CN108251570A - A kind of production method of fructose syrup - Google Patents

A kind of production method of fructose syrup Download PDF

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Publication number
CN108251570A
CN108251570A CN201810038398.6A CN201810038398A CN108251570A CN 108251570 A CN108251570 A CN 108251570A CN 201810038398 A CN201810038398 A CN 201810038398A CN 108251570 A CN108251570 A CN 108251570A
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Prior art keywords
hydrolysis
hydrolyzate
fructose syrup
isomaltoketose
waste liquor
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CN201810038398.6A
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施越
施诲宁
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    • CCHEMISTRY; METALLURGY
    • C13SUGAR INDUSTRY
    • C13KSACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
    • C13K11/00Fructose
    • CCHEMISTRY; METALLURGY
    • C13SUGAR INDUSTRY
    • C13KSACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
    • C13K1/00Glucose; Glucose-containing syrups
    • CCHEMISTRY; METALLURGY
    • C13SUGAR INDUSTRY
    • C13KSACCHARIDES OBTAINED FROM NATURAL SOURCES OR BY HYDROLYSIS OF NATURALLY OCCURRING DISACCHARIDES, OLIGOSACCHARIDES OR POLYSACCHARIDES
    • C13K1/00Glucose; Glucose-containing syrups
    • C13K1/06Glucose; Glucose-containing syrups obtained by saccharification of starch or raw materials containing starch
    • C13K1/08Purifying

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • General Health & Medical Sciences (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)
  • Saccharide Compounds (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)

Abstract

The invention discloses a kind of production method of fructose syrup, this method is catalyst with hydrochloric acid or sulfuric acid using isomaltoketose waste liquor as raw material, after hydrolyzing under the high temperature conditions, by being refining to obtain fructose syrup.Advantages of the present invention:1. the raw material of the present invention is to produce the waste liquor generated after isomaltoketose, the comprehensive utilizing status of the conjunction turned waste into wealth can be realized.2. the raw material of the present invention is to produce the waste liquor generated after isomaltoketose, the environmental protection treatment burden of isomalt manufacturing enterprise can be mitigated.3. the invention has the advantages that the small investment needed for industrialized production, maturation simple for process, product use scope is wide, is a kind of method easy to implement.

