CN102249893B - Citric acid solution decolorizing method - Google Patents
Citric acid solution decolorizing method Download PDFInfo
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- CN102249893B CN102249893B CN201010583588.XA CN201010583588A CN102249893B CN 102249893 B CN102249893 B CN 102249893B CN 201010583588 A CN201010583588 A CN 201010583588A CN 102249893 B CN102249893 B CN 102249893B
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- citric acid
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- acid solution
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- flocculating agent
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Abstract
The invention belongs to the field of biochemical industry, and in particular relates to a citric acid solution decolorizing method. The method is characterized in that: after citric acid solution is decolorized and treated by a flocculating agent, solution with very ideal transmittance can be obtained. After the method is implemented, the pigment contained in the citric acid solution is effectively reduced; and impurities such as colloidal substances and the like difficultly removed in the citric acid solution are effectively removed by flocculation and utilized, so that the post treatment process is reduced, and the production cost is reduced.
Description
Technical field
The invention belongs to biological chemical field, be specifically related to a kind of citric acid solution decolorizing method.
Background technology
Citric acid is a kind of important organic acid, in industry, grocery trade, cosmetic industry etc., has extremely many purposes.China is as citric acid production big country, and the main fermentation method that adopts is produced citric acid at present, although state of the art is improving constantly, still has problems.
The citric acid fermentation wine with dregs through neutralization, affination, acidolysis, acid take out etc. operation extract after the preliminary citric acid solution that obtains, remove most of albumen, colloid and other impurity although citric acid fermentation wine with dregs premenstruum processes, in rear extraction workshop section, can bring a part into again.At first being neutralizing agent calcium carbonate, is generally technical grade, and its index is as the quality of the meeting remote effect acid hydrolysis solutions such as whiteness, purity; Next is hydrolysis procedure, due to what adopt, is the vitriol oil, and temperature of reaction is higher again, and partial organic substances can in this process, carbonization reaction occur, and directly causes acid hydrolysis solution to darken.Most enterprises adopts to adding gac in acid hydrolysis solution and is decoloured, and then with plate-and-frame filter press, realizes solid-liquid separation.The shortcoming of this method is that decolorizing effect is poor, and the filtered liquid index is unstable, and average colloid protein content is 0.1% (w/w), and average transparence is below 65%.In existing patent, have no the relevant report of citric acid solution decolouring aspect.Therefore, finding a kind of effective citric acid solution decolorizing method is very important to obtain high-quality acid hydrolysis solution
Although disclose a kind for the treatment of process of citric acid mother liquor in patent 200710113693.5, the impurity such as colloid wherein are effectively removed, obtain turbidity preferably, but had essence different from the present invention, can't be applied to the processing of citric acid solution.With citric acid mother liquor, compare, citric acid solution is the feed liquid of un-extracted, and wherein citric acid content is high, if citric acid solution can be handled well before extracting citric acid, later stage will obtain better crystallization solution, improves crystallization yield, obtains better quality product.Therefore, finding a kind of effective citric acid solution decolorizing method is very important to obtain high-quality acid hydrolysis solution.
Summary of the invention
The shortcoming existed for traditional decoloring method, the invention provides a kind of brand-new citric acid solution decolorizing method, the present invention does from source, and the impurity such as the inner albumen that is difficult to removal existed of acid hydrolysis solution, colloidalmaterial are effectively removed and taken full advantage of through throwing out.Thereby greatly alleviate the facility load of subsequent disposal, significantly reduce the production run cost.Its concrete technology step is as follows:
(1). add a certain proportion of decolor flocculating agent and stir in citric acid solution;
(2). above-mentioned mixed solution low rate mixing for some time;
(3). above-mentioned mixed solution is carried out to solid-liquid separation;
(4). isolated flco carries out secondary separation after adding a certain proportion of properties-correcting agent, reclaims residual acid;
(5). the flco after secondary separation is for protein fodder production.
Major impurity in citric acid solution is albumen and colloid, and in the present invention, the contriver adopts decolor flocculating agent to be removed.Commercially available decolor flocculating agent mainly contains poly-sial, polymerized aluminium silicon chloride, chitin-alginic acid copolymer; they contain acyl group, aldehyde radical and carbonyl isoreactivity functional group simultaneously; can play decolouring and throwing out simultaneously; further strengthen decontamination effect improving; and be food grade, can not enter in solution the quality that affects citric acid.Because these several effects are more or less the same, therefore can be optionally a kind of with in them.By the experimental data in table 1, drawn, the ratio of the interpolation of decolor flocculating agent is 0.1-2g/m
3the time can obtain comparatively ideal transparence, the colloid protein content is lower.
