CN103725731A - Crystalline dextrose special for sodium gluconate and preparation method of crystalline dextrose - Google Patents
Crystalline dextrose special for sodium gluconate and preparation method of crystalline dextrose 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 146
- 239000008121 dextrose Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims description 15
- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 title abstract 3
- 229940005574 sodium gluconate Drugs 0.000 title abstract 3
- 235000012207 sodium gluconate Nutrition 0.000 title abstract 3
- 239000000176 sodium gluconate Substances 0.000 title abstract 3
- 238000002425 crystallisation Methods 0.000 claims abstract description 116
- 230000008025 crystallization Effects 0.000 claims abstract description 102
- 238000010926 purge Methods 0.000 claims abstract description 40
- 238000005342 ion exchange Methods 0.000 claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 35
- 238000001914 filtration Methods 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 24
- 238000001704 evaporation Methods 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 22
- 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 28
- 238000001816 cooling Methods 0.000 claims description 28
- 239000007787 solid Substances 0.000 claims description 28
- 239000000126 substance Substances 0.000 claims description 28
- 230000008020 evaporation Effects 0.000 claims description 21
- 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
- 238000002347 injection Methods 0.000 claims description 14
- 239000007924 injection Substances 0.000 claims description 14
- 239000011229 interlayer Substances 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 239000008103 glucose Substances 0.000 claims description 12
- 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
- 238000010521 absorption reaction Methods 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
- 239000003610 charcoal Substances 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 239000008120 corn starch Substances 0.000 claims description 7
- 238000005115 demineralization Methods 0.000 claims description 7
- 230000002328 demineralizing effect Effects 0.000 claims description 7
- 230000005611 electricity Effects 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
- 238000009413 insulation Methods 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
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract description 2
- 239000002253 acid Substances 0.000 abstract description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 abstract 1
- 238000011033 desalting Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 11
- 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
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000035484 reaction time Effects 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
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000000654 additive Substances 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
- 239000012467 final product Substances 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
- 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
- 238000009736 wetting Methods 0.000 description 1
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Abstract
The invention discloses a method for preparing crystalline dextrose special for sodium gluconate. The method comprises the following steps: (1) size mixing; (2) liquefying; (3) high-temperature filtering; (4) low-temperature filtering; (5) batching; (6) saccharifying; (7) discoloring; (8) ion exchange desalting; (9) evaporating; (10) heating and crystallizing; (11) performing primary cold crystallization; (12) performing primary crystallized massecuite purging; (13) wet sugar redissolution; (14) performing secondary cold crystallization; (15) performing secondary crystallized massecuite purging; and (16) drying to obtain the finished crystalline dextrose, wherein the pH value is 6.0-6.5, the DX value is more than or equal to 99.8, the clarity and color value is less than or equal to 0.5#, the chloride content is less than or equal to 0.0004, and the sulfate content is less than or equal to 0.0008. According to the method, the addition amount of acid base in the liquid saccharification process is effectively reduced, and the purity of the crystalline dextrose special for sodium gluconate is greatly improved; the content of dextrose in the saccharified liquid is improved; the pH value of the finished product is improved.
Description
Technical field
The present invention relates to a kind of glucose and preparation method thereof, be specifically related to special-purpose crystalline dextrose of a kind of Sunmorl N 60S and preparation method thereof.
Background technology
Sunmorl N 60S, claims again sodium pentahydyoxycaproate, is the organic acid salt of multihydroxyl that a kind of purposes is extremely wide, at aspects such as medicine, food, water quality stabilizer, steel surface clean-out system, vial scavenger specially, cement additives, has purposes widely.Sunmorl N 60S whole world demand, at 500,000 tons/year, increases the ratio with 3-5% every year, and current production rate and demand differ greatly, and is a kind of product that has bright market prospects.
Sunmorl N 60S is very extensive in industrial purposes, in construction industry, be widely used as concrete admixture (water reducer and retardant), it is a Chaoyang industry, it is large rising industry, China is still in the large-scaled construction period, during a large amount of priority projects is being carried out and is planned-and subways of big and medium-sized cities, Civil Aviation Airport, High-speed Railway Network, southwestern construction of hydropower facilities etc.Its diminishing, plasticising, retarding effect are all very remarkable, can greatly improve concrete workability, reduce slump-loss, improve concrete later strength, as retardant, can make the presetting period extend to several days from several hours and harmless intensity.And applied widely, in pump concrete, Cracking of High Flowing Concrete, mass concrete, high grade concrete, all can apply.As starting material important in concrete, Sunmorl N 60S admixture also has very large development space.
Industrial generally to take the material (such as grain) that contains glucose be raw material, adopts fermentation method first by glucose, to make gluconic acid, and then neutralized by sodium hydroxide, gets final product to obtain Sunmorl N 60S, also can adopt electrolytic process and oxidation to synthesize.It is synthetic that China mostly adopts heterogeneous catalytic oxidation method to produce.
