CN104386714B - The method of preparation food-grade sodium pyrosulfite - Google Patents
The method of preparation food-grade sodium pyrosulfite Download PDFInfo
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- CN104386714B CN104386714B CN201410638160.9A CN201410638160A CN104386714B CN 104386714 B CN104386714 B CN 104386714B CN 201410638160 A CN201410638160 A CN 201410638160A CN 104386714 B CN104386714 B CN 104386714B
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Abstract
The present invention discloses a kind of method preparing food-grade sodium pyrosulfite, including: (a) by technical grade sodium pyrosulfite with pure water to mix, stirring intensification sodium pyrosulfite is fully dissolved；B the algal polysaccharides aqueous solution is added among above-mentioned sodium metabisulfite solution by (), the algal polysaccharides aqueous solution is 80%～100% with the volume ratio of above-mentioned sodium metabisulfite solution, stirring at normal temperature, filters；C () adds activated carbon among filtrate, stand 30～50min 70～100 DEG C of insulations；D above-mentioned solution is filtered by (), and concentrate at vacuum 0.06 to 0.09MPa, temperature 80～95 DEG C；E () adds cold water and cools down, filtering for crystallizing drains moisture, is dried, obtains food-grade sodium pyrosulfite.The preparation technology of the present invention is simple, required with low cost, and the product quality level obtained is high.
Description
Technical field
The present invention relates to the preparation method of food-grade sodium pyrosulfite, specifically, the present invention relates to technical grade
Sodium pyrosulfite is the method that food-grade sodium pyrosulfite prepared by raw material.
Background technology
Food additives sodium pyrosulfite is mainly used in food processing making preservative, bleaching agent, raising agent.Outward
See as white or slightly yellow crystalline powder.According to standard GB/T 1893-1998 index: content is (with Na2S2O5
Meter) >=96.0%；Iron content (in terms of Fe) %≤0.005；Content of beary metal (in terms of Pb) %≤0.001；
Arsenic content (in terms of As) %≤0.0002.
Technical grade sodium pyrosulfite, for slightly yellow crystalline powder, can be used as in printing and dyeing, rubber, photosensitive, system
Among the industrial circles such as leather.At present, the preparation method of technical grade sodium pyrosulfite has a following two:
1, sulfur dioxide saturation, is passed through saturated Na by sulfur dioxide2CO3Among solution, make SO2It is saturated,
20 DEG C of solution crystallizes, is filtrated to get sodium pyrosulfite (being shown below):
Na2CO3+2SO2+H2O→2Na2S2O5+CO2
2NaHSO3→2Na2S2O5+H2O
2, sodium hydrogensulfite directly heats and obtains sodium pyrosulfite (seeing following formula):
2NaHSO3→2Na2S2O5+H2O
Technical grade sodium pyrosulfite compares food-grade sodium pyrosulfite, impurity content, especially chloride, iron with
And content of beary metal is too high, human body is had certain toxicity, does not meets food grade standard, accordingly, it would be desirable to industry
Grade sodium pyrosulfite carries out removal of impurities purification etc. and processes, to obtain food-grade sodium pyrosulfite.
Summary of the invention
For problem above, it is desirable to provide a kind of method preparing food-grade sodium pyrosulfite, concrete and
Speech, it is desirable to provide a kind of side preparing food-grade sodium pyrosulfite with technical grade sodium pyrosulfite for raw material
Method.
According to the present invention, it is provided that a kind of method preparing food-grade sodium pyrosulfite, the method includes following step
Rapid:
A technical grade sodium pyrosulfite and pure water are mixed by () with the ratio of≤0.9:1 (quality: volume), stir
Mix and be warming up to 70～100 DEG C sodium pyrosulfite is fully dissolved；
(b) by concentration expressed in percentage by weight be 1～10% the algal polysaccharides aqueous solution add above-mentioned sodium pyrosulfite molten
Among liquid, the algal polysaccharides aqueous solution is 80%～100% with the volume ratio of above-mentioned sodium metabisulfite solution, normal temperature
Stir 20～40 minutes, filter；
(c) add among filtrate 0.4～0.9% (by with the mass ratio of technical grade sodium pyrosulfite in terms of)
Activated carbon, stands 30～50min 70～100 DEG C of insulations；
D above-mentioned solution is filtered by (), and at vacuum-0.06 to-0.09MPa, temperature 80～95 DEG C
Concentrate；
E () adds cold water and cools down, filtering for crystallizing, drains moisture, and is dried at 80～90 DEG C, obtains
Food-grade sodium pyrosulfite.
