公司 | PH regulator method in high fructose syrup production process |
| CN108264528A (en) * | 2016-12-31 | 2018-07-10 | 烟台大学 | A kind of method that lactose is isolated and purified from whey |
| CN108260800A (en) * | 2016-12-31 | 2018-07-10 | 烟台大学 | The technique for preparing Lactulose liquid using whey |
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