CN103382491B - Preparation method of citric acid - Google Patents
Preparation method of citric acid Download PDFInfo
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- CN103382491B CN103382491B CN201310275841.9A CN201310275841A CN103382491B CN 103382491 B CN103382491 B CN 103382491B CN 201310275841 A CN201310275841 A CN 201310275841A CN 103382491 B CN103382491 B CN 103382491B
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- citric acid
- culture medium
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Abstract
The invention discloses a preparation method of citric acid. The preparation method comprises following steps: a, adding a fermentation medium into a fermentation cylinder, wherein the fermentation medium comprises following ingredients, by weight, 7 to 20% of glucose mother liquor, 0.5 to 3% of soybean protein hydrolysate, 0.2 to 0.4% of MnSO4, and 1 to 10% of (NH)2SO4, with the balance being water; and b, adding a fermentation seed culture medium into the fermentation cylinder, and performing fermentation so as to obtain citric acid. According to the preparation method, glucose which is widely used as a raw material in the citric acid fermentation medium is replaced by glucose mother liquor, little influence on ingredients, performance and efficacy on the citric acid fermentation medium is caused, and the quality of the citric acid prepared by using glucose mother liquor is better than that of the citric acid prepared by using glucose, raw material cost is reduced significantly, by-products produced in corn deep processing processes can be utilized comprehensively and reasonably, environment contaminate and sewage treatment cost are reduced, and sewage treatment pressure of corn comprehensive processing is relived.
Description
Technical field
The present invention relates to a kind of production method of citric acid, belong to corn deep processing field of comprehensive utilization.
Background technology
China is large agricultural country, and agricultural resource enriches, and ultimate production, the commodity amount of main farm produce are all at the forefront in the world, and therefore deep processing of farm products is industry rising greatly.
China's maize sown area and ultimate production are only second to the U.S., occupy second place of the world.Corn is very wide in China's distribution, and south is from the Hainan Island of north latitude 18 degree, and north is to the north of the Heihe of the Heilongjiang Province of north latitude 53 degree, and from the east of Taiwan and maritime provinces, to Xinjiang and Qinghai-Tibet Platean, there is certain area in west.
Starch content in maize kernel reaches more than 70%, has straight chain and amylopectin two type.Respectively have important purposes, W-Gum industry both domestic and external all develops very fast.Starch is the requisite raw materials of industry such as food, medicine, chemical industry.Emerging corn sugar industry is also raw material with W-Gum.The purposes of corn has penetrated into the various piece of industrial or agricultural, and the quality of Maize Production, constitutes tremendous influence to national economy.
Citric acid is a kind of important organic acid, has another name called Citric Acid, clear crystal, and normal containing a part crystal water, odorless, has very strong tart flavour, soluble in water.Its calcium salt is than soluble in hot water in cold water, and this character is commonly used to qualification and separation of citric acid.Control suitable temperature during crystallization and can obtain Citric Acid, usp, Anhydrous Powder.Due to the performance of physicals, chemical property, derivative, be widely used in the most important organic acids of industry such as food, medicine, daily use chemicals.
The citric acid industry of China, enters world market earlier, has become world-class production and big export country through effort for many years and struggle.Citric acid is multiduty organic acid, very well sold and in short supply both at home and abroad at present.In recent years by the impact of various fermentation industry develop rapidly and rising in price of raw materials etc., cause cost increase, therefore anxious new raw material to be developed is to reduce production cost.
In recent years, the enterprise producing citric acid in the world adopts direct fermentation mostly, and citric acid fermentation is produced point fermentation and extracted two portions.
The fermentation of citric acid has solid state fermentation, liquid shallow tray fermentation and submerged fermentation 3 kinds of methods.Solid state fermentation is for raw material with potato dry powder, the starch dregs of rice and amyloid agricultural byproducts.Liquid shallow tray fermentation is raw material mainly with molasses, and its production method proceeds to one by one in fermentation dish by the nutrient solution of sterilizing by pipeline, access bacterial classification.
But still need in the industrial fermentation of citric acid in the face of a lot of problem, what wherein rank first is raw material problem.Our raw material main is at present cassava and corn.The former is still coarse fodder fermentation, and it brings a series of intrinsic defect, as the fluctuation of medium nutrient content; A large amount of impurity not participating in biochemical reaction wastes the energy, and increases many burdens to extraction; Fermented liquid total sugar concentration is on the low side, have impact on fermentation index and plant factor; Fermented liquid filter residue is worth very low, is difficult to comprehensive utilization etc.Maize raw material also can only ferment by half fine fodder at last, in order to adjust nitrogenous source, also a certain proportion of Semen Maydis powder directly will be entered tank.Owing to will pursue liquefaction yield high as far as possible, total sugar concentration also cannot be heightened, and causes our fermentation and acid, rests on lower level so far.The comprehensive utilization of maize raw material is also a large problem, except make use of starch, rest part has all been made cheap feed.So actual according to each factory, selecting the raw material be more suitable for, improve resource utilization, is very urgent problems.