Description

A kind of production method of fructose syrup
Technical field
The invention belongs to sour water solution disaccharide to become monosaccharide field.The production method of specifically a kind of fructose syrup is with different The method that maltulose waste liquor produces fructose syrup for raw material.
Background technology
Isomalt starts industrialized production at home as a kind of new resource food, the production of the product Need first to produce the isomaltoketose of high-purity in journey, the production of the sugar be converted using sucrose as raw material through biological isomery and Come, conversion ratio domestic at present is between 80% to 85%, some sucrose inversion is into trehalulose.Preparation of industrialization is high-purity The isomaltoketose of degree is generally using the method for crystallisation by cooling separation, and the waste liquor generated after crystallizing three times is without recycling valency Value, since the solid content in mother liquor is the mixture of isomaltoketose and trehalulose, is non-sugar fermentation, is difficult in other industry It uses, therefore waste liquor becomes the burden of environmental protection of enterprise.
There is the recoverying and utilizing method that open source information publishes the waste liquor, this method is to detach seaweed ketone using Simulation moving bed Sugar, but separation purity can only achieve 70%, and another this method industrialized production equipment investment is big, and it is other that Gu also rests on laboratory level Scale.
Isomaltoketose, trehalulose and sucrose are isomers, by a fructose and the molecule of a glucose Composition, the method for caring for the present invention are using acid-hydrolyzed principle, by adding inorganic acid in waste liquor, are made under the high temperature conditions Fructose and glucose sugar, then neutralized, activated carbon decolorizing filtering, ion are resolved into glycosidic bond fracture between fructose and glucose sugar The fructose syrup containing 50% fructose is made after exchanging refinery decolorization.
Invention content
The purpose of the present invention is to provide a kind of production methods of fructose syrup.
Technical proposal that the invention solves the above-mentioned problems is as follows:
A kind of production method of fructose syrup is using isomaltoketose waste liquor as raw material, is catalysis with hydrochloric acid or sulfuric acid Agent, after hydrolyzing under the high temperature conditions, by being refining to obtain fructose syrup.Operating procedure is as follows:
1. adjust pH value:
The pH value of isomaltoketose waste liquor is adjusted to 1.70~0.95 with sulfuric acid or hydrochloric acid.
2. heating hydrolysis:
Step 1 is adjusted to the waste liquor after pH value to be added in enamel reaction still, heat hydrolysis, the temperature of hydrolysis is 120 DEG C ~150 DEG C, the time of hydrolysis is 30~60min, obtains hydrolyzate, and the temperature of hydrolysis is 120 DEG C~150 DEG C, the time of hydrolysis For 10~60min, hydrolyzate is obtained, the percent hydrolysis of isomaltoketose and trehalulose is 25.5%~97.9%.
3. hydrolyzate is neutralized, decolourizes and is filtered:
Hydrolyzate is cooled to 70 DEG C, calcium carbonate is added in and is neutralized to pH=4.63, add the work of hydrolyzate weight 0.5% Property charcoal, stirring decoloration 30 minutes, filtering removal activated carbon;The activated carbon of hydrolyzate weight 0.5%, stirring decoloration 30 are added in again Minute, filtering removal activated carbon, collection obtains the liquid glucose of yellow transparent.
4. ion exchange resin refines desalination bleaching;
Glass column is packed into large porous strong acid cation exchange resin and macropore weak base type anion exchange resin, through washing After salt washes transition sizing elution, sun-anion exchange resin system is formed, the hydrolyzate of decolorization filtering controls flow with peristaltic pump With the flow velocity of 2BV/H by ion exchange system, the refined liquid glucose of clear, colorless is obtained.
5. concentration;
The sodium pyrosulfite of 100PPM is added in refined liquid glucose, is concentrated with vacuum rotary evaporator, heating water bath Temperature is maintained at 85 DEG C, is concentrated into pol and can obtain fructose syrup to 70%.
The pH value that above-mentioned steps 1 hydrolyze is preferably 1.30.
The temperature hydrolyzed in above-mentioned steps 2 is preferably 140 DEG C.
The time hydrolyzed in above-mentioned steps 2 is preferably 30min.
Specific embodiment
With reference to embodiment, the invention will be further described, but it should be noted that the present invention application range not It is confined to these embodiments.
Embodiment 1
A kind of production method of fructose syrup is using isomaltoketose waste liquor as raw material, is catalysis with hydrochloric acid or sulfuric acid Agent, after hydrolyzing under the high temperature conditions, by being refining to obtain fructose syrup.Operating procedure is as follows:
1. adjust pH value:The pH value of isomaltoketose waste liquor is adjusted to 1.70 with sulfuric acid or hydrochloric acid.
2. heating hydrolysis:Step 1 is adjusted to the waste liquor after pH value to be added in enamel reaction still, heat hydrolysis, hydrolysis Temperature is 120 DEG C, and the time of hydrolysis is 60min, obtains hydrolyzate, and the temperature of hydrolysis is 120 DEG C~150 DEG C, the time of hydrolysis For 60min, hydrolyzate is obtained, the percent hydrolysis of isomaltoketose and trehalulose is 25.5%.
3. hydrolyzate is neutralized, decolourizes and is filtered:Hydrolyzate is cooled to 70 DEG C, calcium carbonate is added in and is neutralized to pH=4.63, Add the activated carbon of hydrolyzate weight 0.5%, stirring decoloration 30 minutes, filtering removal activated carbon;Hydrolyzate weight is added in again The activated carbon of amount 0.5%, stirring decoloration 30 minutes, filtering removal activated carbon, collection obtain the liquid glucose of yellow transparent.
