CN1048233A - Fructose glucose syrup made by sucrose with cation resin hydrolyzing - Google Patents
Fructose glucose syrup made by sucrose with cation resin hydrolyzing Download PDFInfo
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- CN1048233A CN1048233A CN 89104363 CN89104363A CN1048233A CN 1048233 A CN1048233 A CN 1048233A CN 89104363 CN89104363 CN 89104363 CN 89104363 A CN89104363 A CN 89104363A CN 1048233 A CN1048233 A CN 1048233A
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- sucrose
- resin
- hydrolysis
- type
- fructose
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- 229930006000 Sucrose Natural products 0.000 title claims abstract description 76
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 title claims abstract description 76
- 239000011347 resin Substances 0.000 title claims abstract description 73
- 229920005989 resin Polymers 0.000 title claims abstract description 73
- 239000005720 sucrose Substances 0.000 title claims abstract description 70
- 239000006188 syrup Substances 0.000 title abstract description 22
- 235000020357 syrup Nutrition 0.000 title abstract description 22
- 150000001768 cations Chemical class 0.000 title abstract description 10
- PJVXUVWGSCCGHT-ZPYZYFCMSA-N (2r,3s,4r,5r)-2,3,4,5,6-pentahydroxyhexanal;(3s,4r,5r)-1,3,4,5,6-pentahydroxyhexan-2-one Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O.OC[C@@H](O)[C@@H](O)[C@H](O)C(=O)CO PJVXUVWGSCCGHT-ZPYZYFCMSA-N 0.000 title abstract description 4
- 230000003301 hydrolyzing effect Effects 0.000 title description 7
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 68
- 230000007062 hydrolysis Effects 0.000 claims abstract description 66
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 34
- 235000021433 fructose syrup Nutrition 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 26
- 229930091371 Fructose Natural products 0.000 claims abstract description 25
- 239000005715 Fructose Substances 0.000 claims abstract description 25
- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 claims abstract description 25
- 239000008103 glucose Substances 0.000 claims abstract description 17
- 150000002500 ions Chemical class 0.000 claims abstract description 15
- 239000002253 acid Substances 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 11
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims abstract description 10
- 230000002378 acidificating effect Effects 0.000 claims abstract description 9
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 11
- 238000006555 catalytic reaction Methods 0.000 claims description 11
- 150000001450 anions Chemical class 0.000 claims description 9
- 238000005342 ion exchange Methods 0.000 claims description 9
- 229910021536 Zeolite Inorganic materials 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 5
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 5
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 claims description 5
- 239000010457 zeolite Substances 0.000 claims description 5
- 239000003729 cation exchange resin Substances 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 3
- 229920003023 plastic Polymers 0.000 claims 1
- 239000004033 plastic Substances 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 102000004190 Enzymes Human genes 0.000 abstract description 2
- 108090000790 Enzymes Proteins 0.000 abstract description 2
- 238000005903 acid hydrolysis reaction Methods 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000011973 solid acid Substances 0.000 abstract description 2
- 238000004040 coloring Methods 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- LPQOADBMXVRBNX-UHFFFAOYSA-N ac1ldcw0 Chemical compound Cl.C1CN(C)CCN1C1=C(F)C=C2C(=O)C(C(O)=O)=CN3CCSC1=C32 LPQOADBMXVRBNX-UHFFFAOYSA-N 0.000 description 7
- 239000011521 glass Substances 0.000 description 7
- 239000003456 ion exchange resin Substances 0.000 description 7
- 229920003303 ion-exchange polymer Polymers 0.000 description 7
- 125000002091 cationic group Chemical group 0.000 description 5
- 230000008929 regeneration Effects 0.000 description 5
