CN104447653A - Production method of glucono-delta-lactone - Google Patents

Production method of glucono-delta-lactone Download PDF

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Publication number
CN104447653A
CN104447653A CN201410618065.2A CN201410618065A CN104447653A CN 104447653 A CN104447653 A CN 104447653A CN 201410618065 A CN201410618065 A CN 201410618065A CN 104447653 A CN104447653 A CN 104447653A
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tank body
pipe
inlet pipe
gluconolactone
gluconic acid
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朱忠良
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D309/00Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings
    • C07D309/16Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member
    • C07D309/28Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
    • C07D309/30Oxygen atoms, e.g. delta-lactones

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)

Abstract

The invention discloses a production method of glucono-delta-lactone. According to the production method disclosed by the invention, special equipment for producing glucono-delta-lactone including a hydrolysis reactor and a primary distillation tower is adopted. The equipment is characterized in that a washing tank is also arranged between the hydrolysis reactor and the primary distillation tower and consists of a tank body, the top part of the tank body is provided with a gas inlet pipe, the lower end of the gas inlet pipe is arranged at the lower part of the tank body, the upper part of the tank body is provided with a gas outlet pipe, the gas outlet pipe is connected with the primary distillation tower, the lower part of the tank body is provided with a water inlet pipe and a water outlet pipe, a horizontal plane in which the water inlet pipe is located is higher than the horizontal plane in which the water outlet pipe is located, one end of the water outlet pipe in the tank body inclines downwards, a sewage pipe is arranged at the bottom of the tank body, and the tank body is provided with a water level gauge. The production method comprises the following steps: after gluconic acid hydrolysate enters a continuous fluid separation device, carrying out continuous ion exchange on the gluconic acid hydrolysate, concentrating by virtue of a reverse osmosis system to obtain a gluconic acid concentrated solution, and carrying out crystallization concentration on the gluconic acid concentrated solution to obtain glucono-delta-lactone. The production method is simple in preparation and high in yield.