But to restrict Sunmorl N 60S suitability for industrialized production factor also a lot of simultaneously, for example yield low cost is high, vitriol, chloride content exceed standard, heavy metal content exceeds standard etc., the Sunmorl N 60S that production technique makes at present, 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 existing in prior art, special-purpose crystalline dextrose of a kind of Sunmorl N 60S and preparation method thereof is provided, the special-purpose crystalline dextrose of this Sunmorl N 60S is high purity, high pH value, low metal, the crystalline dextrose of subchloride 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 costs.
For achieving the above object, the technical solution used in the present invention is as follows:
The preparation method of the special-purpose crystalline dextrose of a kind of Sunmorl N 60S, comprise the following steps: size mixing (1): 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, electricity is led < 300 us/cm; (2) liquefaction: injection temperature is 105 ~ 108 ℃ for the first time, with pressurely maintains 12 ~ 18 minutes; Injection temperature is 135 ~ 140 ℃ for the second time, with pressurely maintains 2 ~ 3 minutes, enters laminar flow tank, keeps temperature>=98 ℃, liquefaction terminal DE value 13 ~ 17%; (3) high temperature filtration: after liquefaction finishes, feed liquid keeps 85-95 ℃ 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, 3650 revs/min of rotary drum rotating speeds, 29.6 revs/min of spiral and rotating cylinder differentials, separating medium temperature 0-100 ℃, pH value 4-9; (4) filter at low temperature: the liquefier after high temperature filtration changes by 85 ℃ and is down to 18 ℃ through cold water temperature lowering board, enter to coagulate wadding tank insulation 30 minutes, add the agent of food grade diatomite filtration simultaneously, addition 0.8kg/tds, stir 5-10 minute, fine particle albumen and soluble proteins are carried out to the solidifying wadding of cold induced proteins, then carry out low temperature sheet frame squeeze and filter, further remove liquid glucose from the solid substances such as protein, reach pure liquefier; (5) batching: by liquefier and for the second time the isolated glucose mother liquid of crystallization massecuite take volume ratio and mix as 75:25, DE value > 98%; (6) saccharification: pure liquefier is warming up to 60-62 ℃, and 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) decolouring: adjust liquid glucose pH value to 4.8, reach the iso-electric point of protein condenses, and increase activated carbon dosage, make the cohesion of soluble protein generation iso-electric point, become insoluble protein and by charcoal absorption, through sheet frame squeeze and filter, remove the solid substances such as protein, reach pure liquid glucose.Activated carbon dosage is the 4-5% of liquid glucose butt, stirs after 18-25 minute and enter pressure filter in bleacher, and bleaching temperature 75-80 ℃, decolours 30 minutes, the liquid glucose specific conductivity≤300us/cm after decolouring, transmittance>=98%; (8) ion-exchange demineralization: the material that step (6) is 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 to take off 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 ℃, 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) evaporation: it is 72.5～73.5% that liquid glucose is concentrated to solid substance, keeps continuity, pressure>=0. 5Mpa that steam is total, liquid glucose DX value > 90 during well heater work; (10) heat is given crystallization: the liquid glucose after evaporation enters flash tank and carries out flash concentration crystallization, produces fine crystals; (11) cold crystallization for the first time: the sugar concentration 73-75% after thermal crystalline, temperature is 60～62 ℃, transmittance > 98, pH value 3.8～4.2, directly send into crystallizer and adopt the crystallization of nature falling temperature method, crystallizer reserves seed for planting 25～30%, dense syrup during canful after evaporation and mixeding liquid temperature>=48 ℃ of crystal seed, crystallization total time is 60 hours, crystallizer interlayer coolant water temperature and the sugared warm temperature difference≤15 ℃, and crystallizer mixing speed is 0.7 turn/min; (12) crystallization massecuite purging for the first time: massecuite after crystallization is delivered to whizzer and carries out purging, 30 ~ 32 ℃ of control wash water temperature, wet syrup divide < 13%, and isolated mother liquor is outer row all; (13) wet sugared back dissolving: the wet sugar after purging is dissolved to concentration 72-74% with hot deionized water, pH value 6.0-6.5, temperature 60-62 ℃; (14) cold crystallization for the second time: the liquid glucose after dissolving is sent into crystallizer, adopt the crystallization of nature falling temperature method, crystallizer reserves seed for planting 25～30%, and crystallization total time is 60 hours, crystallizer interlayer coolant water temperature and the sugared warm temperature difference≤15 ℃, crystallizer mixing speed is 0.7 turn/min; (15) crystallization massecuite purging for the second time: will be for the second time after cold crystallization massecuite be delivered to whizzer and carry out purging, control 30 ~ 32 ℃ of wash water temperature, wet syrup divides < 13%, isolated mother liquor with filter after liquefier be mixed; (16) dry and obtain the special-purpose 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 nature falling temperature method, crystallisation by cooling 48 hours; Crystallisation by cooling divides two stages: 28 hours first stage, sugar temperature is dropped to 35 ℃ from 46 ℃, and cooling≤0.4 ℃ per hour, subordinate phase 20 hours, drops to 22 ℃, cooling≤0.65 ℃ per hour by sugar temperature from 35 ℃.