- 238000011069 regeneration method Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- NOEGNKMFWQHSLB-UHFFFAOYSA-N 5-hydroxymethylfurfural Chemical compound OCC1=CC=C(C=O)O1 NOEGNKMFWQHSLB-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000003957 anion exchange resin Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- RJGBSYZFOCAGQY-UHFFFAOYSA-N hydroxymethylfurfural Natural products COC1=CC=C(C=O)O1 RJGBSYZFOCAGQY-UHFFFAOYSA-N 0.000 description 3
- 239000000049 pigment Substances 0.000 description 3
- 230000003245 working effect Effects 0.000 description 3
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 229910001424 calcium ion Inorganic materials 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 229910052680 mordenite Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 1
- OAUXSBFJNWOKFV-UHFFFAOYSA-N [C].OS(O)(=O)=O Chemical compound [C].OS(O)(=O)=O OAUXSBFJNWOKFV-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004061 bleaching Methods 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 235000014171 carbonated beverage Nutrition 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010010 raising Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- -1 this Chemical compound 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- Saccharide Compounds (AREA)
Abstract
The present invention is a kind of method with fructose glucose syrup made by sucrose.Sucrose hydrolysis becomes fructose and glucose, and liquid acid is arranged, enzyme and solid acid hydrolysis method etc.It is catalyzer that the present invention selects the high strong acidic ion resin of catalytic activity for use, under chosen temperature, sucrose hydrolysis is become fructose and glucose.According to high fructose syrup requirement of different nature, can select cation seperation column or positive and negative ion column bonded Different Preparation route for use.The high fructose syrup colour that this law is produced is low, and during the sucrose all-hydrolytic, fructose and glucose respectively account for 50%, and sugariness is higher than the high fructose syrup that the acid solution method is produced.Advantages such as this law has easy to operate, and equipment is simple, and energy expenditure is low.
Description
The present invention is the method that a kind of sucrose hydrolysis prepares high fructose syrup.
High fructose syrup, the syrup of forming by fructose and glucose.It can be hydrolyzed into glucose by starch, part glucose is formed with the enzyme isomerization again, and its fructose content is about 42%, and sugariness and sucrose are suitable.Desire to obtain the higher high fructose syrup of fructose content, must separate fructose.Usually, fructose content is higher than 55% syrup, claims high fructose high fructose syrup.This respect has many patents granted, as U.S. Pat 3,684, and 574 and US3,690,948 etc.Another kind of method of producing high fructose syrup is that sucrose hydrolysis is formed, and this method is simple and convenient, is particularly suited for the use with sugared family.
Sucrose hydrolysis is used hydrochloric acid usually, and sulfuric acid and citric acid etc. are the strongest with the hydrolysis ability of hydrochloric acid.Use the acid solution sucrose hydrolysis, need comparatively high temps and long period, as use hydrochloric acid hydrolysis,, need 1～2 hour, 97～103 ℃ of need more than 20 minute at 70～80 ℃.Under such hydrolysising condition, the monose that sucrose hydrolysis generated, especially fructose can be degraded, and generate coloring matter, make the syrup color burn, also reduce the content of fructose in the syrup, thereby reduce the sugariness of high fructose syrup.Sucrose hydrolysis, the fructose and the glucose of generation equivalent, the sugariness of cause and effect sugar is 1.5 times of sucrose, and the sugariness of glucose is 0.8 times of sucrose, like this, when sucrose hydrolysis becomes fructose and glucose, if monose does not destroy, then its sugariness is 1.15 times of sucrose, usually, the high fructose syrup of acid solution method sucrose hydrolysis gained, its fructose content about 42%, sugariness is only suitable with sucrose, and needs bleaching process can prepare qualified high fructose syrup product.