Further, after step (e), repeat step (d) and (e) at least two to filtration is mother liquid obtained
Secondary, and the food-grade sodium pyrosulfite obtained is merged.
Further, among step (b), the concentration expressed in percentage by weight of the algal polysaccharides aqueous solution is 5%.
Further, among filtrate, the activated carbon that mass ratio is 0.8% with technical grade sodium pyrosulfite is added.
The preparation technology of the food-grade sodium pyrosulfite of the present invention is simple, required with low cost；Use the party's legal system
The product quality level of the food-grade sodium pyrosulfite made is high, it is possible to meet the food service industry need to sodium pyrosulfite
Ask.
Detailed description of the invention
The present invention uses technical grade sodium pyrosulfite to be raw material, removes through Physical Processing and reduces in the raw material of industry
Some harmful substance, finally obtain for the sodium pyrosulfite of field of food.Technical grade sodium pyrosulfite outward appearance
Yellowish, content of beary metal is too high, does not meets food grade standard, the being obtained in that property of method of the application present invention
Energy, the most standard compliant product of impurity content.
The preparation method of food-grade sodium pyrosulfite that the present invention provides, mainly includes following step:
A technical grade sodium pyrosulfite and pure water are mixed by () with the ratio of≤0.9:1 (quality: volume), stir
Mix and be warming up to 70～100 DEG C sodium pyrosulfite is fully dissolved；
(b) by concentration expressed in percentage by weight be 1～10% the algal polysaccharides aqueous solution add above-mentioned sodium pyrosulfite molten
Among liquid, the algal polysaccharides aqueous solution is 80%～100% with the volume ratio of above-mentioned sodium metabisulfite solution, normal temperature
Stir 20～40 minutes, filter；
(c) add among filtrate 0.4～0.9% (by with the mass ratio of technical grade sodium pyrosulfite in terms of)
Activated carbon, stands 30～50min 70～100 DEG C of insulations；
D above-mentioned solution is filtered by (), and at vacuum-0.06 to-0.09MPa, temperature 80～95 DEG C
Concentrate；
E () adds cold water and carries out cold cut, filtering for crystallizing, drain moisture, and be dried at 80～90 DEG C, obtain
Food-grade sodium pyrosulfite.
Preferably, after step (e), repeat step (d) and (e) at least secondary to filtration is mother liquid obtained,
And the food-grade sodium pyrosulfite obtained is merged.
Among the method that the present invention prepares food-grade sodium pyrosulfite, among step (a), technical grade is burnt
Sodium sulfite and the mixed proportion of pure water, so that technical grade sodium pyrosulfite can fully be dissolved as purpose, be somebody's turn to do
Mixed proportion can be≤0.9:1 (technical grade sodium pyrosulfite: pure water (g/ml)).In view of later step
Among concentration, the program such as be dried, the consumption of pure water is unsuitable too much, and therefore, this mixed proportion is preferably 0.4:
1～0.7:1, and most preferably 0.6:1.
Among the method according to the invention, among step (b), the algal polysaccharides aqueous solution is joined work
Among the aqueous solution of industry grade sodium pyrosulfite, preferably to adsorb iron ion.Its concentration expressed in percentage by weight be 1～
10%, find after screening that during concentration expressed in percentage by weight 5%, adsorption effect is best.Algal polysaccharides is that natural algae carries
Taking thing, stereoscopic graticule cavernous structure has the essential characteristic that stable in physicochemical property, flow speed stability and adsorption capacity are big,
Prepare metal affinity adsorbent with it for carrier and pass through chelated metal ions, it is possible to obtain good adsorption effect.