4. ion exchange resin refines desalination bleaching;With large porous strong acid cation exchange resin and macropore weak base type the moon from Sub-exchange resin is packed into glass column, after washing salt washes transition sizing elution, forms sun-anion exchange resin system, decoloration The hydrolyzate of filtering peristaltic pump controls flow, by ion exchange system, to obtain the refined of clear, colorless with the flow velocity of 2BV/H Liquid glucose.
5. concentration;The sodium pyrosulfite of 100PPM is added in refined liquid glucose, is concentrated with vacuum rotary evaporator, water Bath heating temperature is maintained at 85 DEG C, is concentrated into pol and can obtain fructose syrup to 70%.
Embodiment 2
A kind of production method of fructose syrup is using isomaltoketose waste liquor as raw material, is catalysis with hydrochloric acid or sulfuric acid Agent, after hydrolyzing under the high temperature conditions, by being refining to obtain fructose syrup.Operating procedure is as follows:
1. adjust pH value:The pPH values of isomaltoketose waste liquor are adjusted to 0.95 with sulfuric acid or hydrochloric acid.
2. heating hydrolysis:Step 1 is adjusted to the waste liquor after pH value to be added in enamel reaction still, heat hydrolysis, hydrolysis Temperature is 120 DEG C, and time of hydrolysis is 60min, obtains hydrolyzate, and the percent hydrolysis of isomaltoketose and trehalulose is 46.3%.
3. hydrolyzate is neutralized, decolourizes and is filtered:Hydrolyzate is cooled to 70 DEG C, calcium carbonate is added in and is neutralized to pH=4.63, Add the activated carbon of hydrolyzate weight 0.5%, stirring decoloration 30 minutes, filtering removal activated carbon;Hydrolyzate weight is added in again The activated carbon of amount 0.5%, stirring decoloration 30 minutes, filtering removal activated carbon, collection obtain the liquid glucose of yellow transparent.
4. ion exchange resin refines desalination bleaching;With large porous strong acid cation exchange resin and macropore weak base type the moon from Sub-exchange resin is packed into glass column, after washing salt washes transition sizing elution, forms sun-anion exchange resin system, decoloration The hydrolyzate of filtering peristaltic pump controls flow, by ion exchange system, to obtain the refined of clear, colorless with the flow velocity of 2BV/H Liquid glucose.
5. concentration;The sodium pyrosulfite of 100PPM is added in refined liquid glucose, is concentrated with vacuum rotary evaporator, water Bath heating temperature is maintained at 85 DEG C, is concentrated into pol and can obtain fructose syrup to 70%.
Embodiment 3
A kind of production method of fructose syrup is using isomaltoketose mother liquor as raw material, is catalyst with hydrochloric acid or sulfuric acid, After hydrolyzing under the high temperature conditions, by being refining to obtain fructose syrup.Operating procedure is as follows:
1. adjust pH value:The pH value of isomaltoketose waste liquor is adjusted to 1.70 with sulfuric acid or hydrochloric acid.
2. heating hydrolysis:Step 1 is adjusted to the waste liquor after pH value to be added in enamel reaction still, heat hydrolysis, hydrolysis Temperature is 150 DEG C, and the time of hydrolysis is 30min, obtains hydrolyzate, obtains the water of hydrolyzate, isomaltoketose and trehalulose Solution rate is 97.9%.
3. hydrolyzate is neutralized, decolourizes and is filtered:Hydrolyzate is cooled to 70 DEG C, calcium carbonate is added in and is neutralized to pH=4.63, Add the activated carbon of hydrolyzate weight 0.5%, stirring decoloration 30 minutes, filtering removal activated carbon;Hydrolyzate weight is added in again The activated carbon of amount 0.5%, stirring decoloration 30 minutes, filtering removal activated carbon, collection obtain the liquid glucose of yellow transparent.
4. ion exchange resin refines desalination bleaching;With large porous strong acid cation exchange resin and macropore weak base type the moon from Sub-exchange resin is packed into glass column, after washing salt washes transition sizing elution, forms sun-anion exchange resin system, decoloration The hydrolyzate of filtering peristaltic pump controls flow, by ion exchange system, to obtain the refined of clear, colorless with the flow velocity of 2BV/H Liquid glucose.
5. concentration;The sodium pyrosulfite of 100PPM is added in refined liquid glucose, is concentrated with vacuum rotary evaporator, water Bath heating temperature is maintained at 85 DEG C, is concentrated into pol and can obtain fructose syrup to 70%.
Embodiment 4
A kind of production method of fructose syrup is using isomaltoketose mother liquor as raw material, is catalyst with hydrochloric acid or sulfuric acid, After hydrolyzing under the high temperature conditions, by being refining to obtain fructose syrup.Operating procedure is as follows:
1. adjust pH value:The pH value of isomaltoketose waste liquor is adjusted to 1.30 with sulfuric acid or hydrochloric acid.
2. heating hydrolysis:Step 1 is adjusted to the waste liquor after pH value to be added in enamel reaction still, heat hydrolysis, hydrolysis Temperature is 140 DEG C, and the time of hydrolysis is 30min, obtains hydrolyzate, obtains the water of hydrolyzate, isomaltoketose and trehalulose Solution rate is 97.5%.
3. hydrolyzate is neutralized, decolourizes and is filtered:Hydrolyzate is cooled to 70 DEG C, calcium carbonate is added in and is neutralized to pH=4.63, Add the activated carbon of hydrolyzate weight 0.5%, stirring decoloration 30 minutes, filtering removal activated carbon;Hydrolyzate weight is added in again The activated carbon of amount 0.5%, stirring decoloration 30 minutes, filtering removal activated carbon, collection obtain the liquid glucose of yellow transparent.
4. ion exchange resin refines desalination bleaching;With large porous strong acid cation exchange resin and macropore weak base type the moon from Sub-exchange resin is packed into glass column, after washing salt washes transition sizing elution, forms sun-anion exchange resin system, decoloration The hydrolyzate of filtering peristaltic pump controls flow, by ion exchange system, to obtain the refined of clear, colorless with the flow velocity of 2BV/H Liquid glucose.
5. concentration;The sodium pyrosulfite of 100PPM is added in refined liquid glucose, is concentrated with vacuum rotary evaporator, water Bath heating temperature is maintained at 85 DEG C, is concentrated into pol and can obtain fructose syrup to 70%.