The better method for preparing high fructose syrup with sucrose is to make catalyzer with storng-acid cation exchange resin, and higher because of its catalyst activity, the temperature of sucrose hydrolysis is lower, and the time is shorter.Public clear 46-15684 of the patent of this respect such as spy and open 49-134852 etc.Yet the hydrolysis temperature that existing relevant patent is controlled is still more than 55 ℃.More than the temperature spot, sucrose is at H at this
+During type resin column internal reaction, degraded still can take place and makes syrup painted in the monose that is generated, especially fructose, and this not only adds decolouring burden of weight resin, shortens regeneration period and work-ing life, and the high fructose syrup sugariness of generation is reduced.People such as E.Berghofer think and use H
+During the type sucrose with cation resin hydrolyzing, the fructose and the glucose of generation are all degraded, but G.Siegers etc. are in certain reaction times, and under differing temps, sucrose is at H
+Hydrolysis is done to test and is drawn on the type strong acidic ion resin post, and when column temperature surpassed 40 ℃, the monose that sucrose hydrolysis becomes just can generate coloring matters such as hydroxymethylfurfural, advocated that sucrose hydrolysis should be controlled at 40 ℃ below the column temperature.In fact, during sucrose hydrolysis, the generation of coloring matter is not only relevant with temperature, and relevant with hydrolysis time, when hydrolysis temperature raise, the hydrolysis rate of sucrose was accelerated, thereby hydrolysis time is just short, thereby makes sucrose hydrolysis and the temperature of coloring matters such as unlikely generation hydroxymethylfurfural also can improve.Cross the decline that lowland reduction hydrolysis temperature must cause productivity for avoiding generating coloring matter, can not bring into play the proper efficiency of catalyzer fully.
Existing other weak points of using cation exchange resin catalyst sucrose hydrolysis fructose glucose syrup made, be the arrangement and the cooperation aspect of ion exchange column, fail to accomplish flexible and changeable, can not give full play to each self-applying, to be suitable for the syrupy production requirement of different properties.
The objective of the invention is to seek to be suitable for the requirement of different properties high fructose syrup, technology is simple, consume energy low, efficient is high, monose does not have degraded, the syrup sugariness is higher than the high fructose syrup production method of sucrose.
The present invention is achieved like this, and at first, sucrose is at H
+The hydrolysis reaction of type strong acidic ion resin post is controlled at 25～54 ℃, preferred 40～52 ℃.Desire is produced sugariness with sucrose and is higher than sucrose and the lower or colourless high fructose syrup of colour, and key is to protect fructose.Experiment shows, at 50 ℃ below the column temperature, and the high fructose syrup of sucrose hydrolysis gained, its specific rotatory power (α)
20 DBe-20 °, illustrate that wherein fructose and glucose respectively account for 50%.At this below temperature spot, sucrose is in resin column during hydrolysis, as long as in time discharge, syrup non-coloring phenomenon then illustrates that fructose and glucose can not give birth to degraded, does not produce coloring matter.Sucrose has slight coloring phenomenon when 50～52 ℃ of column temperature hydrolysis, illustrate in the hydrolysis time, the existing generation of hydroxymethylfurfural in a small amount.During 54 ℃ of column temperatures, pigment generates comparatively obvious.As seen, sucrose hydrolysis is controlled at a monose that does not make generation, mainly is in the temperature range of fructose degraded, is that the production colour is low, and sugariness is higher than the key of the high fructose syrup of sucrose.Simultaneously, to improving the product yield, keep the resin column catalysis activity stable and permanent, it also is important prolonging its life-span.Sucrose is at H
+During hydrolysis, experiment shows, 10 ℃ of the every raisings of column temperature in the type cationic resin column, its hydrolysis rate then is about original 2.1 times, not causing under the monose destructive situation, selects higher hydrolysis temperature, be good the column temperature that the present invention is preferred 40～52 ℃ to improving the high fructose syrup productive rate.
Input concentration has certain influence to sucrose hydrolysis.Doing experiment with Shanghai 734 type ion exchange resin shows, 40 ℃ of column temperatures, during sucrose 99% hydrolysis, if input concentration is 30,40,50,60 and 65Bx, then the air speed of sucrose by resin column is respectively 0.19,0.32,0.38,0.41 and 0.42 gram sucrose/gram wet resin/time, wet resin moisture 60%.Air speed increases with the increase of input concentration, when promptly input concentration is high, in the unit time, every gramion exchange resin can hydrolysis the sucrose amount just many.Improve input concentration, to effectively utilizing catalyzer, it all is favourable reducing the concentrated expense of syrup.But syrup concentration surpasses after the 60Bx, and liquid glucose mobile relatively poor influences its mobile in the catalysis post.On the other hand, sugar concentration is after 50Bx, and concentration is little to the hydrolysis rate influence, so the present invention selects for use the sucrose concentration of 45～62Bx to come sucrose hydrolysis.