The special-purpose crystalline dextrose of Sunmorl N 60S making 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 is controlled and reached high pH value, 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, cold crystallization and for the second time cold crystallization for the first time, and totally three crystallizations, improve the purity of Sunmorl N 60S special use crystalline dextrose greatly; (4) mother liquor of crystallization massecuite purging is all arranged outward for the first time, and the mother liquor of crystallization massecuite purging is used for back joining for the second time, improves the glucose content of saccharified liquid; (5) while wetting sugared back dissolving after purging for the first time, regulate liquid glucose pH value, improve finished product pH value.
Embodiment
embodiment 1
The preparation method of the special-purpose crystalline dextrose of the present embodiment Sunmorl N 60S, comprise the following steps: size mixing (1): 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, electricity is led < 300 us/cm; (2) liquefaction: injection temperature is 105 ℃ for the first time, with pressurely maintains 12 minutes; Injection temperature is 135 ℃ for the second time, with pressurely maintains 2 minutes, enters laminar flow tank, keeps temperature>=98 ℃, liquefaction terminal DE value 13%; (3) high temperature filtration: after liquefaction finishes, feed liquid keeps 85 ℃ and directly enters 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, 3650 revs/min of rotary drum rotating speeds, 29.6 revs/min of spiral and rotating cylinder differentials, 0 ℃ of separating medium temperature, pH value is 4; (4) filter at low temperature: the liquefier after high temperature filtration changes by 85 ℃ and is down to 18 ℃ through cold water temperature lowering board, enter to coagulate wadding tank insulation 30 minutes, add the agent of food grade diatomite filtration simultaneously, addition 0.8kg/tds, stir 5 minutes, fine particle albumen and soluble proteins are carried out to the solidifying wadding of cold induced proteins, then carry out low temperature sheet frame squeeze and filter, further remove liquid glucose from the solid substances such as protein, reach pure liquefier; (5) batching: by liquefier and for the second time the isolated glucose mother liquid of crystallization massecuite take volume ratio and mix as 75:25, DE value > 98%; (6) saccharification: pure liquefier is warming up to 60 ℃, and adjust pH to 4.2, enters saccharifying tank and add compounded saccharifying enzyme 0.4kg/tds, static reaction 48 hours, saccharification terminal DE value>=98%, DX value>=97%; (7) decolouring: adjust liquid glucose pH value to 4.8, reach the iso-electric point of protein condenses, and increase activated carbon dosage, make the cohesion of soluble protein generation iso-electric point, become insoluble protein and by charcoal absorption, through sheet frame squeeze and filter, remove the solid substances such as protein, reach pure liquid glucose.Activated carbon dosage is 4% of liquid glucose butt, stirs after 18 minutes and enter pressure filter in bleacher, and 75 ℃ of bleaching temperatures, decolour 30 minutes, the liquid glucose specific conductivity≤300us/cm after decolouring, transmittance>=98%; (8) ion-exchange demineralization: the material that step (6) is 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 to take off 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 ℃, 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) evaporation: it is 72.5% that liquid glucose is concentrated to solid substance, keeps continuity, pressure>=0. 5Mpa that steam is total, liquid glucose DX value > 90 during well heater work; (10) heat is given crystallization: the liquid glucose after evaporation enters flash tank and carries out flash concentration crystallization, produces fine crystals; (11) cold crystallization for the first time: the sugar concentration 73% after thermal crystalline, temperature is 60 ℃, transmittance > 98, pH value 3.8, directly send into crystallizer and adopt the crystallization of nature falling temperature method, crystallizer reserves seed for planting 25%, dense syrup during canful after evaporation and mixeding liquid temperature>=48 ℃ of crystal seed, crystallization total time is 60 hours, crystallizer interlayer coolant water temperature and the sugared warm temperature difference≤15 ℃, and crystallizer mixing speed is 0.7 turn/min; (12) crystallization massecuite purging for the first time: massecuite after crystallization is delivered to whizzer and carries out purging, 30 ℃ of control wash water temperature, wet syrup divide < 13%, and isolated mother liquor is outer row all; (13) wet sugared back dissolving: the wet sugar after purging is dissolved to concentration 72% with hot deionized water, pH value 6.0, temperature 60 C; (14) cold crystallization for the second time: the liquid glucose after dissolving is sent into crystallizer, adopt the crystallization of nature falling temperature method, crystallizer reserves seed for planting 25%, and crystallization total time is 60 hours, wherein, growing the grain 12 hours, adopts nature falling temperature method, crystallisation by cooling 48 hours; Crystallisation by cooling divides two stages: 28 hours first stage, sugar temperature is dropped to 35 ℃ from 46 ℃, cooling≤0.4 ℃ per hour, subordinate phase 20 hours, sugar temperature is dropped to 22 ℃ from 35 ℃, cooling≤0.65 ℃ per hour, crystallizer interlayer coolant water temperature and the sugared warm temperature difference≤15 ℃, crystallizer mixing speed is 0.7 turn/min; (15) crystallization