CN103725731B - Special crystalline dextrose of Sunmorl N 60S and preparation method thereof - Google Patents
Special crystalline dextrose of Sunmorl N 60S and preparation method thereof Download PDFInfo
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- 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 title claims abstract description 143
- 239000008121 dextrose Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000002425 crystallisation Methods 0.000 claims abstract description 118
- 230000008025 crystallization Effects 0.000 claims abstract description 104
- 238000010926 purge Methods 0.000 claims abstract description 40
- 238000005342 ion exchange Methods 0.000 claims abstract description 36
- 238000001914 filtration Methods 0.000 claims abstract description 30
- 239000007788 liquid Substances 0.000 claims abstract description 24
- 238000002156 mixing Methods 0.000 claims abstract description 22
- 239000008103 glucose Substances 0.000 claims abstract description 13
- 238000005115 demineralization Methods 0.000 claims abstract description 8
- 230000002328 demineralizing effect Effects 0.000 claims abstract description 8
- 102000004169 proteins and genes Human genes 0.000 claims description 63
- 108090000623 proteins and genes Proteins 0.000 claims description 63
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 51
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 42
- 238000000034 method Methods 0.000 claims description 31
- 238000001816 cooling Methods 0.000 claims description 28
- 239000007787 solid Substances 0.000 claims description 28
- 239000000126 substance Substances 0.000 claims description 28
- 239000006188 syrup Substances 0.000 claims description 21
- 235000020357 syrup Nutrition 0.000 claims description 21
- 238000002834 transmittance Methods 0.000 claims description 21
- 239000012452 mother liquor Substances 0.000 claims description 16
- 235000013336 milk Nutrition 0.000 claims description 15
- 239000008267 milk Substances 0.000 claims description 15
- 210000004080 milk Anatomy 0.000 claims description 15
- 239000002826 coolant Substances 0.000 claims description 14
- 239000013078 crystal Substances 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- 238000001704 evaporation Methods 0.000 claims description 14
- 230000008020 evaporation Effects 0.000 claims description 14
- 238000002347 injection Methods 0.000 claims description 14
- 239000007924 injection Substances 0.000 claims description 14
- 239000011229 interlayer Substances 0.000 claims description 14
- 238000012423 maintenance Methods 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 229920002472 Starch Polymers 0.000 claims description 8
- 235000013305 food Nutrition 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- 235000019698 starch Nutrition 0.000 claims description 8
- 239000008107 starch Substances 0.000 claims description 8
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims description 7
- 229920002261 Corn starch Polymers 0.000 claims description 7
- 102000004190 Enzymes Human genes 0.000 claims description 7
- 108090000790 Enzymes Proteins 0.000 claims description 7
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 102000004139 alpha-Amylases Human genes 0.000 claims description 7
- 108090000637 alpha-Amylases Proteins 0.000 claims description 7
- 229940024171 alpha-amylase Drugs 0.000 claims description 7
- 238000004061 bleaching Methods 0.000 claims description 7
- 229910001424 calcium ion Inorganic materials 0.000 claims description 7
- 150000001768 cations Chemical class 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000008120 corn starch Substances 0.000 claims description 7
- 229940088598 enzyme Drugs 0.000 claims description 7
- 239000010419 fine particle Substances 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 7
- 229910001425 magnesium ion Inorganic materials 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 229920001467 poly(styrenesulfonates) Polymers 0.000 claims description 7
- 239000011347 resin Substances 0.000 claims description 7
- 229920005989 resin Polymers 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 7
- 230000003068 static effect Effects 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 abstract description 2
- 239000002253 acid Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000010276 construction Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 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 description 1
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 description 1
- RGHNJXZEOKUKBD-SQOUGZDYSA-N Gluconic acid Natural products OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 230000003467 diminishing effect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 239000000174 gluconic acid Substances 0.000 description 1
- 235000012208 gluconic acid Nutrition 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- -1 organic acid salt Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002516 radical scavenger Substances 0.000 description 1
- 230000000979 retarding effect Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
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Abstract
The invention discloses the preparation method of the special crystalline dextrose of a kind of Sunmorl N 60S, comprise the following steps: (1) sizes mixing; (2) liquefy; (3) high temperature filtration; (4) filter at low temperature; (5) prepare burden; (6) saccharification; (7) decolour; (8) ion-exchange demineralization; (9) evaporate; (10) heat gives crystallization; (11) first time cold crystallization; (12) first time crystallization massecuite purging; (13) wet sugared back dissolving; (14) second time cold crystallization; (15) second time crystallization massecuite purging; (16) oven dry obtains finished product crystalline dextrose: pH value is 6.0 ~ 6.5, DX value >=99.8%, clarity and color≤0.5#, muriate≤0.0004, vitriol≤0.0008; The present invention effectively reduces the addition of thinning operation soda acid; Greatly improve the purity of the special crystalline dextrose of Sunmorl N 60S; Improve the glucose content of saccharified liquid; Improve finished product pH value.
Description
Technical field
The present invention relates to a kind of glucose and preparation method thereof, be specifically related to special crystalline dextrose of a kind of Sunmorl N 60S and preparation method thereof.
Background technology
Sunmorl N 60S, also known as sodium pentahydyoxycaproate, is the organic acid salt of multihydroxyl that a kind of purposes is extremely wide, in medicine, food, water quality stabilizer, steel surface clean-out system, vial scavenger specially, cement additive etc., has purposes widely.Ratio with 3-5%, at 500,000 tons/year, increases by Sunmorl N 60S whole world demand every year, and current production rate and demand differ greatly, and are a kind of products having bright market prospects.
Sunmorl N 60S industrially purposes is very extensive, concrete admixture (water reducer and retardant) is widely used as in construction industry, it is a Chaoyang industry, it is industry rising greatly, China is still in the large-scaled construction period, and a large amount of priority projects carrying out and in planning-subway, Civil Aviation Airport, High-speed Railway Network, southwestern construction of hydropower facilities etc. of big and medium-sized cities.Its diminishing, plasticising, retarding effect are all very remarkable, can greatly improve concrete workability, reduce slump-loss, improve concrete later strength, the presetting period can be made to extend to several days from several hours and can't harm intensity as retardant.And applied widely, all can apply in pump concrete, Cracking of High Flowing Concrete, mass concrete, high grade concrete.As starting material important in concrete, Sunmorl N 60S admixture also has very large development space.