Among the method according to the invention, in the ancestor of step (C), add activated carbon, under high temperature, stand
A period of time, technical grade sodium pyrosulfite is carried out adsorption-edulcoration.Wherein, the consumption of activated carbon, it should to carry
The sodium pyrosulfite of pure acquisition meets food standard, and the yield obtaining food-grade sodium pyrosulfite is unlikely too low
For the purpose of.Among the method for the present invention, the consumption of activated carbon is chosen as, with technical grade pyrosulfurous acid used
The mass ratio of sodium is 0.4～0.9%%, preferably 0.8%.
In sum, the feature of the present invention method for preparing food-grade sodium pyrosulfite is: use marine alga many
Sugar, activated carbon carry out double adsorption-edulcoration to technical grade sodium pyrosulfite, significantly improve refining effect: to work
The consumption of property charcoal carries out preferably so that can reasonable removing impurity, be avoided that again too much sodium pyrosulfite
Loss.
Exemplary embodiment and the comparative example of the present invention will be enumerated herein, in order to more clearly describe the present invention.
Embodiment 1 (adds the algal polysaccharides aqueous solution that concentration expressed in percentage by weight is 5% and activated carbon dosage is 0.8%)
Adding 1000ml pure water among the beaker of 2000ml, stirring is heated, and slowly puts into technical grade Jiao's sulfurous
Acid sodium 800g, is warmed up to 95 DEG C and it is all dissolved, and adds algal polysaccharides adsorption from aqueous solution 30 minutes, sea
The polysaccharides aqueous solution is 90% with the volume ratio of sodium metabisulfite solution.Filter, add 64g (0.8%) activated carbon,
It is incubated 30 minutes at 100 DEG C, uses Filter paper filtering while hot.Finally with about 60ml pure water rinsing filter paper, with filter
Liquid merges.At vacuum-0.07MPa, temperature less than 90 DEG C is concentrated into about 38 times, and cold water cools down, and filters knot
Crystalline substance, drains moisture, obtains finished product 708g at 80 DEG C after being dried.Filter mother liquid obtained 400ml to press again
Upper method is concentrated into about 200ml, and cold cut crystallizes, and filters, is dried to obtain product 76.8g.
Embodiment 2 (add adsorbent 15g/L and activated carbon dosage is 0.8%)
Adding 1000ml pure water among the beaker of 2000ml, stirring is heated, and slowly puts into technical grade Jiao's sulfurous
Acid sodium 800g, is warmed up to 100 DEG C and it is all dissolved, and adds algal polysaccharides adsorption from aqueous solution 40 minutes, sea
The polysaccharides aqueous solution is 80% with the volume ratio of sodium metabisulfite solution.Filter, add 72g (0.9%) activated carbon,
It is incubated 30 minutes at 100 DEG C, uses Filter paper filtering while hot.Finally with about 60ml pure water rinsing filter paper, with filter
Liquid merges.At vacuum-0.06MPa, temperature less than 90 DEG C is concentrated into about 38 times, and cold water cools down, and filters knot
Crystalline substance, drains moisture, obtains finished product 695g at 80 DEG C after being dried.Filter mother liquid obtained 400ml to press again
Upper method is concentrated into about 200ml, and cold cut crystallizes, and filters, is dried to obtain product 69.5g.
Comparison method (recrystallization method is added without the algal polysaccharides aqueous solution and activated carbon)
Adding 1000ml purified water among the beaker of 1500ml, stirring is heated, and slowly puts into technical grade Jiao sub-
Sodium sulphate 800g, is warmed up to 100 DEG C and it is all dissolved, and is incubated 30 minutes, uses Filter paper filtering while hot.?
Rinse filter paper by about 50ml purified water afterwards, merge with filtrate.In vacuum-0.06MPa, temperature less than 90 DEG C
Being concentrated into about 38 times, cold water cools down, and filtering for crystallizing is drained moisture, obtained after being dried at 80 DEG C
Finished product 683g.Filtering mother liquid obtained 400ml and be concentrated into about 200ml by upper method again, cold cut crystallizes, and filters,
It is dried to obtain product 85.6g.
Testing embodiment 1, embodiment 2, the sodium pyrosulfite product of comparative example, the method for inspection is as follows,
Assay sees table 1.