The impact on colloid albumen, transparence of table 1 decolor flocculating agent kind and adding proportion
After adding decolor flocculating agent, the room temperature low rate mixing, rotating speed is 50-70rpm, both can prevent the settling of floccus generated, impact is filtered, and can reduce power consumption again.Churning time is too short, and the effect of decolorization flocculation is undesirable; Churning time is long, and power consumption is large, and cost increases; Through test of many times, prove, the Best Times of stirring is 20-30min.
Said mixture is stirred complete, with board-like hermetic filtering machine, carry out solid-liquid separation.This equipment has good filtration effect, and flux is large, and treatment capacity is large, the characteristics that running cost is low.
By in above-mentioned isolated flco, adding flco properties-correcting agent, by filtering separation or settlement separate, make residual acid with the form of solution infiltrate and reclaim turn back in and operation.Main component in flco is colloid albumen, can be used as protein fodder.Determine by test of many times, according to the nonpolar hydrophobic amino acid of the known employing of the experimental data in table 2, as properties-correcting agent, can obtain effect preferably, wherein preferably glycine, L-Ala, α-amino-isovaleric acid, adding proportion is 0.3-1g/m
3.Add the very few hydrophobic effect that makes bad, add too much effect improved not obvious.Because properties-correcting agent is food grade, on citric acid solution without impact.
The impact on residual acid content of table 2 properties-correcting agent and adding proportion thereof
Flco after secondary separation, because its protein content is higher, need mix with sugared slag or the acid sludge of low albumen, and to reduce its protein content, then drying can be made protein fodder, realizes turning waste into wealth.
In sum, technique of the present invention is advanced, controllability is good, the acid hydrolysis solution good transmittance that adopts the present invention to obtain, the solution of its transparence after than activated carbon treatment improves more than 15%, and the colloid protein content is low, greatly reduces the later stage from handing over column load, energy conservation and consumption reduction effects is obvious, has saved production cost.
The accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Embodiment 1:
1, add the poly-sial of decolor flocculating agent and stir in citric acid solution, adding proportion is 0.5g/m
3;
2, above-mentioned mixed solution low rate mixing 25min, rotating speed 50rpm;
3, above-mentioned mixed solution is carried out to solid-liquid separation with board-like hermetic filtering machine;
4, isolated flco carries out filtering separation after adding glycine, reclaims residual acid, and adding proportion is 0.3g/m
3;
5, the flco after secondary separation is for doing protein fodder.
Embodiment 2:
1, add the decolor flocculating agent polymerized aluminium silicon chloride and stir in citric acid solution, adding proportion is 0.1g/m
3;
2, above-mentioned mixed solution low rate mixing 30min, rotating speed 60rpm;
3, above-mentioned mixed solution is carried out to solid-liquid separation with board-like hermetic filtering machine;
4, isolated flco adds after L-Ala and carries out settlement separately, reclaims residual acid, and adding proportion is 0.6g/m
3;
5, the flco after secondary separation is for doing protein fodder.
Embodiment 3:
1, add the decolor flocculating agent chitin-alginic acid copolymer and stir in citric acid solution, adding proportion is 1.0g/m
3;
2, above-mentioned mixed solution low rate mixing 28min, rotating speed 70rpm;
3, above-mentioned mixed solution is carried out to solid-liquid separation with board-like hermetic filtering machine;
4, isolated flco carries out filtering separation after adding α-amino-isovaleric acid, reclaims residual acid, and adding proportion is 1.0g/m
3;
5, the flco after secondary separation is for doing protein fodder.
Embodiment 4:
1, add the decolor flocculating agent polymerized aluminium silicon chloride and stir in citric acid solution, adding proportion is 2.0g/m
3;
2, above-mentioned mixed solution low rate mixing 20min, rotating speed 55rpm;
3, above-mentioned mixed solution is carried out to solid-liquid separation with board-like hermetic filtering machine;
4, isolated flco carries out filtering separation after adding α-amino-isovaleric acid, reclaims residual acid, and adding proportion is 0.8g/m
3;
5, the flco after secondary separation is for doing protein fodder.
Embodiment 5:
1, add the poly-sial of decolor flocculating agent and stir in citric acid solution, adding proportion is 1.5g/m
3;
2, above-mentioned mixed solution low rate mixing 22min, rotating speed 65rpm;
3, above-mentioned mixed solution is carried out to solid-liquid separation with board-like hermetic filtering machine;
4, isolated flco adds after glycine and carries out settlement separately, reclaims residual acid, and adding proportion is 0.4g/m
3;
5, the flco after secondary separation is for doing protein fodder.
Comparative example
Get with isocyatic citric acid solution, adopt respectively traditional technology and technique of the present invention to be processed.