Industrial general with the material (such as grain) containing glucose for raw material, adopt fermentation method elder generation to obtain gluconic acid by glucose, and then neutralized by sodium hydroxide, Sunmorl N 60S, also can adopt electrolytic process and oxidative synthesis.China mostly adopts heterogeneous catalytic oxidation method to produce synthesis.
But it is also a lot of to restrict Sunmorl N 60S suitability for industrialized production factor simultaneously, such as yield low cost is high, vitriol, chloride content exceed standard, heavy metal content exceeds standard, the Sunmorl N 60S that current production technique is obtained, glucose content < 99.5, pH value 5.0-5.5, clarity and color >=0.5#, muriate≤0.01%, vitriol≤0.02%.
Summary of the invention
The object of the invention is to solve the above-mentioned technical problem existed in prior art, special crystalline dextrose of a kind of Sunmorl N 60S and preparation method thereof is provided, the special crystalline dextrose of this Sunmorl N 60S is high purity, high ph-values, low metal, the crystalline dextrose of low chloride content, makes that product is more single-minded to be produced for Sunmorl N 60S, greatly improve Sunmorl N 60S product yield, Reaction time shorten reduces consumption; And preparation method is simple, the reaction times shortens greatly, reduces production cost.
For achieving the above object, the technical solution used in the present invention is as follows:
The preparation method of the special crystalline dextrose of a kind of Sunmorl N 60S, comprise the following steps: (1) sizes mixing: with deionized water, corn starch milk is transferred to 19-20 B é, regulate pH to 5.4 ~ 5.8, add alpha-amylase total amount 0.45-0.5kg/tds, pH value of starch milk > 5.0, conductance < 300 us/cm; (2) liquefy: injection temperature 105 ~ 108 DEG C for the first time, maintenance with pressure 12 ~ 18 minutes; Second time injection temperature 135 ~ 140 DEG C, maintenance with pressure 2 ~ 3 minutes, enters laminar flow tank, keeps temperature>=98 DEG C, liquefaction terminal DE value 13 ~ 17%; (3) high temperature filtration: after liquefaction terminates, feed liquid keeps 85-95 DEG C and directly enters bipyramid horizontal spiral separator, carries out separation and removes the macrobead solid substances such as solidifying wadding protein, separating machine feed rate≤25m
3/ h, rotary drum rotating speed 3650 revs/min, spiral and rotating cylinder differential 29.6 revs/min, separating medium temperature 0-100 DEG C, pH value 4-9; (4) filter at low temperature: the liquefier after high temperature filtration changes through cold water temperature lowering board and is down to 18 DEG C by 85 DEG C, enter to coagulate wadding tank and be incubated 30 minutes, add food grade kieselguhr filtering medium simultaneously, addition 0.8kg/tds, stir 5-10 minute, fine particle albumen and soluble proteins are carried out the solidifying wadding of cold induced proteins, then carry out low temperature sheet frame squeeze and filter, further removal liquid glucose from the solid substance such as protein, reach pure liquefier; (5) prepare burden: be that 75:25 mixes by liquefier and second time crystallization massecuite isolated glucose mother liquid with volume ratio, DE value > 98%; (6) saccharification: pure liquefier is warming up to 60-62 DEG C, adjust pH, to 4.2-4.4, enters saccharifying tank and adds compounded saccharifying enzyme 0.4-0.45kg/tds, static reaction 48 hours, saccharification terminal DE value>=98%, DX value>=97%; (7) decolour: adjustment liquid glucose pH value to 4.8, reaches the iso-electric point of protein condenses, and increase activated carbon dosage, soluble protein generation iso-electric point is condensed, become insoluble protein and be tightly held by activated carbon, removing the solid substances such as protein through sheet frame squeeze and filter, reach pure liquid glucose.Activated carbon dosage is the 4-5% of liquid glucose butt, enters pressure filter after stirring 18-25 minute in bleacher, bleaching temperature 75-80 DEG C, decolours 30 minutes, the liquid glucose specific conductivity≤300us/cm after decolouring, transmittance>=98%; (8) ion-exchange demineralization: material step (6) obtained is successively through cation bed-anion bed-cation bed-anion bed-adjustable column, totally three groups of ion exchange columns, carry out ion-exchange, remove impurity in liquid glucose, then liquid glucose enters de-taste post, described de-taste post adopts de-taste resin: Dowex Optipore SD-2, carry out ion-exchange, protein in liquid glucose and calcium ions and magnesium ions are removed, reach purer liquid glucose, flow is 2.5 BV/h, temperature≤55 DEG C, pressure≤2.0kg/cm during operation in first post
2, the specific conductivity≤15us/cm of liquid glucose after ion-exchange, pH value 3.8-4.2, transmittance>=98%; (9) evaporate: liquid glucose being concentrated to solid substance is 72.5 ~ 73.5%, during well heater work, keep continuity, pressure>=0. 5Mpa that steam is total, liquid glucose DX value > 90; (10) heat gives crystallization: the liquid glucose after evaporation enters flash tank and carries out flash concentration crystallization, produces fine crystals; (11) first time cold crystallization: the sugar concentration 73-75% after thermal crystalline, temperature is 60 ~ 62 DEG C, transmittance > 98, pH value 3.8 ~ 4.2, direct feeding crystallizer adopts the crystallization of Temperature fall method, crystallizer reserves seed for planting 25 ~ 30%, dense syrup during canful after evaporation and mixeding liquid temperature>=48 DEG C of crystal seed, crystallization total time is 60 hours, the temperature difference≤15 DEG C of crystallizer interlayer coolant water temperature and sugar temperature, and crystallizer mixing speed is 0.7 turn/min; (12) first time crystallization massecuite purging: massecuite after crystallization is delivered to whizzer and carries out purging, control wash water temperature 30 ~ 32 DEG C, wet syrup divides < 13%, isolated mother liquor is outer row all; (13) wet sugared back dissolving: the wet sugar hot deionized water after purging is dissolved to concentration 72-74%, pH value 6.0-6.5, temperature 60-62 DEG C; (14) second time cold crystallization: the liquid glucose after dissolving is sent into crystallizer, adopt the crystallization of Temperature fall method, crystallizer reserves seed for planting 25 ~ 30%, and crystallization total time is 60 hours, the temperature difference≤15 DEG C of crystallizer interlayer coolant water temperature and sugar temperature, crystallizer mixing speed is 0.7 turn/min; (15) second time crystallization massecuite purging: massecuite after second time cold crystallization is delivered to whizzer and carries out purging, controls wash water temperature 30 ~ 32 DEG C, wet syrup divides < 13%, and isolated mother liquor and the liquefier after filtering carry out mixture; (16) oven dry obtains the special crystalline dextrose of finished product: pH value is 6.0 ~ 6.5, DX value>=99.8%, clarity and color≤0.5#, muriate≤0.0004, vitriol≤0.0008.