massecuite purging for the second time: will be for the second time after cold crystallization massecuite be delivered to whizzer and carry out purging, control 30 ℃ of wash water temperature, wet syrup divides < 13%, isolated mother liquor with filter after liquefier be mixed; (16) dry and obtain the special-purpose 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-purpose crystalline dextrose of Sunmorl N 60S making 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-purpose crystalline dextrose of the present embodiment Sunmorl N 60S, comprise the following steps: size mixing (1): 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, electricity is led < 300 us/cm; (2) liquefaction: injection temperature is 106 ℃ for the first time, with pressurely maintains 13 minutes; Injection temperature is 136 ℃ for the second time, with pressurely maintains 2 minutes, enters laminar flow tank, keeps temperature>=98 ℃, liquefaction terminal DE value 14%; (3) high temperature filtration: after liquefaction finishes, feed liquid keeps 86 ℃ and directly enters 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, 3650 revs/min of rotary drum rotating speeds, 29.6 revs/min of spiral and rotating cylinder differentials, separating medium temperature 20-100 ℃, pH value 5; (4) filter at low temperature: the liquefier after high temperature filtration changes by 86 ℃ and is down to 18 ℃ through cold water temperature lowering board, enter to coagulate wadding tank insulation 30 minutes, add the agent of food grade diatomite filtration simultaneously, addition 0.8kg/tds, stir 6 minutes, fine particle albumen and soluble proteins are carried out to the solidifying wadding of cold induced proteins, then carry out low temperature sheet frame squeeze and filter, further remove liquid glucose from the solid substances such as protein, reach pure liquefier; (5) batching: by liquefier and for the second time the isolated glucose mother liquid of crystallization massecuite take volume ratio and mix as 75:25, DE value > 98%; (6) saccharification: pure liquefier is warming up to 61 ℃, and adjust pH to 4.3, enters saccharifying tank and add compounded saccharifying enzyme 0.41kg/tds, static reaction 48 hours, saccharification terminal DE value>=98%, DX value>=97%; (7) decolouring: adjust liquid glucose pH value to 4.8, reach the iso-electric point of protein condenses, and increase activated carbon dosage, make the cohesion of soluble protein generation iso-electric point, become insoluble protein and by charcoal absorption, through sheet frame squeeze and filter, remove the solid substances such as protein, reach pure liquid glucose.Activated carbon dosage is 4.2% of liquid glucose butt, stirs after 20 minutes and enter pressure filter in bleacher, and 76 ℃ of bleaching temperatures, decolour 30 minutes, the liquid glucose specific conductivity≤300us/cm after decolouring, transmittance>=98%; (8) ion-exchange demineralization: the material that step (6) is 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 to take off 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 ℃, 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) evaporation: it is 73% that liquid glucose is concentrated to solid substance, keeps continuity, pressure>=0. 5Mpa that steam is total, liquid glucose DX value > 90 during well heater work; (10) heat is given crystallization: the liquid glucose after evaporation enters flash tank and carries out flash concentration crystallization, produces fine crystals; (11) cold crystallization for the first time: the sugar concentration 73.5% after thermal crystalline, temperature is 61～62 ℃, transmittance > 98, pH value 3.9, directly send into crystallizer and adopt the crystallization of nature falling temperature method, crystallizer reserves seed for planting 26%, dense syrup during canful after evaporation and mixeding liquid temperature>=48 ℃ of crystal seed, crystallization total time is 60 hours, crystallizer interlayer coolant water temperature and the sugared warm temperature difference≤15 ℃, and crystallizer mixing speed is 0.7 turn/min; (12) crystallization massecuite purging for the first time: massecuite after crystallization is delivered to whizzer and carries out purging, 31 ℃ of control wash water temperature, wet syrup divide < 13%, and isolated mother liquor is outer row all; (13) wet sugared back dissolving: the wet sugar after purging is dissolved to concentration 72% with hot deionized water, pH value 6.1, temperature 60 C; (14) cold crystallization for the second time: the liquid glucose after dissolving is sent into crystallizer, adopt the crystallization of nature falling temperature method, crystallizer reserves seed for planting 26%, and crystallization total time is 60 hours, wherein, growing the grain 12 hours, adopts nature falling temperature method, crystallisation by cooling 48 hours; Crystallisation by cooling divides two stages: 28 hours first stage, sugar temperature is dropped to 35 ℃ from 46 ℃, cooling≤0.4 ℃ per hour, subordinate phase 20 hours, sugar temperature is dropped to 22 ℃ from 35 ℃, cooling≤0.65 ℃ per hour, crystallizer interlayer coolant water temperature and the sugared warm temperature difference≤15 ℃, crystallizer mixing speed is 0.7 turn/min; (15) crystallization massecuite purging for the second time: will be for the second time after cold crystallization massecuite be delivered to whizzer and carry out purging, control 31 ~ 32 ℃ of wash water temperature, wet syrup divides < 13%, isolated mother liquor with filter after liquefier be mixed; (16) dry and obtain the special-purpose 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-purpose