Main contents of the present invention also comprise contents such as the coupling of the selection of ion exchange resin type number and exchange column and arrangement except that the selection of hydrolysis temperature and input concentration scope.According to the requirement to syrup character, the preparation of high fructose syrup divides two kinds of cation seperation column method and positive and negative ionic bond methods, and existing division is as follows:
One, cation seperation column method
Sucrose is passed through the H of 25～54 ℃ of column temperatures with the air speed in 0.10～1.74 gram sugar/gram wet resin/time
+The hydrolysis of type cationic exchange coloum.Like this, if use the white sugar raw material, the syrup PH that then produces is usually more than 3, and it is suitable for carbonated drink, purposes such as fruit can.
No matter the production of sucrose adopts sulfurous method or carbon sulfuric acid process, and its syrup or commerieal sugar always have a small amount of ash based on calcium salt to exist.Sucrose liquid passes through H
+During the type ion exchange column, exchange will take place and the liquid glucose pH value is reduced in impurity such as calcium ion, and ash is many more in the liquid glucose, and PH is just low more after the hydrolysis.White sugar solution as 30～60Bx passes through H
+During the type resin column, its PH is between 2.6～2.8.Thereby, H
+The type ion exchange column can progressively reduce its activity because of exchange takes place, and the raw material ash is many more, and the catalysis post lost efficacy just fast more.If protection catalysis post do not reduce catalytic activity because of ion-exchange takes place, then can with liquid glucose with per hour less than the speed of four times of resin column volumes earlier by a H
+The type resin column, to remove impurity such as calcium ion, again with acid syrup by main another H that plays hydrolytic action
+The type ion exchange column.Like this, not only can make the vigor of catalysis post stable permanent, also make the hydrolysis of sucrose that H in the solution is arranged
+H with resin solid acid
+The dual catalytic effect and accelerate hydrolysis rate.On the other hand, play not the resin cation (R.C.) of same-action and can select different resin models for use, to give full play to effect separately.Play the resin of exchange interaction, can select for use degree of crosslinking slightly high, exchange capacity is bigger, and the resin that the ash disposal ability is stronger as Shanghai 732 resins, or can play the material of exchange interaction with other, as natural or synthetic mordenite replacement.Because the hydrolysis reaction of sucrose in ion exchange column has significant diffusional limitation, thus play the resin that the Zeo-karb of katalysis should be selected enough porositys for use, as Shanghai 734 resins or Shanghai 744 macroporous resins.When this law is used 744 type large hole cation exchanger resins as catalyzer, at 54 ℃, sucrose hydrolysis 50.0%, 75.0%, 87.5% and 93.8% o'clock, its reaction times in post was respectively 1.53,3.06,4.59 and 6.12 minutes, and its hydrolysis rate more greatly improves with relevant patent.The resin particle degree also should with due regard to preferably select for use 40～60 purposes than small-particle.
The acid syrup that this law is produced, also available NaOH or Na
2CO
3Transfer its PH Deng alkaline matter, make it to be suitable for the application target that different PH require.
Two, positive and negative ion exchange column combined techniques
With the syrup of aforesaid method gained, with per hour passing through OH less than the speed of 4 times of resin column volumes
+Type weak anion resin post is to remove the H in the liquid glucose
+, and absorption removes residual coloring matter, the low colour higher-grade syrup of subacidity.The high fructose syrup that this law is produced, PH is that acidity is moderate between 6.3～6.5, is suitable for the syrupy effect of depositing for a long time.Sucrose liquid can also be passed through OH earlier
-Type highly basic or weak base anion-exchange resin and H
+The type resin cation (R.C.) gets colourless neutrality or subacidity liquid glucose, again by another H
+The hydrolysis of type ion exchange resin column gets higher-grade neutrality or subacidity high fructose syrup.Weak anion resin can be selected the tertiary amine-type resin for use, as Shanghai 705, D301A and D301B etc.Basic resin is optional with Shanghai 711 and 717 etc.The type selecting principle of resin cation (R.C.) and method＜one〉with.
