CN101709336B - Method for preparing high-concentration fructose syrup - Google Patents
Method for preparing high-concentration fructose syrup Download PDFInfo
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Abstract
The invention relates to a method for preparing high-concentration fructose syrup by hydrolyzing sucrose, which comprises the following steps: (1) decolorizing a high-concentration sucrose solution by using acid with dosage accounting for 0.1-1.0% of the high-concentration sucrose solution as the hydrolyst while adding 0.05-0.8% of powder active carbon, and carrying out the reaction at 50-80 DEG C for 15-75 minutes to obtain the high-concentration fructose syrup of which the concentration is more than or equal to 45%, wherein the degree of hydrolysis is more than or equal to 97%; (2) and removing acid radicals and a small amount of pigments in the fructose syrup by using weak-base anion-exchange resin, and removing cations by using a strong-acid cation exchange resin, thereby adjusting the pH value of the fructose syrup. Compared with the exisiting method, the method of the invention is simple and convenient. Through deep research into the hydrolysis conditions, the invention provides the hydrolysis conditions capable of ensuring the hydrolysis effect and reducing the production cost. In addition, the invention carries out the hydrolysis and the decoloring synchronously, thereby ensuring the appearance of the syrup and simplifying the production technology. Then, the acid radicals and the cations in the syrup are removed by using anion and cation exchange resins, thereby obtaining the qualified high-concentration fructose syrup.
Description
Technical field
The invention belongs to the food chemical technology field, specifically, relate to a kind of preparation method of high-concentration fructose syrup.
Background technology
High fructose syrup is the Dian Fentang crystalline substance of being processed by plant amylum hydrolysis and isomerizing, has peculiar flavour, is a kind of important sweeting agent.Because its composition mainly is fructose and glucose; So be called " high fructose syrup ".High fructose syrup mainly is to be hydrolyzed into glucose by starch, part glucose is formed with the enzyme isomerizing again, and its fructose content is about 42%, and sugariness and sucrose are suitable.
Along with fossil energy supply in the world is becoming tight, be that the development of the corn deep processing industry of representative has caused a lot of disadvantageous effects with the W-Gum, particularly the grain security problem has caused the extensive concern of international community.Therefore except being the raw material production high fructose syrup with starch, be that the technological development of raw material production high fructose syrup has had considerable progress in recent years with using with sucrose.Along with the variation of consumer demand structure, along with the rising of high fructose syrup demand, these technology will come into one's own more.When the white sugar price is at low ebb, be that the raw material production high fructose syrup also can have bigger profit margin with sucrose.
The disaccharides that sucrose is made up of fructose and glucose, it is glycosides hydroxyl and the shrink product between the glycosides hydroxyl in the glucose molecule in the fructose molecule.Under certain conditions, sucrose ability and water hydrolytic reactions are degraded to a fructose and a glucose, have formed fructose and amount of glucose ratio and have been about 1: 1 high fructose syrup, and reaction equation is following:
Sucrose hydrolysis is produced high fructose syrup at present has three kinds of different catalytic way: acid-catalyzed hydrolysis method, enzymatic hydrolysis method and catalyzing cation exchange resin hydrolysis method.Enzyme catalysis technology is suitable for producing high conversion, and the production of the high fructose syrup of low concentration if require to improve syrup concentration, then can make the transformation efficiency of hydrolysis descend.The cost of catalyzing cation exchange resin hydrolysis method is than preceding two kinds of method height, and regeneration of resin is handled the link that has also increased operation.The advantage of acid-catalyzed hydrolysis sucrose is simple to operate, allows syrup that higher concentration is arranged, and is therefore generally adopted at home.Acid catalyzed process adds whole sucrose in the entry usually, and heating for dissolving adds acid and transforms, and reaction finishes the back with alkali neutralization refining step such as decolour again, processes the product of different transforming degrees.But, if product is without H
+, OH
-TREATMENT OF ION EXCHANGE RESINS is removed wherein impurity such as ash content and pigment, and then product can contain a certain amount of NaCl, influences the sweet taste mouthfeel of Nulomoline.Therefore, the existing technology of acid-catalyzed hydrolysis sucrose is comparatively complicated.