60 hours described crystallization total times, wherein, growing the grain 12 hours, adopts Temperature fall method, crystallisation by cooling 48 hours; Crystallisation by cooling divides two stages: 28 hours first stage, sugar temperature is dropped to 35 DEG C from 46 DEG C, cooling≤0.4 DEG C per hour, and subordinate phase 20 hours, drops to 22 DEG C by sugar temperature from 35 DEG C, cooling≤0.65 DEG C per hour.
The special crystalline dextrose of Sunmorl N 60S obtained according to the method described above, its pH value is 6.0 ~ 6.5, DX value >=99.8%, clarity and color≤0.5#, muriate≤0.0004, vitriol≤0.0008.
Compared with prior art, the present invention has following advantage: (1) starch milk raw material controls to reach high ph-values, low inorganic salt content, effectively reduces the addition of thinning operation soda acid, not only reduces supplementary product onsumption but also can alleviate ion exchange resin desalination load; (2) liquefier adopts high temperature filtration, and the solidifying wadding of low temperature, is more conducive to improve saccharification result; (3) crystallization adopts flash concentration crystallization, and cold crystallization and second time cold crystallization, totally three crystallizations, improve the purity of the special crystalline dextrose of Sunmorl N 60S greatly for the first time; (4) mother liquor of first time crystallization massecuite purging all outer rows, the mother liquor of second time crystallization massecuite purging is used for back joining, and improves the glucose content of saccharified liquid; (5) regulate liquid glucose pH value during wet sugared back dissolving after first time purging, improve finished product pH value.
Embodiment
embodiment 1
The preparation method of the special crystalline dextrose of the present embodiment Sunmorl N 60S, comprise the following steps: (1) sizes mixing: with deionized water, corn starch milk is transferred to 19 B é, regulate pH to 5.4, add alpha-amylase total amount 0.45kg/tds, pH value of starch milk > 5.0, conductance < 300 us/cm; (2) liquefy: injection temperature 105 DEG C for the first time, maintenance with pressure 12 minutes; Second time injection temperature 135 DEG C, maintenance with pressure 2 minutes, enters laminar flow tank, keeps temperature>=98 DEG C, liquefaction terminal DE value 13%; (3) high temperature filtration: after liquefaction terminates, feed liquid keeps 85 DEG C directly to enter SEDICANTER S 6E bipyramid horizontal spiral separator, carries out separation and removes the macrobead solid substances such as solidifying wadding protein, separating machine feed rate≤25m
3/ h, rotary drum rotating speed 3650 revs/min, spiral and rotating cylinder differential 29.6 revs/min, separating medium temperature 0 DEG C, pH value is 4; (4) filter at low temperature: the liquefier after high temperature filtration changes through cold water temperature lowering board and is down to 18 DEG C by 85 DEG C, enter to coagulate wadding tank and be incubated 30 minutes, add food grade kieselguhr filtering medium simultaneously, addition 0.8kg/tds, stir 5 minutes, fine particle albumen and soluble proteins are carried out the solidifying wadding of cold induced proteins, then carry out low temperature sheet frame squeeze and filter, further removal liquid glucose from the solid substance such as protein, reach pure liquefier; (5) prepare burden: be that 75:25 mixes by liquefier and second time crystallization massecuite isolated glucose mother liquid with volume ratio, DE value > 98%; (6) saccharification: pure liquefier is warming up to 60 DEG C, adjust pH to 4.2, enters saccharifying tank and adds compounded saccharifying enzyme 0.4kg/tds, static reaction 48 hours, saccharification terminal DE value>=98%, DX value>=97%; (7) decolour: adjustment liquid glucose pH value to 4.8, reaches the iso-electric point of protein condenses, and increase activated carbon dosage, soluble protein generation iso-electric point is condensed, become insoluble protein and be tightly held by activated carbon, removing the solid substances such as protein through sheet frame squeeze and filter, reach pure liquid glucose.Activated carbon dosage is 4% of liquid glucose butt, stirs after 18 minutes and enters pressure filter, bleaching temperature 75 DEG C, decolour 30 minutes, the liquid glucose specific conductivity≤300us/cm after decolouring, transmittance>=98% in bleacher; (8) ion-exchange demineralization: material step (6) obtained is successively through cation bed-anion bed-cation bed-anion bed-adjustable column, totally three groups of ion exchange columns, carry out ion-exchange, remove impurity in liquid glucose, then liquid glucose enters de-taste post, described de-taste post adopts de-taste resin: Dowex Optipore SD-2, carry out ion-exchange, protein in liquid glucose and calcium ions and magnesium ions are removed, reach purer liquid glucose, flow is 2.5 BV/h, temperature≤55 DEG C, pressure≤2.0kg/cm during operation in first post
2, the specific conductivity≤15us/cm of liquid glucose after ion-exchange, pH value 3.8, transmittance>=98%; (9) evaporate: liquid glucose being concentrated to solid substance is 72.5%, during well heater work, keep continuity, pressure>=0. 5Mpa that steam is total, liquid glucose DX value > 90; (10) heat gives crystallization: the liquid glucose after evaporation enters flash tank and carries out flash concentration crystallization, produces fine crystals; (11) first time cold crystallization: the sugar concentration 73% after thermal crystalline, temperature is 60 DEG C, transmittance > 98, pH value 3.8, direct feeding crystallizer adopts the crystallization of Temperature fall method, crystallizer reserves seed for planting 25%, dense syrup during canful after evaporation and mixeding liquid temperature>=48 DEG C of crystal seed, crystallization total time is 60 hours, the temperature difference≤15 DEG C of crystallizer interlayer coolant water temperature and sugar temperature, and crystallizer mixing speed is 0.7 turn/min; (12) first time crystallization massecuite purging: massecuite after crystallization is delivered to whizzer and carries out purging, control wash water temperature 30 DEG C, wet syrup divides < 13%, isolated mother liquor is outer row all; (13) wet sugared back dissolving: the wet sugar hot deionized water after purging is dissolved to concentration 72%, pH value 6.0, temperature 60 C; (14) second time cold crystallization: the liquid glucose after dissolving is sent into crystallizer, adopt the crystallization of Temperature fall method, crystallizer reserves seed for planting 25%, and crystallization total time is 60 hours, and wherein, growing the grain 12 hours, adopts Temperature fall method, crystallisation by cooling 48 hours; Crystallisation by cooling divides two stages: 28 hours first stage, sugar temperature is dropped to 35 DEG C from 46 DEG C, cooling≤0.4 DEG C per hour, subordinate phase 20 hours, sugar temperature is dropped to 22 DEG C from 35 DEG C, cooling≤0.65 DEG C per hour, the temperature difference≤15 DEG C of crystallizer interlayer coolant water temperature and sugar temperature, crystallizer mixing speed is 0.7 turn/min; (15) second time crystallization massecuite purging: massecuite after second time cold crystallization is delivered to whizzer and carries out purging, controls wash water temperature 30 DEG C, wet syrup divides < 13%, and isolated mother liquor and the liquefier after filtering carry out mixture; (16) oven dry obtains the special crystalline dextrose of finished product: pH value is 6.0, DX value>=99.8%, clarity and color≤0.5#, muriate≤0.0004, vitriol≤0.0008.
