CN102367244A - Preparation method of glucolactone - Google Patents
Preparation method of glucolactone Download PDFInfo
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- CN102367244A CN102367244A CN2011103384029A CN201110338402A CN102367244A CN 102367244 A CN102367244 A CN 102367244A CN 2011103384029 A CN2011103384029 A CN 2011103384029A CN 201110338402 A CN201110338402 A CN 201110338402A CN 102367244 A CN102367244 A CN 102367244A
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Abstract
The invention discloses a preparation method of glucolactone. The method comprises the following steps of: dissolving glucose into deionized water to obtain a glucose solution as a raw material, illuminating the glucose solution by using an ultraviolet lamp, additionally providing an air pump in a reaction device to accelerate a mass transferring process, adding hydrogen peroxide in the reaction process, undergoing a catalytic oxidation reaction under a stirring condition at a temperature of 20-60 DEG C for 1-4h and filtering to obtain a glucose acid solution; carrying out reduced-pressure concentration on the glucose acid solution at 70-80 DEG C and concentrating to form 70-90% of crystallization solution; adding seed crystals into a concentrated solution and placing in a crystallization stirrer for crystallization to obtain a glucolactone product. The preparation method of the glucolactone has the advantages of not only shortening the production period and not causing industrial pollution, but also reducing production cost, realizing low energy consumption and high yield and being suitable or industrial production.
Description
Technical field
The invention belongs to the foodstuff additive production field, particularly a kind of method that adopts ultraviolet-hydrogen peroxide method directly to prepare Gluconolactone from glucose solution.
Background technology
Gluconolactone is white crystal or crystalline powder, and is very easily water-soluble, is slightly soluble in ethanol, is dissolved in ether hardly.Slowly hydrolysis generates glucono-in the aqueous solution.Gluconolactone is widely used in the process of foodstuff production and food-processing; Main peptizer as milk proteins and Sunlover 10; Preservation agent in the meat of fish, fowl poultry; The colorant stabilizer of meat product such as luncheon meat and sausage also can be used as the raising agent of cake bread, and it can also be sequestrant, acidic flavoring agent, pH depressant in addition.
Production method of glucolactone mainly contains three kinds at present: a kind of is to be starting raw material with glucose, adopts enzyme process and electrochemical process directly to produce Gluconolactone.But this method transformation efficiency is low, reaction control is comparatively difficult.Another kind is that to adopt calglucon be starting raw material, acidified, press filtration, IX, concentrate, crystallization, separation, dry preparation Gluconolactone.The cycle of this method is longer, and will produce a large amount of trade waste.Also a kind of is to be starting raw material with the Sunmorl N 60S, obtains the product of Gluconolactone through IX, concentrating under reduced pressure, static crystallization, spinning, freeze-day with constant temperature.This method production cycle is long, power consumption is high, production cost is high.
Ultraviolet/hydrogen peroxide method is a kind of novel high-level oxidation technology, and this is to utilize the approach of strong oxidizer and illumination to produce the OH radical of strong oxidation capacity.Because its distinctive, good oxidation susceptibility has obtained paying attention to widely in recent years.Be mainly used in the research of processing, advanced water purifying processing and the desulphurization denitration of nitrogenous waste water from dyestuff.Obtained good effect in these fields.Key of the present invention is to utilize this technology to solve industry and goes up the production problems that Gluconolactone ran into.
Summary of the invention
In order to solve the weak point that exists in the above-mentioned prior art, the object of the present invention is to provide a kind of preparation method of Gluconolactone; This method adopts uv lamp/hydrogen peroxide that glucose is carried out catalyzed oxidation.
The object of the invention is realized through following technical proposals:
A kind of preparation method of Gluconolactone; Comprise following operation steps: be raw material with the glucose solution, adopt uv lamp that glucose solution is shone, stream adds hydrogen peroxide in reaction process; Carry out catalytic oxidation under air and the agitation condition in logical adding; Filter, concentrate, crystallization gets Gluconolactone.
Said glucose solution is glucose to be dissolved in the deionized water to form the mass and size mark be the solution of 0.3～0.6g/ml.
Said uv lamp directly is inserted in the glucose solution, and it is that the uv lamp of 20W～200W shines that every liter of glucose solution adopts power.
It is 1～2 times of glucose mole number that the stream of said hydrogen peroxide adds total amount, and it is 10%～30% of the catalytic oxidation time that stream adds the time.
The temperature of said catalytic oxidation is 20 ℃～60 ℃, and the time of reaction is 1～4h.
Said concentrating is under 70～80 ℃, to carry out concentrating under reduced pressure, and being concentrated into solid content is 70%～90%.
The Gluconolactone crystal seed that adds in the said crystallisation process (being the pure article of Gluconolactone) is 0.1%～0.5% of Gluconolactone theoretical yield (in mass).