Glucose mother liquid is by production of corn starch engineering of producing crystalline dextrose, isolates the original mother liquor after crystalline dextrose.Because glucose mother liquid is the industrial waste liquid of glucose, cannot recrystallize because its purity is low, impurity is many, can only discharge.But glucose mother liquid concentration is about 70Be, sugar degree is about 86%, and direct discharge obviously can cause the wasting of resources and environmental pollution.
Summary of the invention
The problem to be solved in the present invention is the deficiency for above-mentioned technical problem, provides a kind of and can reduce the raw materials cost of citric acid production further and produce outfit facility investment, can synthetical recovery corn deep processing
In byproduct resource, the production method of the citric acid of energy-conserving and environment-protective.
In order to solve the problem, the present invention by the following technical solutions: a kind of method of producing citric acid, comprises the steps:
A, in fermentor tank, add fermention medium, described fermention medium comprises the material of following weight part: glucose mother liquid 7-20%, soybean protein hydrolyate 5-30 ‰, MnSO
42-4 ‰, (NH)
2sO
41-10%, surplus are water;
B, in above-mentioned fermention medium, access ferment-seeded substratum, carry out fermentation culture and obtain citric acid.
Below further improvement of the present invention:
The volume of the ferment-seeded substratum accessed in step b accounts for the 10%-20% of fermention medium cumulative volume, and leavening temperature is 34-38 DEG C, and fermentation period is 70 hours, and in fermentor tank, the dissolved oxygen amount of unit volume is 20-30%.
Further improvement:
The culturing step of described ferment-seeded substratum is as follows:
(1), seed culture medium is prepared;
(2), aspergillus niger list bacterium colony cultivate, by carry out on dull and stereotyped seed culture medium streak culture go out aspergillus niger list bacterium;
(3), aspergillus niger list bacterium colony activation, activate in picking list colony inoculation to activation medium;
(4), the aspergillus niger after activation is inoculated into inclined-plane seed culture medium and carries out going down to posterity of seed;
(5), treat that spawn culture is good after, with transfering loop scraping bacterial classification, in the pure water after scraping bacterial classification 1-10 ring to sterilizing, then the water containing bacterial classification is poured in the seed culture medium prepared in step (1);
(6), carry out fermentation obtain ferment-seeded substratum by pouring in fermentor tank containing the seed culture medium of aspergillus niger strain in step (5).
Further improvement:
The seed culture medium predominant quantity percentage composition described in culturing step (1) of ferment-seeded substratum is as follows:
Glucose mother liquid: 7-20%;
Soybean protein hydrolyate: 0.45-9 ‰;
MnSO
4：2-4‰；
MgSO
4：1-2‰；
Surplus is water.
Further improvement:
Dull and stereotyped seed culture medium predominant quantity percentage composition described in the culturing step (2) of ferment-seeded substratum is as follows:
Wort: 10-30%;
Soybean protein hydrolyate: 5-30 ‰;
(NH
4)
2SO
4：1-10%；
Agar: 10-25%;
Surplus is water.
Further improvement:
The pH of described dull and stereotyped seed culture medium controls 7.5, and culture temperature controls at 30 DEG C-40 DEG C, and incubation time is 3-10 days.
Further improvement:
The activation medium predominant quantity percentage composition described in culturing step (3) of described ferment-seeded substratum is as follows:
Wort: 10-30%;
MnSO
4：2-4‰；
(NH
4)
2SO
4：1-10%；
Surplus is water.
Further improvement:
The pH of described activation medium controls 7.5, and culture temperature controls at 30 DEG C-40 DEG C, controls incubation time 3-10 days.
Further improvement:
The inclined-plane seed culture medium predominant quantity percentage composition described in culturing step (4) of described ferment-seeded substratum is as follows:
Wort: 10-30%;
(NH
4)
2SO
4：1-10%；
FeCl
2：0.01-0.1‰；
Agar: 10-25%;
Surplus is water.
Further improvement:
The pH of described inclined-plane seed culture medium controls to be 7.5, and culture temperature controls at 30 DEG C-40 DEG C, controls incubation time 3-10 days.