The special crystalline dextrose of Sunmorl N 60S obtained according to the method described above, its pH value is 6.0, DX value >=99.8%, clarity and color≤0.5#, muriate≤0.0004, vitriol≤0.0008.
embodiment 2
The preparation method of the special crystalline dextrose of the present embodiment Sunmorl N 60S, comprise the following steps: (1) sizes mixing: with deionized water, corn starch milk is transferred to 19.2 B é, regulate pH to 5.5, add alpha-amylase total amount 0.46kg/tds, pH value of starch milk > 5.0, conductance < 300 us/cm; (2) liquefy: injection temperature 106 DEG C for the first time, maintenance with pressure 13 minutes; Second time injection temperature 136 DEG C, maintenance with pressure 2 minutes, enters laminar flow tank, keeps temperature>=98 DEG C, liquefaction terminal DE value 14%; (3) high temperature filtration: after liquefaction terminates, feed liquid keeps 86 DEG C directly to enter SEDICANTER S 6E bipyramid horizontal spiral separator, carries out separation and removes the macrobead solid substances such as solidifying wadding protein, separating machine feed rate≤25m
3/ h, rotary drum rotating speed 3650 revs/min, spiral and rotating cylinder differential 29.6 revs/min, separating medium temperature 20-100 DEG C, pH value 5; (4) filter at low temperature: the liquefier after high temperature filtration changes through cold water temperature lowering board and is down to 18 DEG C by 86 DEG C, enter to coagulate wadding tank and be incubated 30 minutes, add food grade kieselguhr filtering medium simultaneously, addition 0.8kg/tds, stir 6 minutes, fine particle albumen and soluble proteins are carried out the solidifying wadding of cold induced proteins, then carry out low temperature sheet frame squeeze and filter, further removal liquid glucose from the solid substance such as protein, reach pure liquefier; (5) prepare burden: be that 75:25 mixes by liquefier and second time crystallization massecuite isolated glucose mother liquid with volume ratio, DE value > 98%; (6) saccharification: pure liquefier is warming up to 61 DEG C, adjust pH to 4.3, enters saccharifying tank and adds compounded saccharifying enzyme 0.41kg/tds, static reaction 48 hours, saccharification terminal DE value>=98%, DX value>=97%; (7) decolour: adjustment liquid glucose pH value to 4.8, reaches the iso-electric point of protein condenses, and increase activated carbon dosage, soluble protein generation iso-electric point is condensed, become insoluble protein and be tightly held by activated carbon, removing the solid substances such as protein through sheet frame squeeze and filter, reach pure liquid glucose.Activated carbon dosage is 4.2% of liquid glucose butt, stirs after 20 minutes and enters pressure filter, bleaching temperature 76 DEG C, decolour 30 minutes, the liquid glucose specific conductivity≤300us/cm after decolouring, transmittance>=98% in bleacher; (8) ion-exchange demineralization: material step (6) obtained is successively through cation bed-anion bed-cation bed-anion bed-adjustable column, totally three groups of ion exchange columns, carry out ion-exchange, remove impurity in liquid glucose, then liquid glucose enters de-taste post, described de-taste post adopts de-taste resin: Dowex Optipore SD-2, carry out ion-exchange, protein in liquid glucose and calcium ions and magnesium ions are removed, reach purer liquid glucose, flow is 2.5 BV/h, temperature≤55 DEG C, pressure≤2.0kg/cm during operation in first post
2, the specific conductivity≤15us/cm of liquid glucose after ion-exchange, pH value 4.0, transmittance>=98%; (9) evaporate: liquid glucose being concentrated to solid substance is 73%, during well heater work, keep continuity, pressure>=0. 5Mpa that steam is total, liquid glucose DX value > 90; (10) heat gives crystallization: the liquid glucose after evaporation enters flash tank and carries out flash concentration crystallization, produces fine crystals; (11) first time cold crystallization: the sugar concentration 73.5% after thermal crystalline, temperature is 61 ~ 62 DEG C, transmittance > 98, pH value 3.9, direct feeding crystallizer adopts the crystallization of Temperature fall method, crystallizer reserves seed for planting 26%, dense syrup during canful after evaporation and mixeding liquid temperature>=48 DEG C of crystal seed, crystallization total time is 60 hours, the temperature difference≤15 DEG C of crystallizer interlayer coolant water temperature and sugar temperature, and crystallizer mixing speed is 0.7 turn/min; (12) first time crystallization massecuite purging: massecuite after crystallization is delivered to whizzer and carries out purging, control wash water temperature 31 DEG C, wet syrup divides < 13%, isolated mother liquor is outer row all; (13) wet sugared back dissolving: the wet sugar hot deionized water after purging is dissolved to concentration 72%, pH value 6.1, temperature 60 C; (14) second time cold crystallization: the liquid glucose after dissolving is sent into crystallizer, adopt the crystallization of Temperature fall method, crystallizer reserves seed for planting 26%, and crystallization total time is 60 hours, and wherein, growing the grain 12 hours, adopts Temperature fall method, crystallisation by cooling 48 hours; Crystallisation by cooling divides two stages: 28 hours first stage, sugar temperature is dropped to 35 DEG C from 46 DEG C, cooling≤0.4 DEG C per hour, subordinate phase 20 hours, sugar temperature is dropped to 22 DEG C from 35 DEG C, cooling≤0.65 DEG C per hour, the temperature difference≤15 DEG C of crystallizer interlayer coolant water temperature and sugar temperature, crystallizer mixing speed is 0.7 turn/min; (15) second time crystallization massecuite purging: massecuite after second time cold crystallization is delivered to whizzer and carries out purging, controls wash water temperature 31 ~ 32 DEG C, wet syrup divides < 13%, and isolated mother liquor and the liquefier after filtering carry out mixture; (16) oven dry obtains the special crystalline dextrose of finished product: pH value is 6.1, DX value>=99.8%, clarity and color≤0.5#, muriate≤0.0004, vitriol≤0.0008.