Therefore, be necessary to improve existing acid-catalyzed hydrolysis sucrose technology.
Summary of the invention
The purpose of this invention is to provide a kind of method of utilizing sucrose hydrolysis to prepare high-concentration fructose syrup.
The method of utilizing sucrose hydrolysis to prepare high-concentration fructose syrup of the present invention may further comprise the steps:
(1) adding consumption in the high concentration sucrose solution is 0.1%～1% (m/v of sucrose solution; Be meant that every 100ml sucrose solution adds 0.1～1g acid; The acid here is the acid after pure) acid hydrolysis, under 50 ℃～80 ℃ conditions, hydrolysis 15min～75min is after filter and obtain syrup;
(2) syrup is removed acid group and pigment through weakly basic anion exchange resin, removes positively charged ion through strongly acidic cationic exchange resin again, regulates syrup pH value.
Wherein, said step (1) also comprises, adds Powdered Activated Carbon when adding said diluted acid and decolours, and amount of activated is 0.05%～0.8% (m/v is meant every 100ml sucrose solution 0.05～0.8g gac) of sucrose solution.
In the step (1), said high concentration sucrose solution be mass and size concentration be 45%～60% (m/v, promptly 45～60g sucrose dissolved in hot water and be settled to 100mL) sucrose solution.
In the step (2), said acid is one or more of sulfuric acid, hydrochloric acid, phosphoric acid;
Among the present invention, specialize like nothing, the acid of being adopted is the consumption after pure with commercially available acid.
Through step (1), can obtain the high-concentration fructose syrup of concentration >=45%, sucrose hydrolysis rate >=97%.
In the step (2), said weakly basic anion exchange resin is a kind of of D301, D315, D318 weakly basic anion exchange resin, because the D315 resin can better remove the sulfate radical in the syrup, if sulfuric acid is selected in said acid, and then preferred D315 type resin;
With D315 anionite-exchange resin is example, and give-and-take conditions more excellent under the normal temperature condition are: input speed is twice column volume (2BV/h) per hour, and inlet amount is that (35～40BV), exchange finishes SO in the syrup of back to 35～40 times of column volumes
4 2-Concentration≤200ppm, other resin working conditions is consistent.
In the step (2), said strongly acidic cationic exchange resin is a kind of of 732,734 strongly acidic cationic exchange resins, preferred 732 type strongly acidic cationic exchange resins; Said pH value is 6～7.With 732 strongly acidic cationic exchange resins is example, and give-and-take conditions more excellent under the normal temperature condition are: (4～5BV/h), inlet amount is that (80～100BV), exchange finishes Ca in the syrup of back to 80～100 times of column volumes to input speed for 4～5 times of column volumes per hour
2+, Mg
2+Etc. cationic concentration≤10ppm, other resin working conditions is consistent.
Syrup passes through strongly acidic cationic exchange resin again after weakly basic anion exchange resin removes acid group, can pH regulator to 6～7 be removed Ca simultaneously basically
2+, Mg
2+Deng positively charged ion.
The processing of anion-cation exchange resin and regeneration: new anionite-exchange resin re-uses after answering alkali cleaning, pickling, alkali cleaning, washing; New Zeo-karb re-uses after answering pickling, alkali cleaning, pickling, washing.Anionite-exchange resin is with the regeneration of 4%～8% sodium hydroxide, and Zeo-karb is with 3～5% regeneration of hydrochloric acid, and the soda acid consumption is 3～5 times of resin volume, flow velocity 2～4BV/h.Washing is discharged regenerated liquid with the water of 1.25～1.5 times of resin volumes, uses the per hour water rinse resin of the speed of 8～10 times of resin volumes again, and is approaching neutral until anion-cation exchange resin flushing flow fluid.