Description

A kind of production method of Gluconolactone
Technical field
The present invention relates to a kind of production method of Gluconolactone.
Background technology
The abbreviation of existing Gluconolactone system glucono delta lactone (Glucono-δ-lactone), molecular formula is C6H10O6, molecular weight 178.14, and outward appearance is white crystal or crystalline powder, is slightly soluble in ethanol, very easily water-soluble.Be hydrolyzed slowly under room temperature or lesser temps, along with the rising of temperature, hydrolysis rate is accelerated.Gluconolactone is the foodstuffs without toxicity additive of generally acknowledging in the world at present, and it is widely used in the food industry.
Current is that raw material production Gluconolactone mainly contains following several method with glucose: (1) produces Gluconolactone by gluconate: present method is divided into again microbe fermentation method and air catalytic oxidation method.Air catalytic oxidation method is due to catalyst metal palladium source difficulty, and method for preparing catalyst requires high, is not thus used widely.Microbe transformation method, because transformation efficiency is high, production cost is lower, is easy to carry out suitability for industrialized production, and thus the production method of Gluconolactone all adopts microbe fermentation method at present.(2) enzyme process and electrochemical process: glucose Direct Catalytic Oxidation is become Gluconolactone, this law transformation efficiency is low, reaction controlling difficulty, and the making step of catalyzer is loaded down with trivial details, current this method is only limited to the laboratory study stage, unsuccessful for suitability for industrialized production.
Microbe fermentation method mainly contains calcium salt method and sodium salt method.In calcium salt method, glucose generates gluconic acid through fermentable, then adds calcium carbonate and change into calglucon, and then condensing crystal obtains calglucon crystal, calglucon crystal obtains gluconic acid through acidifying decalcification again, obtains grape acid lactone finally by condensing crystal.This production method has following shortcoming: 1) calglucon solubleness is little, and therefore in fermented liquid, glucose concn can not be too high, otherwise fermented liquid has crystallization; 2) acidifying decalcification needs to use the vitriol oil, and temperature of reaction is up to 100 DEG C, high to equipment requirements; 3) fermented liquid will concentrate through twice, and just can obtain Gluconolactone, energy consumption is high.It is low that these shortcomings cause calcium salt method production Gluconolactone yield, and cost is higher.
Sodium salt method first the gluconic acid that fermentation generates is converted into Sunmorl N 60S, then generate gluconic acid through ion-exchange, and last condensing crystal obtains Gluconolactone.It is low that sodium salt method preferably resolves calglucon solubleness in calcium salt method, and save the steps such as vitriol oil acidifying decalcification, has yield high, low cost and other advantages.Counting bright year academician waits Gluconolactone in CN1049455C patent to produce in fermenting process the pH value adding NaOH control fermented liquid, and the fermentation later stage adds glucose, carries out high sugar-fermenting.Achieve good production effect.But in this patent, just describe detailed fermentation process, follow-up step was just simply with, and what adopt after fermentation is that filter bag is simply degerming, and effect is also bad, serious to the resin stain in ion-exchange step below; Have what be exactly that gluconic acid concentrates employing to be vacuum concentration at 70 DEG C again, energy consumption is high.
Transglucosylase (α-glucosyltanferase).(this fungi preservation is in American Type Culture Collection (ATCC) (ATCC) for Serratiaplymuthica bacterial classification for the bacterial classification used, its standard model number is ATCC15928) culture, the strain fermentation nutrient media components adopted is containing 1 ~ 6% (W/V) sucrose, 0.5 ~ 5% (W/V) corn steep liquor (filtration disgorging), 0.01 ~ 0.4% (W/V) KCl, the nutrition source that stream adds is the yeast extract paste of concentration 1 ~ 7% or the corn steep liquor (filtration disgorging) (nitrogenous source) of concentration 1 ~ 8%, and the sucrose solution of concentration 1 ~ 15%, fed-batch mode can be Continuous Flow and to add or interval stream adds.Following is one group of good parameter index, nutrient media components: 2% (W/V) sucrose, 2% (W/V) corn steep liquor (filtration disgorging), 0.2% (W/V) KCL, Continuous Flow adds or interval stream adds the sucrose solution that concentration is the yeast extract paste of 2 ~ 3% or the corn steep liquor (filtration disgorging) of 2% and 2%.Its processing condition are: available any volume fermentation culture bacterial classification is with proliferative cell, and fermenting process temperature is 25 ~ 35 DEG C, PH5.0 ~ 8.5, stir, in stream Ensure Liquid source, 1 ~ 20 hour inner edge fermentation limit, fermentation time is 8 ~ 24 hours, in logarithmic phase results somatic cells.The solidification process of alpha-glucosyl transferring enzyme or somatic cells comprises: use with kaolin the additive of the clay class being major ingredient as upholder and absorb attached somatic cells, with the whole somatic cells of sodium alginate to embed, again with CaCl 2 solution by shaping for embedded material cured, again with glutaraldehyde process, be cross-linked again, kill viable cell to prepare the harden monitoring of Transglucosylase simultaneously.Saidly can be potter's clay, clay, kaolin etc. for the somatic additive of adhered bacteria.Additive amount can be 2 ~ 30% of fermented liquid, and is good with 6 ~ 9%, and granularity can be 100 ~ 300 orders, and is good with 150 ~ 200 orders.Alpha-glucosyl transferring enzyme or somatic cells immobilization to prepare the specific embodiment of harden monitoring are: (1), additive added in fermented liquid, be fully uniformly mixed adherent cell after, harvested by centrifugation additive and the cell adsorbed thereof, or first obtain cytoplasm by centrifugal for fermented liquid, again additive is added wherein, be fully uniformly mixed adherent cell; (2) material (cell comprising additive and adsorb), by (1) gathered in the crops and sodium alginate mixing, form gel, fully stir.The consumption of sodium alginate is 1 ~ 6% (W/V), and cell embedding amount is 5 ~ 50% (WWC); (3), with particle squeezer, embedded material to be clamp-oned concentration be curing molding in the CaCl 2 of 0.1 ~ 0.8%, and limit squish lip stirs more than 2 hours; (4), suction filtration blots the immobilized enzyme that collection has been cured, with physiological saline or phosphoric acid buffer (PH7.0) washing; (5), by the glutaraldehyde process of this harden monitoring, then exchange, kill viable cell simultaneously, then wash with physiological saline or phosphoric acid buffer, namely cryodrying obtains harden monitoring.