Claims (3)

1. a kind of production method of fructose syrup, which is characterized in that using isomaltoketose waste liquor as raw material, with sulfuric acid or hydrochloric acid For catalyst, hydrolysis under the high temperature conditions obtains fructose syrup, and operating procedure is as follows:
(1) pH value is adjusted:The pH value of isomaltoketose waste liquor is adjusted to 1.70~0.95 with sulfuric acid or hydrochloric acid;
(2) heating hydrolysis:
Step (1) is adjusted to the waste liquor after pH value and is added to heating hydrolysis in enamel reaction still, the temperature of hydrolysis for 120 DEG C~ 150 DEG C, time of hydrolysis is 30~60min, obtains hydrolyzate, the percent hydrolysis of isomaltoketose and trehalulose for 25.5%~ 97.9%;
(3) hydrolyzate is neutralized, decolourizes and is filtered:
Hydrolyzate is cooled to 70 DEG C, calcium carbonate is added in and is neutralized to pH=4.63, add the activity of hydrolyzate weight 0.5% Charcoal, stirring decoloration 30 minutes, filtering removal activated carbon;The activated carbon of hydrolyzate weight 0.5%, 30 points of stirring decoloration are added in again Clock, filtering removal activated carbon, collection obtain the liquid glucose of yellow transparent;
(4) ion exchange resin refines desalination bleaching;
Glass column is packed into large porous strong acid cation exchange resin and macropore weak base type anion exchange resin, is washed through washing salt After transition sizing elution, form sun-anion exchange resin system, the hydrolyzate of decolorization filtering peristaltic pump control flow with The flow velocity of 2BV/H obtains the refined liquid glucose of clear, colorless by ion exchange system;
(5) it concentrates;
The sodium pyrosulfite of 100PPM is added in refined liquid glucose, is concentrated with vacuum rotary evaporator, water bath heating temperature 85 DEG C are maintained at, pol is concentrated into and can obtain fructose syrup to 70%.
A kind of 2. production method of fructose syrup according to claim 1, which is characterized in that the p of step (1) hydrolysis H values are 1.30.
3. the production method of a kind of fructose syrup according to claim 1, which is characterized in that hydrolyzed in the step (2) Temperature for 140 DEG C, the time of hydrolysis is 30min.
CN201810038398.6A 2018-01-13 2018-01-13 A kind of production method of fructose syrup Pending CN108251570A (en)

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CN105256079A (en) * 2015-10-22 2016-01-20 林树仁 Purification method for HFCS (high fructose corn syrup) in fructose production process
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CN105256079A (en) * 2015-10-22 2016-01-20 林树仁 Purification method for HFCS (high fructose corn syrup) in fructose production process
CN105331751A (en) * 2015-10-22 2016-02-17 邓和超 Method for preparing medicinal waterless crystallized fructose by taking sugarcane as raw material
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Application publication date: 20180706