crystalline dextrose of Sunmorl N 60S making 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-purpose crystalline dextrose of the present embodiment Sunmorl N 60S, comprise the following steps: size mixing (1): 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, electricity is led < 300 us/cm; (2) liquefaction: injection temperature is 107 ℃ for the first time, with pressurely maintains 15 minutes; Injection temperature is 138 ℃ for the second time, with pressurely maintains 3 minutes, enters laminar flow tank, keeps temperature>=98 ℃, liquefaction terminal DE value 15%; (3) high temperature filtration: after liquefaction finishes, feed liquid keeps 88 ℃ and directly enters 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, 3650 revs/min of rotary drum rotating speeds, 29.6 revs/min of spiral and rotating cylinder differentials, separating medium temperature 60 C, pH value 6; (4) filter at low temperature: the liquefier after high temperature filtration changes by 88 ℃ and is down to 18 ℃ through cold water temperature lowering board, enter to coagulate wadding tank insulation 30 minutes, add the agent of food grade diatomite filtration simultaneously, addition 0.8kg/tds, stir 7 minutes, fine particle albumen and soluble proteins are carried out to the solidifying wadding of cold induced proteins, then carry out low temperature sheet frame squeeze and filter, further remove liquid glucose from the solid substances such as protein, reach pure liquefier; (5) batching: by liquefier and for the second time the isolated glucose mother liquid of crystallization massecuite take volume ratio and mix as 75:25, DE value > 98%; (6) saccharification: pure liquefier is warming up to 61 ℃, and adjust pH to 4.3, enters saccharifying tank and add compounded saccharifying enzyme 0.43kg/tds, static reaction 48 hours, saccharification terminal DE value>=98%, DX value>=97%; (7) decolouring: adjust liquid glucose pH value to 4.8, reach the iso-electric point of protein condenses, and increase activated carbon dosage, make the cohesion of soluble protein generation iso-electric point, become insoluble protein and by charcoal absorption, through sheet frame squeeze and filter, remove the solid substances such as protein, reach pure liquid glucose.Activated carbon dosage is 4.5% of liquid glucose butt, stirs after 22 minutes and enter pressure filter in bleacher, and 78 ℃ of bleaching temperatures, decolour 30 minutes, the liquid glucose specific conductivity≤300us/cm after decolouring, transmittance>=98%; (8) ion-exchange demineralization: the material that step (6) is 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 to take off 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 ℃, 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) evaporation: it is 73.2% that liquid glucose is concentrated to solid substance, keeps continuity, pressure>=0. 5Mpa that steam is total, liquid glucose DX value > 90 during well heater work; (10) heat is given crystallization: the liquid glucose after evaporation enters flash tank and carries out flash concentration crystallization, produces fine crystals; (11) cold crystallization for the first time: the sugar concentration 74% after thermal crystalline, temperature is 61.5 ℃, transmittance > 98, pH value 4.0, directly send into crystallizer and adopt the crystallization of nature falling temperature method, crystallizer reserves seed for planting 28%, dense syrup during canful after evaporation and mixeding liquid temperature>=48 ℃ of crystal seed, crystallization total time is 60 hours, crystallizer interlayer coolant water temperature and the sugared warm temperature difference≤15 ℃, and crystallizer mixing speed is 0.7 turn/min; (12) crystallization massecuite purging for the first time: massecuite after crystallization is delivered to whizzer and carries out purging, 31 ℃ of control wash water temperature, wet syrup divide < 13%, and isolated mother liquor is outer row all; (13) wet sugared back dissolving: the wet sugar after purging is dissolved to concentration 72% with hot deionized water, pH value 6.3, temperature 60 C; (14) cold crystallization for the second time: the liquid glucose after dissolving is sent into crystallizer, adopt the crystallization of nature falling temperature method, crystallizer reserves seed for planting 28%, and crystallization total time is 60 hours, wherein, growing the grain 12 hours, adopts nature falling temperature method, crystallisation by cooling 48 hours; Crystallisation by cooling divides two stages: 28 hours first stage, sugar temperature is dropped to 35 ℃ from 46 ℃, cooling≤0.4 ℃ per hour, subordinate phase 20 hours, sugar temperature is dropped to 22 ℃ from 35 ℃, cooling≤0.65 ℃ per hour, crystallizer interlayer coolant water temperature and the sugared warm temperature difference≤15 ℃, crystallizer mixing speed is 0.7 turn/min; (15) crystallization massecuite purging for the second time: will be for the second time after cold crystallization massecuite be delivered to whizzer and carry out purging, control 31 ℃ of wash water temperature, wet syrup divides < 13%, isolated mother liquor with filter after liquefier be mixed; (16) dry and obtain the special-purpose 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-purpose crystalline dextrose of Sunmorl N 60S making 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-purpose crystalline dextrose of the present embodiment Sunmorl N 60S, comprise the following steps: size mixing (1): 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, electricity is led < 300 us/cm; (2) liquefaction: injection temperature is 107 ℃ for the first time, with