The production method of Gluconolactone mainly contains three kinds: a kind of fermentation of Aspergillus niger glucose by calcium carbonate as neutralizing agent, then condensing crystal generates calglucon, use sulfuric acid and its reaction with precipitated calcium again, through the anion-cation exchange resin removal of impurity, last condensing crystal drying obtains Gluconolactone, and the method yield of this method to calglucon is 62% (in calglucon); Two is that glucose generates calglucon by electrocatalytic method, then lactonizes through sulfuric acid reaction and cation and anion exchange, and last condensing crystal drying obtains Gluconolactone, and this method yield is 45% (with glucose meter); Three is generate Gluconolactone by the method for immobilized cell by glucose one step, and this method yield is 50% (with glucose meter).In above-mentioned three kinds of methods, first method is due to calglucon solubleness less (4%), therefore glucose fermentation concentration can not be too high, at most can only 15%, otherwise fermented liquid has crystallization, in such fermented liquid, glucose concn is too rare, production Gluconolactone cannot be directly used in, first can only generate calglucon, just finally produce Gluconolactone through sulfation regulating YIN and YANG amberlite is esterified again, due to need through two kinds of resins exchange, solution is by extension rate large (about 5 ~ 6 times), when finally concentrating, energy consumption is large, this method calglucon and sulfuric acid reaction need carry out at 100 DEG C of temperature, energy consumption is high, high to equipment requirements, second method needs numerous and diverse step except catalyzer, and its technical process is long, energy consumption is high, and yield is low, the third method is still in the laboratory study stage, also not for industrial production.
CN1155012A discloses a kind of cultivation of preparation method's seed liquor: add in the seed culture medium after sterilizing below by a few ring of aspergillus niger IFFI2230 slant strains picking: 5% glucose, 0.012%MgSO4,0.02%KCl, 0.015%KH 2PO 4,0.08%NH 4H 2PO 4,0.2% peptone and 0.3% extractum carnis, in 30 DEG C, 250rpm shaking table cultivates 24 hours, obtains seed liquor, 2. ferment: in 15 liters of mechanical agitating fermentation tanks, loading is sterilized contains 15% glucose, 0.03%KH 2PO 4, 0.055% urea, 0.015%MgSO 4, the fermentation culture of 0.1%CaCO 3, inoculum size with 10% connects the cultured seed liquor of people, at 32 DEG C, vapour-liquid ratio 1.7 ~ 2.1m 3/m 3.mia, mixing speed is ventilate under 600 ~ 800rpm condition to stirring fermentation, in fermenting process, stream adds 50% NaOH solution to control the PH of fermented liquid between 2.0 ~ 6.5, when fermented liquid residual sugar is 15 ~ 80g/L, adding glucose to total reducing sugar is 400 ~ 450g/L, continue fermentation to residual sugar be 2.0 ~ 2.9g/L maybe cannot stream add NaOH time, terminate fermentation.3. except thalline: put tank sock filtration fermented liquid except thalline; 4. decolour: add 2% gac and boil and decolour.Centrifugation removing gac again; 5. ion-exchange is except sodium ion: destainer: exchange removing sodium ion through 732 Zeo-karbs (Φ 150 × 1000).6. condensing crystal: exchange liquid vacuum concentration to 80 ~ 90% (Gluconolactone meter) at 70 DEG C, proportion 1.4 ~ 1.5, puts into crystallizer tank and add 0.1 ~ 0.2% glucose sugar lactone as crystal seed, stirred crystallization at 48 ~ 54 DEG C of temperature; 7. wash drying: after whizzer centrifugation is put in gained crystallization, add 10 ~ 40% (concentrated solution Gluconate meter) frozen water or a small amount of edible ethanol washing, then dry in 50 DEG C and obtain Gluconolactone.Present method Gluconolactone total recovery is about 60%, and Zinc Gluconate yield is more than 0.1kg/kg Gluconolactone.The inventive method has the advantages that technical process is simple, energy consumption is low, yield is high, can add ZnO, react and can obtain byproduct Zinc Gluconate through condensing crystal drying in the secondary crystal mother liquor of Gluconolactone.
Summary of the invention
The object of the invention is to the production method proposing a kind of Gluconolactone.
For reaching this object, the present invention by the following technical solutions:
A kind of production method of Gluconolactone, it is characterized in that adopting production Gluconolactone specific equipment to comprise hydrolysis kettle and first gold-plating tower, it is characterized in that: between described hydrolysis kettle and primary tower, be also provided with water washing tank, this water washing tank comprises tank body, tank body top is provided with inlet pipe, inlet pipe lower end is positioned at tank body lower part, tank body top is provided with escape pipe, escape pipe is connected with primary tower, tank body lower part is provided with water inlet pipe and rising pipe, water inlet pipe place horizontal plane is higher than rising pipe place horizontal plane, one end that rising pipe is positioned at tank body is downward-sloping, tank base is provided with blow-off pipe, tank body is provided with water level gauge, continuous fluid tripping device is entered after gluconic acid hydrolyzed solution, carry out continuous ionic exchange, concentrate through reverse osmosis system again, obtain gluconic acid concentrated solution, crystallization is concentrated can obtain Gluconolactone.。
Embodiment
Embodiment 1
A kind of production method of Gluconolactone, it is characterized in that adopting production Gluconolactone specific equipment to comprise hydrolysis kettle and first gold-plating tower, it is characterized in that: between described hydrolysis kettle and primary tower, be also provided with water washing tank, this water washing tank comprises tank body, tank body top is provided with inlet pipe, inlet pipe lower end is positioned at tank body lower part, tank body top is provided with escape pipe, escape pipe is connected with primary tower, tank body lower part is provided with water inlet pipe and rising pipe, water inlet pipe place horizontal plane is higher than rising pipe place horizontal plane, one end that rising pipe is positioned at tank body is downward-sloping, tank base is provided with blow-off pipe, tank body is provided with water level gauge, continuous fluid tripping device is entered after gluconic acid hydrolyzed solution, carry out continuous ionic exchange, concentrate through reverse osmosis system again, obtain gluconic acid concentrated solution, crystallization is concentrated can obtain Gluconolactone.
Obviously, the above embodiment of the present invention is only for example of the present invention is clearly described, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all embodiments.And these belong to spirit institute's apparent change of extending out of the present invention or change and are still among protection scope of the present invention.