The method of inspection of food-grade sodium pyrosulfite and test stone:
Molysite: this assay method uses GB 3049-82 " the general side that in inorganic chemical product, iron content measures
Luxuriant and rich with fragrance (mouth sieve) the quinoline AAS of method neighbour " method that specifies carries out.With ascorbic acid by sample solution
Ferric ion is reduced into ferrous ion, and when pH2～9, ferrous ion can generate by (mouth sieve) quinoline luxuriant and rich with fragrance with neighbour
Orange red complex compound, under maximum absorption wavelength (510nm), by its absorbance of spectrophotometric determination.
Heavy metal: in weak acidic medium, the heavy metal ion in sample and hydrogen sulfide effect, generate brown color sulphur
Compound precipitates, and compares with standard reference solution, measures its content.Weigh 1 ± 0.01g sample, be dissolved in 5ml water,
Add 2ml hydrochloric acid, water-bath is evaporated to dryness.Adding 5ml water, 1ml hydrochloric acid, re-evaporation is to dry.Add 5ml acetic acid
Solution, 20ml water dissolved residue.It is transferred completely in 50ml colorimetric cylinder.Add 10ml saturated hydrogen sulfide water, dilute
Release to scale, shake up.In the dark place 10min.Aobvious color must not be deeper than standard.Standard is to take 2ml lead
Standard liquid, adds 0.5ml acetic acid solution, 10ml saturated hydrogen sulfide water, is diluted to scale, shakes up.In the dark put
Put 10min.
Table 1: to embodiment 1-2, the assay of the sodium pyrosulfite product of comparative example
| Project | Food-grade sodium pyrosulfite | Embodiment 1 | Embodiment 2 | Comparative example |
| Outward appearance | Colourless or white crystalline powder | White crystalline powder | White crystalline powder | Yellow crystalline powder |
| Molysite | ≤ 0.005% | ≤ 0.005% | ≤ 0.005% | > 0.005% |
| Heavy metal | ≤20ppm | ≤20ppm | ≤20ppm | ≤20ppm |
| Yield | -- | 91.76% | 90.54% | 84.65% |
As shown in Table 1, through inspection, the sodium pyrosulfite product appearance that comparative example obtains is yellow, and molysite contains
Amount > 0.005%, do not meet food grade standard；The burnt sulfurous that embodiment 1,2 according to the inventive method obtains
Acid sodium product, either outward appearance or impurity content all meet food-grade sodium pyrosulfite standard.But by contrast,
The algal polysaccharides aqueous solution that makes concentration expressed in percentage by weight be 5% and the enforcement of activated carbon that activated carbon dosage is 0.8%
Example 1 can obtain food-grade sodium pyrosulfite with higher yield.
In sum, the method according to the invention, it is possible to technical grade sodium pyrosulfite as raw material, through dissolving,
Absorption to iron ion, charcoal absorption removal of impurities, filter, concentrate, cold cut crystallization, the step such as filtration drying,
Final acquisition meets the sodium pyrosulfite of food-grade.
Claims (2)
1. the method preparing food-grade sodium pyrosulfite, the method comprises the following steps:
A technical grade sodium pyrosulfite is mixed with the ratio of 0.8g:1ml by () with pure water, stirring is warming up to 90 DEG C
Sodium pyrosulfite is fully dissolved；
(b) the algal polysaccharides aqueous solution that concentration expressed in percentage by weight is 5% is added above-mentioned sodium metabisulfite solution it
In, the algal polysaccharides aqueous solution is 90% with the volume ratio of above-mentioned sodium metabisulfite solution, stirring at normal temperature 30 minutes,
Filter；
(c) add among filtrate by with the mass ratio of technical grade sodium pyrosulfite in terms of 0.8% activated carbon,
30min is stood 100 DEG C of insulations；
D above-mentioned solution is filtered by (), and concentrate at vacuum-0.07MPa, temperature 90 DEG C；
E () adds cold water and cools down, filtering for crystallizing, drains moisture, and is dried at 80 DEG C, obtains food
Grade sodium pyrosulfite.
The method of preparation food-grade sodium pyrosulfite the most according to claim 1, it is characterised in that: in step
After (e), to filtering mother liquid obtained step (d) and (e) at least secondary of repeating, and the food-grade that will obtain
Sodium pyrosulfite merges.
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