pressurely maintains 16 minutes; Injection temperature is 139 ℃ for the second time, with pressurely maintains 3 minutes, enters laminar flow tank, keeps temperature>=98 ℃, liquefaction terminal DE value 16%; (3) high temperature filtration: after liquefaction finishes, feed liquid keeps 90 ℃ and directly enters 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, 3650 revs/min of rotary drum rotating speeds, 29.6 revs/min of spiral and rotating cylinder differentials, 80 ℃ of separating medium temperature, pH value 8; (4) filter at low temperature: the liquefier after high temperature filtration changes by 90 ℃ and is down to 18 ℃ through cold water temperature lowering board, enter to coagulate wadding tank insulation 30 minutes, add the agent of food grade diatomite filtration simultaneously, addition 0.8kg/tds, stir 8 minutes, fine particle albumen and soluble proteins are carried out to the solidifying wadding of cold induced proteins, then carry out low temperature sheet frame squeeze and filter, further remove liquid glucose from the solid substances such as protein, reach pure liquefier; (5) batching: by liquefier and for the second time the isolated glucose mother liquid of crystallization massecuite take volume ratio and mix as 75:25, DE value > 98%; (6) saccharification: pure liquefier is warming up to 61 ℃, and adjust pH to 4.3, enters saccharifying tank and add compounded saccharifying enzyme 0.43kg/tds, static reaction 48 hours, saccharification terminal DE value>=98%, DX value>=97%; (7) decolouring: adjust liquid glucose pH value to 4.8, reach the iso-electric point of protein condenses, and increase activated carbon dosage, make the cohesion of soluble protein generation iso-electric point, become insoluble protein and by charcoal absorption, through sheet frame squeeze and filter, remove the solid substances such as protein, reach pure liquid glucose.Activated carbon dosage is 4.8% of liquid glucose butt, stirs after 24 minutes and enter pressure filter in bleacher, and 79 ℃ of bleaching temperatures, decolour 30 minutes, the liquid glucose specific conductivity≤300us/cm after decolouring, transmittance>=98%; (8) ion-exchange demineralization: the material that step (6) is 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 to take off 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 ℃, 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) evaporation: it is 73% that liquid glucose is concentrated to solid substance, keeps continuity, pressure>=0. 5Mpa that steam is total, liquid glucose DX value > 90 during well heater work; (10) heat is given crystallization: the liquid glucose after evaporation enters flash tank and carries out flash concentration crystallization, produces fine crystals; (11) cold crystallization for the first time: the sugar concentration 74% after thermal crystalline, temperature is 61.5 ℃, transmittance > 98, pH value 4.0, directly send into crystallizer and adopt the crystallization of nature falling temperature method, crystallizer reserves seed for planting 28%, dense syrup during canful after evaporation and mixeding liquid temperature>=48 ℃ of crystal seed, crystallization total time is 60 hours, crystallizer interlayer coolant water temperature and the sugared warm temperature difference≤15 ℃, and crystallizer mixing speed is 0.7 turn/min; (12) crystallization massecuite purging for the first time: massecuite after crystallization is delivered to whizzer and carries out purging, 31 ℃ of control wash water temperature, wet syrup divide < 13%, and isolated mother liquor is outer row all; (13) wet sugared back dissolving: the wet sugar after purging is dissolved to concentration 73% with hot deionized water, pH value 6.4,61 ℃ of temperature; (14) cold crystallization for the second time: the liquid glucose after dissolving is sent into crystallizer, adopt the crystallization of nature falling temperature method, crystallizer reserves seed for planting 28%, and crystallization total time is 60 hours, wherein, growing the grain 12 hours, adopts nature falling temperature method, crystallisation by cooling 48 hours; Crystallisation by cooling divides two stages: 28 hours first stage, sugar temperature is dropped to 35 ℃ from 46 ℃, cooling≤0.4 ℃ per hour, subordinate phase 20 hours, sugar temperature is dropped to 22 ℃ from 35 ℃, cooling≤0.65 ℃ per hour, crystallizer interlayer coolant water temperature and the sugared warm temperature difference≤15 ℃, crystallizer mixing speed is 0.7 turn/min; (15) crystallization massecuite purging for the second time: will be for the second time after cold crystallization massecuite be delivered to whizzer and carry out purging, control 31 ℃ of wash water temperature, wet syrup divides < 13%, isolated mother liquor with filter after liquefier be mixed; (16) dry and obtain the special-purpose 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-purpose crystalline dextrose of Sunmorl N 60S making 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-purpose crystalline dextrose of the present embodiment Sunmorl N 60S, comprise the following steps: size mixing (1): 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, electricity is led < 300 us/cm; (2) liquefaction: injection temperature is 108 ℃ for the first time, with pressurely maintains 18 minutes; Injection temperature is 140 ℃ for the second time, with pressurely maintains 3 minutes, enters laminar flow tank, keeps temperature>=98 ℃, liquefaction terminal DE value 17%; (3) high temperature filtration: after liquefaction finishes, feed liquid keeps 95 ℃ and directly enters 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, 3650 revs/min of