Specifically, the described method of utilizing sucrose hydrolysis to prepare high-concentration fructose syrup may further comprise the steps:
(1) 60 ℃～80 ℃ hot water dissolving's sucrose are mixed with the sucrose solution that concentration is 45%～60% (m/v);
(2) with consumption be 0.1%～1.0% acid catalysis sucrose hydrolysis, add 0.05%～0.8% Powdered Activated Carbon simultaneously and decolour 50 ℃～100 ℃ of hydrolysis temperatures, time 15min-75min;
(3) high-concentration fructose syrup is removed acid group and pigment through weak anion resin, removes positively charged ion through strongly acidic cationic exchange resin again, and regulating syrup pH value is 6～7.
The principal feature that the present invention utilizes sucrose hydrolysis to prepare high-concentration fructose syrup is:
(1) inventor finds through the lower concentration acid catalysis sucrose hydrolysis reaction kinetics in the research sucrose solution; In certain threshold concentration scope; Sugar syrup hydrolysed speed strengthens with the rising of sucrose concentration; Select 45%～60% syrup concentration, both guaranteed hydrolysis effect, reduce production costs again;
(2) hydrolysis and decolorization are carried out synchronously, for subsequent step provides outward appearance qualified syrup, have simplified production technique;
(3) select (acid of consumption 0.1%～1.0% of relatively mild hydrolysising condition; 50 ℃～80 ℃ of temperature; Time 15min～75min); Prevent that under low excessively pH value, long hydrolysis time or hot conditions, hydrolysate (fructose and glucose) continues degraded, causes the increase of non-sugared impurity and the generation of excessive pigment;
(4) adopting weakly basic anion exchange resin to remove acid group earlier, is example with the D315 resin, and exchange finishes SO in the syrup of back
4 2-Concentration≤200ppm; And then remove Ca with strongly acidic cationic exchange resin
2+, Mg
2+Deng positively charged ion, regulate pH to 6～7 simultaneously, prepare qualified high-concentration fructose syrup.
Compare with existing method; The present invention adopts the acid catalysis sucrose hydrolysis of lower concentration in the sucrose solution; Hydrolysis and decolouring are carried out synchronously; Adopt weakly basic anion exchange resin to remove acid ion, obtain qualified syrup, simplified technical process again with after the strongly acidic cationic exchange resin adjusting syrup pH value.Method of the present invention is simple and convenient, through having furtherd investigate hydrolysising condition, provided and both guaranteed hydrolysis effect, the hydrolysising condition that reduces production costs again, and with hydrolysis with the decolouring carry out synchronously, both guaranteed syrupy outward appearance, simplified production technique again; Adopt anion-cation exchange resin to remove acid group and positively charged ion in the syrup subsequently, prepare qualified high-concentration fructose syrup product.
Embodiment
Following examples are used to explain the present invention, but are not used for limiting scope of the present invention.Specialize like nothing, used strongly acidic cationic exchange resin and weakly basic anion exchange resin are all from commercial.
Embodiment 1
Sucrose solution 500mL (sucrose concentration 48.73%; 420nm measures transmittance 45.4%); Add sucrose solution 0.2% (reaction 30min is hydrolyzed under 75 ℃ of conditions for m/v, the Powdered Activated Carbon of vitriol oil 1.02g) (pure) and 0.05% (m/v); The sucrose hydrolysis rate is 99.32% (syrup transmittance 76.9%, fructose content 49.96%).
Syrup is through D315 type anionite-exchange resin, and input speed is 2BV/h, and inlet amount is 35BV, removes acid group and small amount of coloring matter, detects the SO in the syrup
4 2-Concentration, SO
4 2-≤100ppm; Through 732 Zeo-karbs, input speed is 4BV/h again, and inlet amount is 80BV, regulates pH value to 6.0～6.5, Ca
2+, Mg
2+Concentration is lower than 10ppm, obtains concentration and be 50.74% high fructose syrup.