The processing of cationic, anionic exchange resin is identical with the method for refining cane mill with regeneration.New ion exchange resin re-uses after answering pickling, alkali cleaning, washing.The concentration of acid, alkali is generally 2N.Zeo-karb 5-10% regeneration of hydrochloric acid, consumption are 3 times of resin volume, are no less than 60 minutes duration of contact.Washing is discharged regenerated liquid with the water of 1.25～1.5 times of resin volumes, again usefulness per hour the speed of 16 times of resin volumes water, cationic, anionic exchange resin is washed till effluent liquid PH respectively is respectively 4 and 8 and can comes into operation.
Characteristics of the present invention are that the sucrose hydrolysis temperature is controlled at 25～54 ℃, preferred 40～52 ℃, give full play to catalyst efficiency, sucrose hydrolysis does not produce coloring matter, the ratio of fructose and glucose is 1: 1 in the syrup, improve the sugariness that sucrose hydrolysis becomes high fructose syrup to greatest extent, also improve the yield of high fructose syrup, and can prolong regeneration of ion-exchange resin cycle and work-ing life.
Use two H
+The placed in-line method of type ion column can be selected suitable ion exchange resin type number, gives full play to the characteristics of each post, keeps catalysis H
+The catalysis activity of post is stable and permanent, is beneficial to the control of catalyzed reaction, also prolongs catalyst regeneration cycle and work-ing life, simultaneously, also brings into play the H in the liquid glucose fully
+H with resin
+Hydrolytic action.
According to syrup requirement of different nature, select different resin columns and matching way for use, can give full play to the effect of various ion exchange resin, save unnecessary step, make equipment simple and practical.
Embodiment 1
Two 1250mm height, the glass column that has insulation jacket of 4.9mm is adorned H respectively in the post
+The storng-acid cation exchange resin of the type 734 and 744 trades mark, its volume all are 80ml.With the white sugar solution (purity 99.8%) of 50.2Bx, respectively by above-mentioned resin column, make sucrose hydrolysis become fructose and glucose with friction-motion speed.The result is as shown in table 1: the 744(20-40 order), 734(40～60 orders)
Table 1 column temperature and air speed are to the influence of sucrose hydrolysis
| Hydrolysis column temperature ℃ | Air speed | High fructose syrup Bx | Fructose % | Glucose % | Sucrose hydrolysis % | Colour (S °) | Mean P H | ||||||
| 734 | 744 | 734 | 744 | 734 | 744 | 734 | 744 | 734 | 744 | 734 | 744 | ||
| 25 | 0.10 | 0.20 | 52.0 | 52.1 | 48.5 | 48.5 | 48.5 | 48.5 | 97 | 97 | 0.38 | 0.37 | 2.85 |
| 35 | 0.24 | 0.41 | 52.4 | 52.3 | 50.0 | 49.5 | 50.0 | 49.5 | 100 | 99 | 0.38 | 0.38 | |
| 40 | 0.50 | 0.74 | 52.1 | 52.1 | 48.5 | 49.0 | 48.5 | 49.0 | 97 | 98 | 0.39 | 0.38 | |
| 45 | 0.52 | 0.79 | 52.3 | 52.2 | 49.5 | 49.5 | 49.5 | 49.5 | 99 | 99 | 0.40 | 0.40 | |
| 50 | 0.76 | 1.23 | 52.2 | 52.2 | 49.0 | 49.5 | 49.0 | 49.5 | 98 | 99 | 0.44 | 0.43 | |
| 54 | 1.07 | 1.74 | 52.2 | 52.3 | 49.5 | 49.5 | 49.5 | 49.5 | 99 | 99 | 0.56 | 0.52 | |
The ※ air speed: in gram sucrose/gram wet resin/time,, wet resin is moisture 60%, white sugar colour 0.60s
Embodiment two
A 1000mm height, the glass column of internal diameter 10mm, interior dress H
+Type 732 strong acidic ion resins, the resin bed height is 800mm, the white sugar solution of 60.5Bx is per hour used passed through this post less than the speed of 4 times of resin bed volumes, and column temperature is controlled at below 40 ℃, again by the resin column hydrolysis of embodiment 1, the result is as shown in table 2 with the gained liquid glucose.