The present invention adopts technique scheme, glucose mother liquid is adopted to be the raw materials of glucose that raw material replaces in known citric acid fermentation substratum, to the composition of lemon fermented substratum, performance, effects etc., almost without any impact, more more have quality guarantee with the citric acid of liquid glucose fermentative production, obviously can reduce raw materials cost, the byproduct resource of corn deep processing process can also be utilized by right combination, reduce environmental pollution and sewage disposal expense, alleviate the pressure of sewage disposal in corn comprehensive process.
embodiment:
Embodiment, a kind of method of producing citric acid, comprises the steps:
1, in fermentor tank, add fermention medium, described fermention medium comprises the material of following weight part: Portugal
Grape sugar mother liquor 7-20%, soybean protein hydrolyate 5-30 ‰, MnSO4 2-4 ‰, (NH)
2sO4 1-10%, surplus are water.
2, in above-mentioned fermention medium, access ferment-seeded substratum, the volume that access ferment-seeded is cultivated accounts for
The 10%-20% of fermention medium cumulative volume, leavening temperature controls at 34-38 DEG C, and fermentation period is 70 hours, and the dissolved oxygen amount in fermentor tank in unit volume controls at 20-30%.
The culturing step of described ferment-seeded substratum is as follows:
1, prepare seed culture medium, the material getting following weight part is mixed to get seed culture medium: glucose mother liquid: 7-20%, soybean protein hydrolyate: 0.45-9 ‰, MnSO
4: 2-4 ‰, MgSO
4: 1-2 ‰, surplus is water, places stand-by by the seed culture medium prepared.
2, aspergillus niger list bacterium colony is cultivated, and aspergillus niger strain needed to activate after long afterwards in storage time, bacterium
The activation of planting mainly is carried out on dull and stereotyped seed culture medium.Described dull and stereotyped seed culture medium is perfect medium, for Aspergillus Niger Growth provides required various trace element and Carbon and nitrogen sources, dull and stereotyped seed culture medium is rule, turns out aspergillus niger list bacterium.
Described dull and stereotyped seed culture medium predominant quantity percentage composition is as follows:
Wort: 10-30%;
Soybean protein hydrolyate: 5-30 ‰;
(NH
4)
2SO
4：1-10%；
Agar: 10-25%;
Surplus is water.
The pH of described dull and stereotyped seed culture medium controls 7.5, and culture temperature controls at 30 DEG C-40 DEG C, and incubation time is 3-10 days.
3, aspergillus niger list bacterium colony activation, activates in picking list colony inoculation to activation medium.Activation medium is except the necessary carbon source providing thalli growth, and nitrogenous source, also provides some to promote the trace element of citric acid production outside trace element.
Described activation medium main component weight percentage is as follows:
Wort: 10-30%;
MnSO
4：2-4‰；
(NH
4)
2SO
4：1-10%；
Surplus is water.
The pH of described activation medium controls 7.5, and culture temperature controls at 30 DEG C-40 DEG C, controls incubation time at 3-10 days.
4, the aspergillus niger after activation is inoculated into inclined-plane seed culture medium.Inclined-plane seed culture medium is perfect medium, and wherein such as, containing organic and inorganic nutrients source, carbon source, nitrogenous source and other micro-nutrients, be mainly used in going down to posterity of seed, stores.Described inclined-plane seed culture medium predominant quantity percentage composition is as follows:
Wort: 10-30%;
(NH
4)
2SO
4：1-10%；
FeCl
2：0.01-0.1‰；
Agar: 10-25%;
Surplus is water.
The pH of described inclined-plane seed culture medium controls 7.5, and culture temperature controls at 30 DEG C-40 DEG C, controls incubation time at 3-10 days.
Cultivated in inclined-plane seed culture medium by bacterial classification well, bacterial classification presents black on substratum, crude sense, there will be the mycelium of white on substratum upper strata.
5, after treating that spawn culture is good, with transfering loop scraping bacterial classification, in the pure water after scraping bacterial classification 1-10 ring to sterilizing, then water is poured in the seed culture medium configured.
Above-mentioned seed culture medium being put into volume is 30m
3vertical digester, simultaneously control temperature is at 30-40 DEG C, and incubation time is 1-4 days, control pH is at 6.5-8.5, aspergillus niger cultivates suitable product acid in seed culture medium, can obtain ferment-seeded substratum, then can be inoculated in fermention medium after acid production rate reaches 1.1-3.1g/dL.