The special crystalline dextrose of Sunmorl N 60S obtained according to the method described above, its pH value is 6.1, DX value >=99.8%, clarity and color≤0.5#, muriate≤0.0004, vitriol≤0.0008.
embodiment 3
The preparation method of the special crystalline dextrose of the present embodiment Sunmorl N 60S, comprise the following steps: (1) sizes mixing: with deionized water, corn starch milk is transferred to 19.5 B é, regulate pH to 5.6, add alpha-amylase total amount 0.47kg/tds, pH value of starch milk > 5.0, conductance < 300 us/cm; (2) liquefy: injection temperature 107 DEG C for the first time, maintenance with pressure 15 minutes; Second time injection temperature 138 DEG C, maintenance with pressure 3 minutes, enters laminar flow tank, keeps temperature>=98 DEG C, liquefaction terminal DE value 15%; (3) high temperature filtration: after liquefaction terminates, feed liquid keeps 88 DEG C directly to enter SEDICANTER S 6E bipyramid horizontal spiral separator, carries out separation and removes the macrobead solid substances such as solidifying wadding protein, separating machine feed rate≤25m
3/ h, rotary drum rotating speed 3650 revs/min, spiral and rotating cylinder differential 29.6 revs/min, separating medium temperature 60 C, pH value 6; (4) filter at low temperature: the liquefier after high temperature filtration changes through cold water temperature lowering board and is down to 18 DEG C by 88 DEG C, enter to coagulate wadding tank and be incubated 30 minutes, add food grade kieselguhr filtering medium simultaneously, addition 0.8kg/tds, stir 7 minutes, fine particle albumen and soluble proteins are carried out the solidifying wadding of cold induced proteins, then carry out low temperature sheet frame squeeze and filter, further removal liquid glucose from the solid substance such as protein, reach pure liquefier; (5) prepare burden: be that 75:25 mixes by liquefier and second time crystallization massecuite isolated glucose mother liquid with volume ratio, DE value > 98%; (6) saccharification: pure liquefier is warming up to 61 DEG C, adjust pH to 4.3, enters saccharifying tank and adds compounded saccharifying enzyme 0.43kg/tds, static reaction 48 hours, saccharification terminal DE value>=98%, DX value>=97%; (7) decolour: adjustment liquid glucose pH value to 4.8, reaches the iso-electric point of protein condenses, and increase activated carbon dosage, soluble protein generation iso-electric point is condensed, become insoluble protein and be tightly held by activated carbon, removing the solid substances such as protein through sheet frame squeeze and filter, reach pure liquid glucose.Activated carbon dosage is 4.5% of liquid glucose butt, stirs after 22 minutes and enters pressure filter, bleaching temperature 78 DEG C, decolour 30 minutes, the liquid glucose specific conductivity≤300us/cm after decolouring, transmittance>=98% in bleacher; (8) ion-exchange demineralization: material step (6) obtained is successively through cation bed-anion bed-cation bed-anion bed-adjustable column, totally three groups of ion exchange columns, carry out ion-exchange, remove impurity in liquid glucose, then liquid glucose enters de-taste post, described de-taste post adopts de-taste resin: Dowex Optipore SD-2, carry out ion-exchange, protein in liquid glucose and calcium ions and magnesium ions are removed, reach purer liquid glucose, flow is 2.5 BV/h, temperature≤55 DEG C, pressure≤2.0kg/cm during operation in first post
2, the specific conductivity≤15us/cm of liquid glucose after ion-exchange, pH value 4.0, transmittance>=98%; (9) evaporate: liquid glucose being concentrated to solid substance is 73.2%, during well heater work, keep continuity, pressure>=0. 5Mpa that steam is total, liquid glucose DX value > 90; (10) heat gives crystallization: the liquid glucose after evaporation enters flash tank and carries out flash concentration crystallization, produces fine crystals; (11) first time cold crystallization: the sugar concentration 74% after thermal crystalline, temperature is 61.5 DEG C, transmittance > 98, pH value 4.0, direct feeding crystallizer adopts the crystallization of Temperature fall method, crystallizer reserves seed for planting 28%, dense syrup during canful after evaporation and mixeding liquid temperature>=48 DEG C of crystal seed, crystallization total time is 60 hours, the temperature difference≤15 DEG C of crystallizer interlayer coolant water temperature and sugar temperature, and crystallizer mixing speed is 0.7 turn/min; (12) first time crystallization massecuite purging: massecuite after crystallization is delivered to whizzer and carries out purging, control wash water temperature 31 DEG C, wet syrup divides < 13%, isolated mother liquor is outer row all; (13) wet sugared back dissolving: the wet sugar hot deionized water after purging is dissolved to concentration 72%, pH value 6.3, temperature 60 C; (14) second time cold crystallization: the liquid glucose after dissolving is sent into crystallizer, adopt the crystallization of Temperature fall method, crystallizer reserves seed for planting 28%, and crystallization total time is 60 hours, and wherein, growing the grain 12 hours, adopts Temperature fall method, crystallisation by cooling 48 hours; Crystallisation by cooling divides two stages: 28 hours first stage, sugar temperature is dropped to 35 DEG C from 46 DEG C, cooling≤0.4 DEG C per hour, subordinate phase 20 hours, sugar temperature is dropped to 22 DEG C from 35 DEG C, cooling≤0.65 DEG C per hour, the temperature difference≤15 DEG C of crystallizer interlayer coolant water temperature and sugar temperature, crystallizer mixing speed is 0.7 turn/min; (15) second time crystallization massecuite purging: massecuite after second time cold crystallization is delivered to whizzer and carries out purging, controls wash water temperature 31 DEG C, wet syrup divides < 13%, and isolated mother liquor and the liquefier after filtering carry out mixture; (16) oven dry obtains the special crystalline dextrose of finished product: pH value is 6.3, DX value>=99.8%, clarity and color≤0.5#, muriate≤0.0004, vitriol≤0.0008.