Claims (1)

1. the production method of a Gluconolactone, it is characterized in that adopting production Gluconolactone specific equipment to comprise hydrolysis kettle and first gold-plating tower, it is characterized in that: between described hydrolysis kettle and primary tower, be also provided with water washing tank, this water washing tank comprises tank body, tank body top is provided with inlet pipe, inlet pipe lower end is positioned at tank body lower part, tank body top is provided with escape pipe, escape pipe is connected with primary tower, tank body lower part is provided with water inlet pipe and rising pipe, water inlet pipe place horizontal plane is higher than rising pipe place horizontal plane, one end that rising pipe is positioned at tank body is downward-sloping, tank base is provided with blow-off pipe, tank body is provided with water level gauge, continuous fluid tripping device is entered after gluconic acid hydrolyzed solution, carry out continuous ionic exchange, concentrate through reverse osmosis system again, obtain gluconic acid concentrated solution, crystallization is concentrated can obtain Gluconolactone.
CN201410618065.2A 2014-11-05 2014-11-05 Production method of glucono-delta-lactone Pending CN104447653A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114105925A (en) * 2021-10-22 2022-03-01 江苏环宇康力科技有限公司 Production process and equipment for preparing glucolactone from sodium gluconate

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114105925A (en) * 2021-10-22 2022-03-01 江苏环宇康力科技有限公司 Production process and equipment for preparing glucolactone from sodium gluconate
CN114105925B (en) * 2021-10-22 2024-04-30 江苏环宇康力科技有限公司 Production process and equipment for preparing gluconolactone from sodium gluconate

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Application publication date: 20150325