rotary drum rotating speeds, 29.6 revs/min of spiral and rotating cylinder differentials, 100 ℃ of separating medium temperature, pH value 9; (4) filter at low temperature: the liquefier after high temperature filtration changes by 95 ℃ and is down to 18 ℃ through cold water temperature lowering board, enter to coagulate wadding tank insulation 30 minutes, add the agent of food grade diatomite filtration simultaneously, addition 0.8kg/tds, stir 10 minutes, fine particle albumen and soluble proteins are carried out to the solidifying wadding of cold induced proteins, then carry out low temperature sheet frame squeeze and filter, further remove liquid glucose from the solid substances such as protein, reach pure liquefier; (5) batching: by liquefier and for the second time the isolated glucose mother liquid of crystallization massecuite take volume ratio and mix as 75:25, DE value > 98%; (6) saccharification: pure liquefier is warming up to 62 ℃, and adjust pH to 4.4, enters saccharifying tank and add compounded saccharifying enzyme 0.45kg/tds, static reaction 48 hours, saccharification terminal DE value>=98%, DX value>=97%; (7) decolouring: adjust liquid glucose pH value to 4.8, reach the iso-electric point of protein condenses, and increase activated carbon dosage, make the cohesion of soluble protein generation iso-electric point, become insoluble protein and by charcoal absorption, through sheet frame squeeze and filter, remove the solid substances such as protein, reach pure liquid glucose.Activated carbon dosage is 5% of liquid glucose butt, stirs after 25 minutes and enter pressure filter in bleacher, and 80 ℃ of bleaching temperatures, decolour 30 minutes, the liquid glucose specific conductivity≤300us/cm after decolouring, transmittance>=98%; (8) ion-exchange demineralization: the material that step (6) is 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 to take off 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 ℃, 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) evaporation: it is 73.5% that liquid glucose is concentrated to solid substance, keeps continuity, pressure>=0. 5Mpa that steam is total, liquid glucose DX value > 90 during well heater work; (10) heat is given crystallization: the liquid glucose after evaporation enters flash tank and carries out flash concentration crystallization, produces fine crystals; (11) cold crystallization for the first time: the sugar concentration 75% after thermal crystalline, temperature is 62 ℃, transmittance > 98, pH value 4.2, directly send into crystallizer and adopt the crystallization of nature falling temperature method, crystallizer reserves seed for planting 30%, dense syrup during canful after evaporation and mixeding liquid temperature>=48 ℃ of crystal seed, crystallization total time is 60 hours, crystallizer interlayer coolant water temperature and the sugared warm temperature difference≤15 ℃, and crystallizer mixing speed is 0.7 turn/min; (12) crystallization massecuite purging for the first time: massecuite after crystallization is delivered to whizzer and carries out purging, 32 ℃ of control wash water temperature, wet syrup divide < 13%, and isolated mother liquor is outer row all; (13) wet sugared back dissolving: the wet sugar after purging is dissolved to concentration 74% with hot deionized water, pH value 6.5,62 ℃ of temperature; (14) cold crystallization for the second time: the liquid glucose after dissolving is sent into crystallizer, adopt the crystallization of nature falling temperature method, crystallizer reserves seed for planting 30%, and crystallization total time is 60 hours, wherein, growing the grain 12 hours, adopts nature falling temperature method, crystallisation by cooling 48 hours; Crystallisation by cooling divides two stages: 28 hours first stage, sugar temperature is dropped to 35 ℃ from 46 ℃, cooling≤0.4 ℃ per hour, subordinate phase 20 hours, sugar temperature is dropped to 22 ℃ from 35 ℃, cooling≤0.65 ℃ per hour, crystallizer interlayer coolant water temperature and the sugared warm temperature difference≤15 ℃, crystallizer mixing speed is 0.7 turn/min; (15) crystallization massecuite purging for the second time: will be for the second time after cold crystallization massecuite be delivered to whizzer and carry out purging, control 32 ℃ of wash water temperature, wet syrup divides < 13%, isolated mother liquor with filter after liquefier be mixed; (16) dry and obtain the special-purpose 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-purpose crystalline dextrose of Sunmorl N 60S making 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 (3)
1. the preparation method of the special-purpose crystalline dextrose of a Sunmorl N 60S, it is characterized in that comprising the following steps: size mixing (1): 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, electricity is led < 300 us/cm; (2) liquefaction: injection temperature is 105 ~ 108 ℃ for the first time, with pressurely maintains 12 ~ 18 minutes; Injection temperature is 135 ~ 140 ℃ for the second time, with pressurely maintains 2 ~ 3 minutes, enters laminar flow tank, keeps temperature>=98 ℃, liquefaction terminal DE value 13 ~ 17%; (3) high temperature filtration: after liquefaction finishes, feed liquid keeps 85-95 ℃ 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, 3650 revs/min of rotary drum rotating speeds, 29.6 revs/min of spiral and rotating cylinder differentials, separating medium temperature 0-100 ℃, pH value 4-9; (4) filter at low temperature: the liquefier after high temperature filtration changes by 85 ℃ and is down to 18 ℃ through cold water temperature lowering board, enter to coagulate