The special crystalline dextrose of Sunmorl N 60S obtained according to the method described above, its pH value is 6.3, DX value >=99.8%, clarity and color≤0.5#, muriate≤0.0004, vitriol≤0.0008.
embodiment 4
The preparation method of the special crystalline dextrose of the present embodiment Sunmorl N 60S, comprise the following steps: (1) sizes mixing: with deionized water, corn starch milk is transferred to 19.8B é, regulate pH to 5.7, add alpha-amylase total amount 0.49kg/tds, pH value of starch milk > 5.0, conductance < 300 us/cm; (2) liquefy: injection temperature 107 DEG C for the first time, maintenance with pressure 16 minutes; Second time injection temperature 139 DEG C, maintenance with pressure 3 minutes, enters laminar flow tank, keeps temperature>=98 DEG C, liquefaction terminal DE value 16%; (3) high temperature filtration: after liquefaction terminates, feed liquid keeps 90 DEG C directly to enter SEDICANTER S 6E bipyramid horizontal spiral separator, carries out separation and removes the macrobead solid substances such as solidifying wadding protein, separating machine feed rate≤25m
3/ h, rotary drum rotating speed 3650 revs/min, spiral and rotating cylinder differential 29.6 revs/min, separating medium temperature 80 DEG C, pH value 8; (4) filter at low temperature: the liquefier after high temperature filtration changes through cold water temperature lowering board and is down to 18 DEG C by 90 DEG C, enter to coagulate wadding tank and be incubated 30 minutes, add food grade kieselguhr filtering medium simultaneously, addition 0.8kg/tds, stir 8 minutes, fine particle albumen and soluble proteins are carried out the solidifying wadding of cold induced proteins, then carry out low temperature sheet frame squeeze and filter, further removal liquid glucose from the solid substance such as protein, reach pure liquefier; (5) prepare burden: be that 75:25 mixes by liquefier and second time crystallization massecuite isolated glucose mother liquid with volume ratio, DE value > 98%; (6) saccharification: pure liquefier is warming up to 61 DEG C, adjust pH to 4.3, enters saccharifying tank and adds compounded saccharifying enzyme 0.43kg/tds, static reaction 48 hours, saccharification terminal DE value>=98%, DX value>=97%; (7) decolour: adjustment liquid glucose pH value to 4.8, reaches the iso-electric point of protein condenses, and increase activated carbon dosage, soluble protein generation iso-electric point is condensed, become insoluble protein and be tightly held by activated carbon, removing the solid substances such as protein through sheet frame squeeze and filter, reach pure liquid glucose.Activated carbon dosage is 4.8% of liquid glucose butt, stirs after 24 minutes and enters pressure filter, bleaching temperature 79 DEG C, decolour 30 minutes, the liquid glucose specific conductivity≤300us/cm after decolouring, transmittance>=98% in bleacher; (8) ion-exchange demineralization: material step (6) obtained is successively through cation bed-anion bed-cation bed-anion bed-adjustable column, totally three groups of ion exchange columns, carry out ion-exchange, remove impurity in liquid glucose, then liquid glucose enters de-taste post, described de-taste post adopts de-taste resin: Dowex Optipore SD-2, carry out ion-exchange, protein in liquid glucose and calcium ions and magnesium ions are removed, reach purer liquid glucose, flow is 2.5 BV/h, temperature≤55 DEG C, pressure≤2.0kg/cm during operation in first post
2, the specific conductivity≤15us/cm of liquid glucose after ion-exchange, pH value 4.1, transmittance>=98%; (9) evaporate: liquid glucose being concentrated to solid substance is 73%, during well heater work, keep continuity, pressure>=0. 5Mpa that steam is total, liquid glucose DX value > 90; (10) heat gives crystallization: the liquid glucose after evaporation enters flash tank and carries out flash concentration crystallization, produces fine crystals; (11) first time cold crystallization: the sugar concentration 74% after thermal crystalline, temperature is 61.5 DEG C, transmittance > 98, pH value 4.0, direct feeding crystallizer adopts the crystallization of Temperature fall method, crystallizer reserves seed for planting 28%, dense syrup during canful after evaporation and mixeding liquid temperature>=48 DEG C of crystal seed, crystallization total time is 60 hours, the temperature difference≤15 DEG C of crystallizer interlayer coolant water temperature and sugar temperature, and crystallizer mixing speed is 0.7 turn/min; (12) first time crystallization massecuite purging: massecuite after crystallization is delivered to whizzer and carries out purging, control wash water temperature 31 DEG C, wet syrup divides < 13%, isolated mother liquor is outer row all; (13) wet sugared back dissolving: the wet sugar hot deionized water after purging is dissolved to concentration 73%, pH value 6.4, temperature 61 DEG C; (14) second time cold crystallization: the liquid glucose after dissolving is sent into crystallizer, adopt the crystallization of Temperature fall method, crystallizer reserves seed for planting 28%, and crystallization total time is 60 hours, and wherein, growing the grain 12 hours, adopts Temperature fall method, crystallisation by cooling 48 hours; Crystallisation by cooling divides two stages: 28 hours first stage, sugar temperature is dropped to 35 DEG C from 46 DEG C, cooling≤0.4 DEG C per hour, subordinate phase 20 hours, sugar temperature is dropped to 22 DEG C from 35 DEG C, cooling≤0.65 DEG C per hour, the temperature difference≤15 DEG C of crystallizer interlayer coolant water temperature and sugar temperature, crystallizer mixing speed is 0.7 turn/min; (15) second time crystallization massecuite purging: massecuite after second time cold crystallization is delivered to whizzer and carries out purging, controls wash water temperature 31 DEG C, wet syrup divides < 13%, and isolated mother liquor and the liquefier after filtering carry out mixture; (16) oven dry obtains the special crystalline dextrose of finished product: pH value is 6.3, DX value>=99.8%, clarity and color≤0.5#, muriate≤0.0004, vitriol≤0.0008.