Unless the liquid glucose hydrolysis behind the positive resin hydrogen cation of table 2
Embodiment three
A high 1000mm, the glass column of internal diameter 10mm, interior dress OH
-Type 705 weak anion resins, resin bed height 750mm, with the acid high fructose syrup of embodiment 2 744 resin hydrolyzing gained, at 40 ℃ below the column temperature, with per hour less than the speed of 4 times of resin column volumes by this post, remove residual pigment and H in the liquid glucose
+, the result is as shown in table 3:
Table 3 weakly basic anion resin decolours, takes off H
+Effect
Embodiment four
Two high 1000mm, the glass column of internal diameter 10mm is adorned OH respectively
-Type 717 strongly basic anionic resins and H
+Type 732 strong acidic ion resins, the resin bed height is respectively 750mm and 800mm, with the white sugar solution of 45Bx, per hour passes through OH earlier less than the speed of 4 times of resin bed volumes in usefulness below 40 ℃
+Behind the type resin anion(R.A) post, pass through H again
+The type cationic resin column, removing ion and the pigment in the liquid glucose, and then the H by embodiment 1
+The hydrolysis of type strong acidic ion resin post, the result is as shown in table 4:
The hydrolysis of the no ion sucrose of table 4 liquid
| Hydrolysis column temperature ℃ | Air speed | High fructose syrup Bx | Fructose % | Glucose % | Sucrose hydrolysis % | Colour (S °) | Mean P H | ||||||
| 734 | 744 | 734 | 744 | 734 | 744 | 734 | 744 | 734 | 744 | 734 | 744 | ||
| 25 | 0.09 | 0.18 | 45.9 | 45.8 | 48.5 | 49.0 | 48.5 | 49.0 | 97 | 98 | 0 | 0 | 6.90 |
| 35 | 0.22 | 0.38 | 46.3 | 46.0 | 49.5 | 49.0 | 49.5 | 49.0 | 99 | 98 | 0 | 0 | |
| 40 | 0.33 | 0.52 | 46.5 | 46.4 | 49.5 | 49.5 | 49.5 | 49.5 | 99 | 99 | 0 | 0 | |
| 45 | 0.48 | 0.70 | 46.2 | 46.1 | 49.0 | 50.0 | 49.0 | 50.0 | 98 | 100 | 0 | 0 | |
| 50 | 0.62 | 1.04 | 46.3 | 46.2 | 49.5 | 49.5 | 49.5 | 49.5 | 99 | 99 | 0.03 | 0.02 | |
| 55 | 1.01 | 1.65 | 46.2 | 46.1 | 49.5 | 49.5 | 49.5 | 49.5 | 99 | 99 | 0.12 | 0.10 | |
Embodiment five
A high 1000mm, the glass column of internal diameter 20mm, interior dress H
+The type natural mordenite zeolite, zeolite beds height 850mm with the white sand liquid glucose of 50Bx, below 40 ℃, per hour uses and passes through this post less than the speed of 3 times of zeolite beds volumes, and with the resin column hydrolysis of gained liquid glucose by embodiment 1, its result is as shown in table 5 again:
Unless the hydrolysis of sucrose liquid behind the table 5 zeolite hydrogen ion
Embodiment six
A high 1600mm, the glass column of internal diameter 20mm, the 700mm of lower floor adorns H
+Type 732 strong acidic ion resins, upper strata 700mm adorns OH
-Type 705 weak anion resins, with the white sand liquid glucose of 55Bx, more than 40 ℃ with per hour less than the speed of 850ml liquid glucose by this yin, yang post, the gained liquid glucose is again through too high 1000mm, internal diameter 20mm, interior dress H
+The insulation jacket glass column of type 744 strong acidic ion resins.Hydrolytic resin bed height 900mm.Results of hydrolysis is as shown in table 6:
Table 6 removes the hydrolysis of salt sucrose liquid
Claims (7)
1, a kind of method of producing high fructose syrup with sucrose comprises and uses H
+The type strong acid cation exchange resin catalyst makes sucrose hydrolysis become fructose and glucose, it is characterized by catalyzed reaction and is controlled in 25～54 ℃ of temperature ranges, before the sucrose feed liquid enters the hydrolysis post, makes it pass through H earlier
+The type exchange column is removed non-hydrogen cation, or makes plastics liquid pass through OH earlier
-Type negatively charged ion and H
+The type ion exchange column is removed salt.