Temperature is controlled at 40 ℃～55 ℃ in the said crystallisation process, and crystallization time is 15～30h.
The purpose of said blowing air is in order to accelerate mass transfer process.
The reaction equation of reaction process of the present invention is:
The present invention has following advantage and beneficial effect with respect to prior art: present invention is directed at the problems of the method existence of producing Gluconolactone on the traditional industry, is raw material with glucose; Adopt ultraviolet radiation method synthesis of glucose acid lactone, not only shortened the production cycle, can not cause industrial pollution; And energy consumption is low, has reduced production cost, and productive rate is high; Economic benefit is considerable, is fit to suitability for industrialized production.
Description of drawings
Fig. 1 is the HPLC collection of illustrative plates that adopts the glucono-that the inventive method obtained;
Fig. 2 is the HPLC collection of illustrative plates that adopts the Gluconolactone that the inventive method obtained.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is described in further detail, but embodiment of the present invention is not limited thereto.
Embodiment 1:
In the graduated cylinder of 1L, add 100g glucose, add the deionized water constant volume, obtain glucose solution to 200ml; Be in the glucose solution of uv lamp insertion graduated cylinder of 40W with ventilation pump and power; Graduated cylinder is put into reaction unit, and temperature is set 40 ℃, under bubbling air and agitation condition, carries out catalytic oxidation; To add the 103ml massfraction be 30% hydrogen peroxidase 10 .6 hour to stream in the reaction process, and catalytic oxidation filtered after 2 hours, obtained 280ml glucono-solution.The transformation efficiency that record glucose this moment reaches 99.1%, and as shown in Figure 1, what when 1.801min, go out the peak is the title product glucono-, can know that through quadrature conversion the glucono-selectivity of generation is better, reaches 90%.
Above-mentioned gained glucono-solution is evaporated to solid content under 70 ℃ be 70%; The Gluconolactone crystal seed that adds Gluconolactone Theoretical Mass content 0.25% again; Crystallization 15h in the stirred crystallization machine, 45 ℃ of temperature controls, rotating speed 10 commentaries on classics/min; Obtain Gluconolactone product 79g, yield 87.9%.Products obtained therefrom is carried out HPLC measure, as shown in Figure 2, be the target product Gluconolactone what 1.824min went out the peak, purity is higher.
Embodiment 2:
In the reactor of 30L, add 5kg glucose, add the deionized water constant volume, obtain glucose solution to 16L; The uv lamp that is 40W with ventilation pump and 8 power evenly is inserted in the glucose solution; The reactor temperature is set in 50 ℃, under bubbling air and agitation condition, carries out catalytic oxidation; To add the 2.58L massfraction be 30% hydrogen peroxidase 10 .6 hour to stream in the reaction process, and catalytic oxidation filtered after 3 hours, obtained 18.6L glucono-solution.The transformation efficiency that record glucose this moment reaches 98.3%, and the glucono-selectivity of generation reaches 88.6%.
Above-mentioned gained glucono-solution is evaporated to solid content under 75 ℃ be 80%; The Gluconolactone crystal seed that adds Gluconolactone Theoretical Mass content 0.3% again; Crystallization 25h in the stirred crystallization machine, 50 ℃ of temperature controls, rotating speed 10 commentaries on classics/min; Obtain Gluconolactone product 3.74kg, yield 83.1%.
Embodiment 3:
In the reactor of 200L, add 40kg glucose, add deionized water and be settled to 66L, obtain glucose solution; The uv lamp that is 200W with ventilation pump and 10 power is inserted in the glucose solution; The reactor temperature is set in 60 ℃, under bubbling air and agitation condition, carries out catalytic oxidation; To add the 42L massfraction be 30% hydrogen peroxidase 10 .3 hour to stream in the reaction process, and catalytic oxidation filtered after 1 hour, obtained 103L glucono-solution.The transformation efficiency that record glucose this moment reaches 97.5%, and the glucono-selectivity of generation reaches 88.2%.
Above-mentioned gained glucono-solution is evaporated to solid content under 80 ℃ be 85%; The Gluconolactone crystal seed that adds Gluconolactone Theoretical Mass content 0.1% again; Crystallization 30h in the stirred crystallization machine, 40 ℃ of temperature controls, rotating speed 10 commentaries on classics/min; Obtain Gluconolactone product 29.77kg, yield is 82.8%.
Embodiment 4:
In the reactor of 500L, add 100kg glucose, add deionized water and be settled to 250L, obtain glucose solution; The uv lamp that is 200W with ventilation pump and 33 power is inserted in the glucose solution; The reactor temperature is set in 20 ℃, under bubbling air and agitation condition, carries out catalytic oxidation; To add the 103L massfraction be 30% hydrogen peroxidase 10 .4 hour to stream in the reaction process, and catalytic oxidation filtered after 4 hours, obtained 340L glucono-solution.The transformation efficiency that record glucose this moment reaches 97.8%, and the glucono-selectivity of generation reaches 87.5%.