The special crystalline dextrose of Sunmorl N 60S obtained according to the method described above, its pH value is 6.3, DX value >=99.8%, clarity and color≤0.5#, muriate≤0.0004, vitriol≤0.0008.
embodiment 5
The preparation method of the special crystalline dextrose of the present embodiment Sunmorl N 60S, comprise the following steps: (1) sizes mixing: with deionized water, corn starch milk is transferred to 20 B é, regulate pH to 5.8, add alpha-amylase total amount 0.5kg/tds, pH value of starch milk > 5.0, conductance < 300 us/cm; (2) liquefy: injection temperature 108 DEG C for the first time, maintenance with pressure 18 minutes; Second time injection temperature 140 DEG C, maintenance with pressure 3 minutes, enters laminar flow tank, keeps temperature>=98 DEG C, liquefaction terminal DE value 17%; (3) high temperature filtration: after liquefaction terminates, feed liquid keeps 95 DEG C directly to enter SEDICANTER S 6E bipyramid horizontal spiral separator, carries out separation and removes the macrobead solid substances such as solidifying wadding protein, separating machine feed rate≤25m
3/ h, rotary drum rotating speed 3650 revs/min, spiral and rotating cylinder differential 29.6 revs/min, separating medium temperature 100 DEG C, pH value 9; (4) filter at low temperature: the liquefier after high temperature filtration changes through cold water temperature lowering board and is down to 18 DEG C by 95 DEG C, enter to coagulate wadding tank and be incubated 30 minutes, add food grade kieselguhr filtering medium simultaneously, addition 0.8kg/tds, stir 10 minutes, fine particle albumen and soluble proteins are carried out the solidifying wadding of cold induced proteins, then carry out low temperature sheet frame squeeze and filter, further removal liquid glucose from the solid substance such as protein, reach pure liquefier; (5) prepare burden: be that 75:25 mixes by liquefier and second time crystallization massecuite isolated glucose mother liquid with volume ratio, DE value > 98%; (6) saccharification: pure liquefier is warming up to 62 DEG C, adjust pH to 4.4, enters saccharifying tank and adds compounded saccharifying enzyme 0.45kg/tds, static reaction 48 hours, saccharification terminal DE value>=98%, DX value>=97%; (7) decolour: adjustment liquid glucose pH value to 4.8, reaches the iso-electric point of protein condenses, and increase activated carbon dosage, soluble protein generation iso-electric point is condensed, become insoluble protein and be tightly held by activated carbon, removing the solid substances such as protein through sheet frame squeeze and filter, reach pure liquid glucose.Activated carbon dosage is 5% of liquid glucose butt, stirs after 25 minutes and enters pressure filter, bleaching temperature 80 DEG C, decolour 30 minutes, the liquid glucose specific conductivity≤300us/cm after decolouring, transmittance>=98% in bleacher; (8) ion-exchange demineralization: material step (6) obtained is successively through cation bed-anion bed-cation bed-anion bed-adjustable column, totally three groups of ion exchange columns, carry out ion-exchange, remove impurity in liquid glucose, then liquid glucose enters de-taste post, described de-taste post adopts de-taste resin: Dowex Optipore SD-2, carry out ion-exchange, protein in liquid glucose and calcium ions and magnesium ions are removed, reach purer liquid glucose, flow is 2.5 BV/h, temperature≤55 DEG C, pressure≤2.0kg/cm during operation in first post
2, the specific conductivity≤15us/cm of liquid glucose after ion-exchange, pH value 4.2, transmittance>=98%; (9) evaporate: liquid glucose being concentrated to solid substance is 73.5%, during well heater work, keep continuity, pressure>=0. 5Mpa that steam is total, liquid glucose DX value > 90; (10) heat gives crystallization: the liquid glucose after evaporation enters flash tank and carries out flash concentration crystallization, produces fine crystals; (11) first time cold crystallization: the sugar concentration 75% after thermal crystalline, temperature is 62 DEG C, transmittance > 98, pH value 4.2, direct feeding crystallizer adopts the crystallization of Temperature fall method, crystallizer reserves seed for planting 30%, dense syrup during canful after evaporation and mixeding liquid temperature>=48 DEG C of crystal seed, crystallization total time is 60 hours, the temperature difference≤15 DEG C of crystallizer interlayer coolant water temperature and sugar temperature, and crystallizer mixing speed is 0.7 turn/min; (12) first time crystallization massecuite purging: massecuite after crystallization is delivered to whizzer and carries out purging, control wash water temperature 32 DEG C, wet syrup divides < 13%, isolated mother liquor is outer row all; (13) wet sugared back dissolving: the wet sugar hot deionized water after purging is dissolved to concentration 74%, pH value 6.5, temperature 62 DEG C; (14) second time cold crystallization: the liquid glucose after dissolving is sent into crystallizer, adopt the crystallization of Temperature fall method, crystallizer reserves seed for planting 30%, and crystallization total time is 60 hours, and wherein, growing the grain 12 hours, adopts Temperature fall method, crystallisation by cooling 48 hours; Crystallisation by cooling divides two stages: 28 hours first stage, sugar temperature is dropped to 35 DEG C from 46 DEG C, cooling≤0.4 DEG C per hour, subordinate phase 20 hours, sugar temperature is dropped to 22 DEG C from 35 DEG C, cooling≤0.65 DEG C per hour, the temperature difference≤15 DEG C of crystallizer interlayer coolant water temperature and sugar temperature, crystallizer mixing speed is 0.7 turn/min; (15) second time crystallization massecuite purging: massecuite after second time cold crystallization is delivered to whizzer and carries out purging, controls wash water temperature 32 DEG C, wet syrup divides < 13%, and isolated mother liquor and the liquefier after filtering carry out mixture; (16) oven dry obtains the special crystalline dextrose of finished product: pH value is 6.5, DX value>=99.8%, clarity and color≤0.5#, muriate≤0.0004, vitriol≤0.0008.
The special crystalline dextrose of Sunmorl N 60S obtained according to the method described above, its pH value is 6.5, DX value >=99.8%, clarity and color≤0.5#, muriate≤0.0004, vitriol≤0.0008.