In traditional activated carbon decolorizing technique, need to be warming up to 70-75 ℃ after adding activated carbon, stir 30-40min, so high temperature can shorten ion-exchange resins work-ing life.And the acid hydrolysis solution that adds decolor flocculating agent in technique of the present invention does not need to heat up, stir 20-30min and get final product, flow process is simpler, easy to operate.The average colloid protein content of acid hydrolysis solution after traditional activated carbon treatment is 0.1% (w/w), average transparence is 60%, and decolor flocculating agent is processed rear minimum 0.15 ‰ (w/w) that reach of acid hydrolysis solution colloid protein content, average transparence is more than 70%.The acid hydrolysis solution that decolor flocculating agent was processed, from handing over average multiprocessing 150m of the single cycle of operation of post
3above, it is from handing over column regeneration water unit consumption to reduce 0.2m
3/ t citric acid, sour unit consumption reduces the 3kg/t citric acid, and the alkali unit consumption reduces the 2kg/t citric acid.
Table 3 is the present invention and the contrast of traditional technology average result.
Table 3 the present invention and the contrast of traditional technology average result
| Project | Transparence | Colloid albumen | Turbidity |
| Traditional technology [on average] | ～60％ | ～0.11％ | ～9 |
| The present invention's [on average] | ～70％ | ～0.06％ | ～4 |
Claims (4)
1. a citric acid solution decolorizing method, comprise decolorization flocculation, solid-liquid separation and three workshop sections of flco processing, and it is characterized in that: concrete citric acid solution decolorizing method step is:
(1). add 0.1-2g/m in citric acid solution
3decolor flocculating agent and stir;
(2). above-mentioned mixed solution is with the rotating speed low rate mixing 20-30min of 50-70rpm;
(3). above-mentioned mixed solution is carried out to solid-liquid separation;
(4). isolated flco adds 0.3-1g/m
3properties-correcting agent after carry out secondary separation, reclaim residual acid;
(5). the flco after secondary separation is for doing protein fodder;
A kind of in poly-sial, polymerized aluminium silicon chloride, chitin-alginic acid copolymer of the decolor flocculating agent added in step (1);
Described citric acid solution is that the citric acid fermentation wine with dregs takes out after operation is extracted through neutralization, affination, acidolysis, acid the solution tentatively obtained;
Properties-correcting agent described in step (4) is nonpolar hydrophobic amino acid.
2. treatment process according to claim 1, it is characterized in that: the solid-liquid separating equipment described in step (3) is board-like hermetic filtering machine.
3. treatment process according to claim 1 is characterized in that: described in step (4), be separated into filtering separation or settlement separate.
4. treatment process according to claim 1 is characterized in that: the solution of its transparence of citric acid solution after decolor flocculating agent is processed after than activated carbon treatment improves more than 15%.
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| CN201010583588.XA CN102249893B (en) | 2010-12-13 | 2010-12-13 | Citric acid solution decolorizing method |
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|---|---|---|---|
| CN201010583588.XA CN102249893B (en) | 2010-12-13 | 2010-12-13 | Citric acid solution decolorizing method |
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| CN102249893B true CN102249893B (en) | 2014-01-08 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1151250A (en) * | 1995-12-02 | 1997-06-11 | 杨宇澄 | Method fox extracting thallus protein from waste fermented liquid |
| CN1197038A (en) * | 1998-04-24 | 1998-10-28 | 中国科学院生态环境研究中心 | High effective polymeric aluminium-silicon chloride flocculant and prepn. tech. thereof |
| CN1903741A (en) * | 2006-08-02 | 2007-01-31 | 袁毅桦 | Preparation method of chitin-alginic acid copolymer flocculant |
| CN101182079A (en) * | 2007-11-26 | 2008-05-21 | 日照金禾生化集团有限公司 | Citric acid mother liquor treatment process |
-
2010
- 2010-12-13 CN CN201010583588.XA patent/CN102249893B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1151250A (en) * | 1995-12-02 | 1997-06-11 | 杨宇澄 | Method fox extracting thallus protein from waste fermented liquid |
| CN1197038A (en) * | 1998-04-24 | 1998-10-28 | 中国科学院生态环境研究中心 | High effective polymeric aluminium-silicon chloride flocculant and prepn. tech. thereof |
| CN1903741A (en) * | 2006-08-02 | 2007-01-31 | 袁毅桦 | Preparation method of chitin-alginic acid copolymer flocculant |
| CN101182079A (en) * | 2007-11-26 | 2008-05-21 | 日照金禾生化集团有限公司 | Citric acid mother liquor treatment process |
Non-Patent Citations (2)
| Title |
|---|
| 何宁等.生物絮凝剂的最新研究进展及其应用.《微生物学通报》.2005,第32卷(第2期),104-108. |
| 生物絮凝剂的最新研究进展及其应用;何宁等;《微生物学通报》;20051231;第32卷(第2期);104-108 * |
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