Embodiment 2
Sucrose solution 1000mL (sucrose concentration 59.32%; 420nm measures transmittance 44.7%); Add the vitriol oil (pure) of 0.5% (5.1g) and 0.8% Powdered Activated Carbon; Under 50 ℃ of conditions, be hydrolyzed, hydrolysis 15,30 respectively, 45min, the percent hydrolysis of sucrose is respectively 97.02%, 99.78%, 99.84%.
Syrup is through D301 type anionite-exchange resin, and input speed is 2BV/h, and inlet amount is 40BV, removes acid group and small amount of coloring matter, detects the SO in the syrup
4 2-Concentration, SO
4 2-≤100ppm; Through 734 Zeo-karbs, input speed is 5BV/h again, and inlet amount is 80BV, regulates pH value to 6.5～6.8, Ca
2+, Mg
2+Concentration is lower than 10ppm, obtains concentration and be 61.97% high fructose syrup.
Embodiment 3
Sucrose solution 20L (sucrose concentration 51.26%, transmittance 43.5%, Ca
2+, Mg
2+Concentration is 64ppm, 11ppm respectively), add the vitriol oil (pure) of 0.5% (102g) and 0.4% Powdered Activated Carbon, under 60 ℃ of conditions, be hydrolyzed, hydrolysis 60min, the percent hydrolysis of sucrose are 99.47%.
Syrup is through the D315 type anionite-exchange resin of 900mL, and input speed is 2BV/h, and inlet amount is 38BV, and through 732 Zeo-karbs of 200mL, input speed is 5BV/h again, and inlet amount is 100BV, regulates pH value to 6.7～7, obtains high fructose syrup.
The concentration of high fructose syrup is 53.06%, and pH is 6.8, SO
4 2-Concentration≤125ppm, Ca
2+, Mg
2+Concentration is lower than 5ppm, transmittance 91.7%.
Embodiment 4
Sucrose solution 1000mL (sucrose concentration 51.26%, transmittance 43.5%, Ca
2+, Mg
2+Concentration is 64ppm, 11ppm respectively), add 1% (50g, mass concentration: hydrochloric acid 20%) (pure back 10gHCl), add 0.1% Powdered Activated Carbon simultaneously, under 80 ℃ of conditions, be hydrolyzed, hydrolysis 75min, the percent hydrolysis of sucrose are 98.64%.
Through D318 type resin anion(R.A) and 732 resin cation(R.C.)s, input speed is respectively 2BV/h, 4BV/h to syrup respectively, and inlet amount is respectively 35BV, 90BV, obtains the high fructose syrup product.
The concentration of high fructose syrup is 52.63%, and pH is 6.6, Cl
-Concentration is 58ppm, Ca
2+, Mg
2+Concentration is lower than 1ppm, transmittance 87.9%.
Though, the present invention has been done detailed description in the preceding text with general explanation and specific embodiments, on basis of the present invention, can to some modifications of do or improvement, this will be apparent to those skilled in the art.Therefore, these modifications or the improvement on the basis of not departing from spirit of the present invention, made all belong to the scope that requirement of the present invention is protected.