wadding tank insulation 30 minutes, add the agent of food grade diatomite filtration simultaneously, addition 0.8kg/tds, stir 5-10 minute, fine particle albumen and soluble proteins are carried out to the solidifying wadding of cold induced proteins, then carry out low temperature sheet frame squeeze and filter, further remove liquid glucose from the solid substances such as protein, reach pure liquefier; (5) batching: by liquefier and for the second time the isolated glucose mother liquid of crystallization massecuite take volume ratio and mix as 75:25, DE value > 98%; (6) saccharification: pure liquefier is warming up to 60-62 ℃, and 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) decolouring: adjust liquid glucose pH value to 4.8, reach the iso-electric point of protein condenses, and increase activated carbon dosage, make the cohesion of soluble protein generation iso-electric point, become insoluble protein and by charcoal absorption, through sheet frame squeeze and filter, remove the solid substances such as protein, reach pure liquid glucose, activated carbon dosage is the 4-5% of liquid glucose butt, in bleacher, stir after 18-25 minute and enter pressure filter, bleaching temperature 75-80 ℃, decolours 30 minutes, liquid glucose specific conductivity≤300us/cm after decolouring, transmittance>=98%; (8) ion-exchange demineralization: the material that step (6) is 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 to take off 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 ℃, 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) evaporation: it is 72.5～73.5% that liquid glucose is concentrated to solid substance, keeps continuity, pressure>=0. 5Mpa that steam is total, liquid glucose DX value > 90 during well heater work; (10) heat is given crystallization: the liquid glucose after evaporation enters flash tank and carries out flash concentration crystallization, produces fine crystals; (11) cold crystallization for the first time: the sugar concentration 73-75% after thermal crystalline, temperature is 60～62 ℃, transmittance > 98, pH value 3.8～4.2, directly send into crystallizer and adopt the crystallization of nature falling temperature method, crystallizer reserves seed for planting 25～30%, dense syrup during canful after evaporation and mixeding liquid temperature>=48 ℃ of crystal seed, crystallization total time is 60 hours, crystallizer interlayer coolant water temperature and the sugared warm temperature difference≤15 ℃, and crystallizer mixing speed is 0.7 turn/min; (12) crystallization massecuite purging for the first time: massecuite after crystallization is delivered to whizzer and carries out purging, 30 ~ 32 ℃ of control wash water temperature, wet syrup divide < 13%, and isolated mother liquor is outer row all; (13) wet sugared back dissolving: the wet sugar after purging is dissolved to concentration 72-74% with hot deionized water, pH value 6.0-6.5, temperature 60-62 ℃; (14) cold crystallization for the second time: the liquid glucose after dissolving is sent into crystallizer, adopt the crystallization of nature falling temperature method, crystallizer reserves seed for planting 25～30%, and crystallization total time is 60 hours, crystallizer interlayer coolant water temperature and the sugared warm temperature difference≤15 ℃, crystallizer mixing speed is 0.7 turn/min; (15) crystallization massecuite purging for the second time: will be for the second time after cold crystallization massecuite be delivered to whizzer and carry out purging, control 30 ~ 32 ℃ of wash water temperature, wet syrup divides < 13%, isolated mother liquor with filter after liquefier be mixed; (16) dry and obtain the special-purpose 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-purpose crystalline dextrose of Sunmorl N 60S according to claim 1, is characterized in that: 60 hours described crystallization total times, wherein, growing the grain 12 hours, adopts nature falling temperature method, crystallisation by cooling 48 hours; Crystallisation by cooling divides two stages: 28 hours first stage, sugar temperature is dropped to 35 ℃ from 46 ℃, and cooling≤0.4 ℃ per hour, subordinate phase 20 hours, drops to 22 ℃, cooling≤0.65 ℃ per hour by sugar temperature from 35 ℃.
3. the special-purpose crystalline dextrose of Sunmorl N 60S making according to the preparation method of the special-purpose crystalline dextrose of the arbitrary described Sunmorl N 60S of claim 1 or 2, it is characterized in that: its pH value is 6.0 ~ 6.5, DX value >=99.8%, clarity and color≤0.5#, muriate≤0.0004, vitriol≤0.0008.
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| CN104830918A (en) * | 2015-04-07 | 2015-08-12 | 山东西王糖业有限公司 | Novel production method of sodium gluconate |
| 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 |
| 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 |
| 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 |
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| CN114015734A (en) * | 2021-10-31 | 2022-02-08 | 扬州明增生物科技有限公司 | Glucose separation and purification method |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104830918A (en) * | 2015-04-07 | 2015-08-12 | 山东西王糖业有限公司 | Novel production method of sodium gluconate |
| 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 |
| CN111500794A (en) * | 2020-04-15 | 2020-08-07 | 潍坊盛泰药业有限公司 | Production method of water-containing glucose |
| CN112159829A (en) * | 2020-10-29 | 2021-01-01 | 秦皇岛骊骅淀粉股份有限公司 | Glucose production process |
| CN114015734A (en) * | 2021-10-31 | 2022-02-08 | 扬州明增生物科技有限公司 | Glucose separation and purification method |
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