Claims (2)
1. the preparation method of the special crystalline dextrose of Sunmorl N 60S, it is characterized in that comprising the following steps: (1) sizes mixing: with deionized water, corn starch milk is transferred to 19-20 B é, regulate pH to 5.4 ~ 5.8, add alpha-amylase total amount 0.45-0.5kg/tds, pH value of starch milk > 5.0, conductance < 300 us/cm, (2) liquefy: injection temperature 105 ~ 108 DEG C for the first time, maintenance with pressure 12 ~ 18 minutes, second time injection temperature 135 ~ 140 DEG C, maintenance with pressure 2 ~ 3 minutes, enters laminar flow tank, keeps temperature >=98 DEG C, liquefaction terminal DE value 13 ~ 17%, (3) high temperature filtration: after liquefaction terminates, feed liquid keeps 85-95 DEG C and directly enters bipyramid horizontal spiral separator, carry out separation and remove solidifying wadding protein macrobead solid substance, separating machine feed rate≤25m3/h, rotary drum rotating speed 3650 revs/min, spiral and rotating cylinder differential 29.6 revs/min, separating medium temperature 0-100 DEG C, pH value 4-9, (4) filter at low temperature: the liquefier after high temperature filtration changes through cold water temperature lowering board and is down to 18 DEG C by 85 DEG C, enter to coagulate wadding tank and be incubated 30 minutes, add food grade kieselguhr filtering medium simultaneously, addition 0.8kg/tds, stir 5-10 minute, fine particle albumen and soluble proteins are carried out the solidifying wadding of cold induced proteins, then carry out low temperature sheet frame squeeze and filter, protein solid substance in further removal liquid glucose, reaches pure liquefier, (5) prepare burden: be that 75:25 mixes by liquefier and second time crystallization massecuite isolated glucose mother liquid with volume ratio, DE value > 98%, (6) saccharification: the liquid that described step (5) mixes is warming up to 60-62 DEG C, adjust pH, to 4.2-4.4, enters saccharifying tank and adds compounded saccharifying enzyme 0.4-0.45kg/tds, static reaction 48 hours, saccharification terminal DE value >=98%, DX value >=97%, (7) decolour: adjustment liquid glucose pH value to 4.8, reach the iso-electric point of protein condenses, and increase activated carbon dosage, soluble protein generation iso-electric point is condensed, become insoluble protein and be tightly held by activated carbon, protein solid substance is removed through sheet frame squeeze and filter, reach pure liquid glucose, activated carbon dosage is the 4-5% of liquid glucose butt, enter pressure filter stir 18-25 minute in bleacher after, bleaching temperature 75-80 DEG C, decolour 30 minutes, liquid glucose specific conductivity≤300us/cm after decolouring, transmittance >=98%, (8) ion-exchange demineralization: material step (7) obtained is successively through cation bed-anion bed-cation bed-anion bed-adjustable column, totally three groups of ion exchange columns, carry out ion-exchange, remove impurity in liquid glucose, then liquid glucose enters de-taste post, described de-taste post adopts de-taste resin: Dowex Optipore SD-2, carry out ion-exchange, protein in liquid glucose and calcium ions and magnesium ions are removed, reach purer liquid glucose, flow is 2.5 BV/h, temperature≤55 DEG C, pressure≤2.0kg/cm2 during operation in first post, specific conductivity≤the 15us/cm of liquid glucose after ion-exchange, pH value 3.8-4.2, transmittance >=98%, (9) evaporate: liquid glucose being concentrated to solid substance is 72.5 ~ 73.5%, during well heater work, keep continuity, pressure >=0. 5Mpa that steam is total, liquid glucose DX value > 90%, (10) thermal crystalline: the liquid glucose after evaporation enters flash tank and carries out flash concentration crystallization, produces fine crystals, (11) first time cold crystallization: the sugar concentration 73-75% after thermal crystalline, temperature is 60 ~ 62 DEG C, transmittance > 98, pH value 3.8 ~ 4.2, direct feeding crystallizer adopts the crystallization of Temperature fall method, crystallizer reserves seed for planting 25 ~ 30%, dense syrup during canful after evaporation and mixeding liquid temperature >=48 DEG C of crystal seed, crystallization total time is 60 hours, the temperature difference≤15 DEG C of crystallizer interlayer coolant water temperature and sugar temperature, and crystallizer mixing speed is 0.7 turn/min, (12) first time crystallization massecuite purging: massecuite after crystallization is delivered to whizzer and carries out purging, control wash water temperature 30 ~ 32 DEG C, wet syrup divides < 13%, isolated mother liquor is outer row all, (13) wet sugared back dissolving: the wet sugar hot deionized water after purging is dissolved to concentration 72-74%, pH value 6.0-6.5, temperature 60-62 DEG C, (14) second time cold crystallization: the liquid glucose after dissolving is sent into crystallizer, adopt the crystallization of Temperature fall method, crystallizer reserves seed for planting 25 ~ 30%, and crystallization total time is 60 hours, the temperature difference≤15 DEG C of crystallizer interlayer coolant water temperature and sugar temperature, crystallizer mixing speed is 0.7 turn/min, (15) second time crystallization massecuite purging: massecuite after second time cold crystallization is delivered to whizzer and carries out purging, controls wash water temperature 30 ~ 32 DEG C, wet syrup divides < 13%, and isolated mother liquor and the liquefier after filtering carry out mixture, (16) oven dry obtains the special crystalline dextrose of finished product: pH value is 6.0 ~ 6.5, DX value >=99.8%, clarity and color≤0.5#, muriate≤0.0004, vitriol≤0.0008.
2. the preparation method of the special crystalline dextrose of Sunmorl N 60S according to claim 1, is characterized in that: 60 hours crystallization total times in described step (14), and wherein, growing the grain 12 hours, adopts Temperature fall method, crystallisation by cooling 48 hours; Crystallisation by cooling divides two stages: 28 hours first stage, sugar temperature is dropped to 35 DEG C from 46 DEG C, cooling≤0.4 DEG C per hour, and subordinate phase 20 hours, drops to 22 DEG C by sugar temperature from 35 DEG C, cooling≤0.65 DEG C per hour.
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| CN104928405A (en) * | 2015-05-22 | 2015-09-23 | 山东祥瑞药业有限公司 | Technique for extracting glucose from starch saccharified liquid |
| CN105821095A (en) * | 2015-09-14 | 2016-08-03 | 呼伦贝尔东北阜丰生物科技有限公司 | Optimization method for crystallization of glucose |
| CN105483181A (en) * | 2015-12-28 | 2016-04-13 | 河南飞天农业开发股份有限公司 | Preparation method of high-purity glucose |
| CN110835657A (en) * | 2019-11-15 | 2020-02-25 | 河南飞天农业开发股份有限公司 | Production process of low-oligosaccharide edible glucose |
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| FR2791703B1 (en) * | 1999-04-02 | 2001-06-15 | Roquette Freres | PROCESS FOR THE PREPARATION OF A HIGH PURITY ANHYDROUS ALPHA CRYSTALLINE DEXTROSE |
| CN101555508B (en) * | 2009-05-20 | 2012-05-30 | 万福生科(湖南)农业开发股份有限公司 | Method for preparing crystalline dextrose by rice |
| CN102703547B (en) * | 2012-06-14 | 2013-09-25 | 万福生科(湖南)农业开发股份有限公司 | Method for producing glucose bulk drug for injection by using rice |
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