Above-mentioned gained glucono-solution is evaporated to solid content under 80 ℃ be 90%; The Gluconolactone crystal seed that adds Gluconolactone Theoretical Mass content 0.5% again; Crystallization 15h in the stirred crystallization machine, 55 ℃ of temperature controls, rotating speed 10 commentaries on classics/min; Obtain Gluconolactone product 72.18kg, yield is 80.3%.
The foregoing description is a preferred implementation of the present invention; But embodiment of the present invention is not restricted to the described embodiments; Other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; All should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (8)
1. the preparation method of a Gluconolactone; It is characterized in that comprising following operation steps: be raw material with the glucose solution, adopt uv lamp that glucose solution is shone, stream adds hydrogen peroxide in reaction process; Under bubbling air and agitation condition, carry out catalytic oxidation; Filter, concentrate, crystallization gets Gluconolactone.
2. the preparation method of a kind of Gluconolactone according to claim 1 is characterized in that: said glucose solution is glucose to be dissolved in to form the mass and size mark in the deionized water be the solution of 0.3～0.6g/ml.
3. the preparation method of a kind of Gluconolactone according to claim 1, it is characterized in that: said uv lamp directly is inserted in the glucose solution, and it is that the uv lamp of 20W～200W shines that every liter of glucose solution adopts power.
4. the preparation method of a kind of Gluconolactone according to claim 1 is characterized in that: it is 1～2 times of glucose mole number that the stream of said hydrogen peroxide adds total amount, and it is 10%～30% of the reaction times that stream adds the time.
5. the preparation method of a kind of Gluconolactone according to claim 1, it is characterized in that: the temperature of said catalytic oxidation is 20 ℃～60 ℃, and the time of reaction is 1～4h.
6. the preparation method of a kind of Gluconolactone according to claim 1 is characterized in that: said concentrating is under 70～80 ℃, to carry out concentrating under reduced pressure, and being concentrated into solid content is 70%～90%.
7. the preparation method of a kind of Gluconolactone according to claim 1, it is characterized in that: the Gluconolactone crystal seed that adds in the said crystallisation process is 0.1%～0.5% of a Gluconolactone theoretical yield.
8. the preparation method of a kind of Gluconolactone according to claim 1, it is characterized in that: temperature is controlled at 40 ℃～55 ℃ in the said crystallisation process, and crystallization time is 15～30h.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103651766A (en) * | 2013-12-19 | 2014-03-26 | 陕西师范大学 | Preservative specially used for fresh pomegranate fruit storage |
| CN104447653A (en) * | 2014-11-05 | 2015-03-25 | 朱忠良 | Production method of glucono-delta-lactone |
| CN107739357A (en) * | 2017-11-08 | 2018-02-27 | 湖北中烟工业有限责任公司 | A kind of flavouring essence for tobacco of its preparation of the preparation method and application of glucolactone |
| CN111903919A (en) * | 2020-06-16 | 2020-11-10 | 温州市顶诺食品有限公司 | Beefsteak processing technology |
| CN112028948A (en) * | 2020-07-02 | 2020-12-04 | 浙江晟格生物科技有限公司 | Method for preparing lactobionic acid by using lactose as raw material |
| 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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| US20100075381A1 (en) * | 2007-05-08 | 2010-03-25 | Tetsuya Ito | Method for Producing Glucuronic Acid by Glucuronic Acid Fermentation |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103651766A (en) * | 2013-12-19 | 2014-03-26 | 陕西师范大学 | Preservative specially used for fresh pomegranate fruit storage |
| CN103651766B (en) * | 2013-12-19 | 2015-01-07 | 陕西师范大学 | Preservative specially used for fresh pomegranate fruit storage |
| CN104447653A (en) * | 2014-11-05 | 2015-03-25 | 朱忠良 | Production method of glucono-delta-lactone |
| CN107739357A (en) * | 2017-11-08 | 2018-02-27 | 湖北中烟工业有限责任公司 | A kind of flavouring essence for tobacco of its preparation of the preparation method and application of glucolactone |
| CN107739357B (en) * | 2017-11-08 | 2020-07-10 | 湖北中烟工业有限责任公司 | Preparation method of gluconolactone and tobacco essence prepared by using gluconolactone |
| CN111903919A (en) * | 2020-06-16 | 2020-11-10 | 温州市顶诺食品有限公司 | Beefsteak processing technology |
| CN111903919B (en) * | 2020-06-16 | 2023-04-07 | 温州市顶诺食品有限公司 | Beefsteak processing technology |
| CN112028948A (en) * | 2020-07-02 | 2020-12-04 | 浙江晟格生物科技有限公司 | Method for preparing lactobionic acid by using lactose as raw material |
| 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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