Claims (4)
1. method of utilizing sucrose hydrolysis to prepare high-concentration fructose syrup may further comprise the steps:
(1) add 0.1%～1% the acid hydrolysis that quality is the sucrose solution volume in the high concentration sucrose solution, under 50 ℃～80 ℃ conditions, hydrolysis 15min～75min is after filter and obtain syrup;
(2) syrup is removed acid group and pigment through weakly basic anion exchange resin, removes positively charged ion through strongly acidic cationic exchange resin again, and regulates syrup pH value;
In the step (1), said high concentration sucrose solution is that mass and size concentration is 45%～60% sucrose solution;
In the step (2), said acid is one or more in sulfuric acid, hydrochloric acid, the phosphoric acid; Said weakly basic anion exchange resin is a kind of in D301, D315, the D318 type weakly basic anion exchange resin; Said strongly acidic cationic exchange resin is a kind of in 732, the 734 type strongly acidic cationic exchange resins; Input speed through weakly basic anion exchange resin is twice column volume per hour, and inlet amount is 35～40 times of column volumes; Input speed through strongly acidic cationic exchange resin is 4～5 times of column volumes per hour, and inlet amount is 80～100 times of column volumes.
2. the method for claim 1 is characterized in that, said step (1) also comprises, adds Powdered Activated Carbon when adding said acid and decolours, and the consumption of gac is that quality is 0.05%～0.8% of a sucrose solution volume.
3. the method for claim 1 is characterized in that, said acid is sulfuric acid, and said weakly basic anion exchange resin is a D315 type weakly basic anion exchange resin.
4. the method for claim 1 is characterized in that, said strongly acidic cationic exchange resin is 732 type strongly acidic cationic exchange resins.
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| CN2009102595877A CN101709336B (en) | 2009-12-21 | 2009-12-21 | Method for preparing high-concentration fructose syrup |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102808045A (en) * | 2012-08-02 | 2012-12-05 | 鲜活果汁工业（昆山）有限公司 | Method for removing browning precursors of high fructose syrup |
| CN103385342A (en) * | 2013-07-15 | 2013-11-13 | 佐源集团有限公司 | Rock candy syrup production technology |
| 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 |
| CN103695568B (en) * | 2013-12-12 | 2016-01-06 | 朱辉 | A kind of syrup |
| CN105131129B (en) * | 2015-10-12 | 2017-12-15 | 长春工业大学 | A kind of preparation method of nano-cellulose |
| CN107455732B (en) * | 2017-07-14 | 2021-02-02 | 西王药业有限公司 | Method for reducing consumption of active carbon in high fructose corn syrup production process |
| CN107373072A (en) * | 2017-08-10 | 2017-11-24 | 江西兴鼎科技有限公司 | A kind of feed addictive and preparation method thereof |
| CN107495084B (en) * | 2017-09-08 | 2020-08-18 | 宁波大学 | Method for removing isovaleraldehyde in F55 high fructose corn syrup |
| CN108251570A (en) * | 2018-01-13 | 2018-07-06 | 施越 | A kind of production method of fructose syrup |
| CN109136304A (en) * | 2018-09-18 | 2019-01-04 | 安徽源森生物科技有限公司 | A kind of utilization, which is cracked rice, produces the processing technology of fructose syrup |
| CN110938099A (en) * | 2019-12-23 | 2020-03-31 | 南通市常海食品添加剂有限公司 | Method for removing acetate in sucralose |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1048233A (en) * | 1989-06-21 | 1991-01-02 | 中国科学院广州化学研究所 | Fructose glucose syrup made by sucrose with cation resin hydrolyzing |
| US6709527B1 (en) * | 1999-04-07 | 2004-03-23 | Ufion (Pty) Limited | Treatment of sugar juice |
-
2009
- 2009-12-21 CN CN2009102595877A patent/CN101709336B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1048233A (en) * | 1989-06-21 | 1991-01-02 | 中国科学院广州化学研究所 | Fructose glucose syrup made by sucrose with cation resin hydrolyzing |
| US6709527B1 (en) * | 1999-04-07 | 2004-03-23 | Ufion (Pty) Limited | Treatment of sugar juice |
Non-Patent Citations (2)
| Title |
|---|
| Eduardo A. Borges da Silva.Analysis of the high-fructose syrup production using reactive SMB technology.《Chemical Engineering Journal》.2006,第118卷第167-181页. * |
| JP平4-131090A 1992.05.01 |
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