2,, it is characterized in that the optimum temperature range of catalyzed reaction control is 40～52 ℃ according to the method described in the claim 1.
3, according to the method described in the claim 1, it is characterized in that the sucrose feed liquid is removed non-hydrogen cation after, only pass through H
+The hydrolysis of type positively charged ion catalysis post gets acid high fructose syrup, changes the adjustment of syrupy PH available bases or passes through OH
-Type weak anion resin post.
4, according to the method described in the claim 1, it is characterized in that OH
-The type resin anion(R.A) can be earlier with strong basicity or weak anion resin, H
+The type ion exchange column can be zeolite or Zeo-karb.
5, according to the method described in the claim 1, when it is characterized in that liquid glucose is removed non-hydrogen cation or salt, column temperature is controlled at below 40 ℃.
6, according to the method described in the claim 1, it is characterized in that H
+Type strong acidic ion resin catalyzer can be bigger ordinary gel resin or a macroporous resin of porosity.
7,, it is characterized in that sucrose hydrolysis adopts the input concentration of 45～62Bx according to the method described in the claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89104363 CN1023327C (en) | 1989-06-21 | 1989-06-21 | High fructose corn syrup prepared by hydrolyzing sucrose with cationic resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89104363 CN1023327C (en) | 1989-06-21 | 1989-06-21 | High fructose corn syrup prepared by hydrolyzing sucrose with cationic resin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1048233A true CN1048233A (en) | 1991-01-02 |
| CN1023327C CN1023327C (en) | 1993-12-29 |
Family
ID=4855530
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 89104363 Expired - Fee Related CN1023327C (en) | 1989-06-21 | 1989-06-21 | High fructose corn syrup prepared by hydrolyzing sucrose with cationic resin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1023327C (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100460522C (en) * | 2004-08-13 | 2009-02-11 | 南宁市化工研究设计院 | High yield crystallized diabetin production process |
| CN101709336B (en) * | 2009-12-21 | 2012-05-23 | 安徽丰原发酵技术工程研究有限公司 | Preparation method of high-concentration high fructose corn syrup |
| CN108719867A (en) * | 2018-04-23 | 2018-11-02 | 西北农林科技大学 | A kind of big jujube products and preparation method thereof rich in oligosaccharide |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101481745B (en) * | 2008-01-09 | 2011-08-31 | 广西工学院 | Method for damaging oxidase in cane juice |
-
1989
- 1989-06-21 CN CN 89104363 patent/CN1023327C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100460522C (en) * | 2004-08-13 | 2009-02-11 | 南宁市化工研究设计院 | High yield crystallized diabetin production process |
| CN101709336B (en) * | 2009-12-21 | 2012-05-23 | 安徽丰原发酵技术工程研究有限公司 | Preparation method of high-concentration high fructose corn syrup |
| CN108719867A (en) * | 2018-04-23 | 2018-11-02 | 西北农林科技大学 | A kind of big jujube products and preparation method thereof rich in oligosaccharide |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1023327C (en) | 1993-12-29 |
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