Ferment-seeded cultivates the quantity being mainly used for expanding black-koji mould, makes have enough bacterium to ferment in the fermentation in later stage.Generally, just can be inoculated into fermention medium after cultivating about 20 hours to 30 hours in ferment-seeded substratum, now biomass is all proper with product acid.
Below that the fermention medium production citric acid that the present invention adopts glucose mother liquid to prepare contrasts as follows with the technical indicator of the fermention medium fermentation production of citric acid adopting known employing glucose to prepare:
| Index | The present invention | Known technology |
| Leavening temperature | 34-38℃ | 34-38℃ |
| Fermentation period | 70 hours | 68 hours |
| Access bacterial classification amount | 10-20% | 33% |
| Acid production rate (g/dl) | 13% | 15% |
| Glucose acid invert ratio | 95% | 96% |
Compared with existing known method, citric acid per ton can reduce costs 900 yuan, can increase profit 1,000 ten thousand yuan the whole year.Fully utilized the waste liquor of discharging in glucose production system simultaneously, decreased liquid waste disposal expense, year saves sewage disposal expense 500,000 yuan.The investment construction expense 3,600 ten thousand yuan of liquid sugar production equipment supporting needed for known technology can also be reduced.
Adopt glucose mother liquid of the present invention to be the raw materials of glucose that raw material replaces in known citric acid fermentation substratum, to the composition of lemon fermented substratum, performance, effect etc. are almost without any impact.
Test and rig-site utilization experiment prove after deliberation, owing to remaining a small amount of polysaccharide in glucose mother liquid, when bacterial classification just proceeds to ferment tank, may not too adapt to, and therefore, can observe produce the slower situation of acid in the early stage of fermentation.But in the middle and later periods of fermentation, the generation speed of citric acid can improve slowly, finally also can reach the product acid that other substratum can reach and measure.Can not have a negative impact to the product fermented and net result.
The citric acid product quality of the substratum fermentative production adopting glucose mother liquid of the present invention to prepare is as follows:
Citric acid product:
| Index name | GB | The inventive method |
| Citric acid content (%) | 99.5-101 | 99.6 |
| Clarity | Clarification | Clarification |
| Sample liquid color and luster | Qualified | |
| Moisture | ≤1.0 | 0.5 |
| Readily carbonizable substance (% ,≤) | Be not deeper than standard | Be not deeper than standard |
| Sulphated ash, % ,≤ | 0.07 | 0.05 |
| Vitriol, % ,≤ | 0.02 | 0.011 |
| Calcium salt, % ,≤ | Meet experiment | Meet experiment |
| Iron ,≤ | 0.001% | 0.001% |
Glucose mother liquid of the present invention is adopted to produce the method for citric acid, the byproduct resource of corn deep processing process can be utilized by right combination, reduce environmental pollution and sewage disposal expense, obviously can reduce raw materials cost, reduce support equipment investment, reduce the pressure of sewage disposal in corn comprehensive process, its product is impure few, more more has quality guarantee with the citric acid of liquid glucose fermentative production.
Claims (8)
1. produce a method for citric acid, it is characterized in that: comprise the steps:
A, in fermentor tank, add fermention medium, described fermention medium comprises the material of following weight part: glucose mother liquid 7-20%, soybean protein hydrolyate 5-30 ‰, MnSO
42-4 ‰, (NH
4)
2sO
41-10%, surplus are water;
B, in above-mentioned fermention medium, access ferment-seeded substratum, carry out fermentation culture and obtain citric acid;
The volume of the ferment-seeded substratum accessed in step b accounts for the 10%-20% of fermention medium cumulative volume, and leavening temperature is 34-38 DEG C, and fermentation period is 70 hours, and in fermentor tank, the dissolved oxygen amount of unit volume is 20-30%;
The culturing step of described ferment-seeded substratum is as follows:
(1), seed culture medium is prepared;
(2), aspergillus niger list bacterium colony cultivate, by carry out on dull and stereotyped seed culture medium streak culture go out aspergillus niger list bacterium;
(3), aspergillus niger list bacterium colony activation, activate in picking list colony inoculation to activation medium;
(4), the aspergillus niger after activation is inoculated into inclined-plane seed culture medium and carries out going down to posterity of seed;
(5), treat that spawn culture is good after, with transfering loop scraping bacterial classification, in the pure water after scraping bacterial classification 1-10 ring to sterilizing, then the water containing bacterial classification is poured in the seed culture medium prepared in step (1);
(6), carry out fermentation obtain ferment-seeded substratum by pouring in fermentor tank containing the seed culture medium of aspergillus niger strain in step (5).
2. a kind of method of producing citric acid according to claim 1, is characterized in that: fermentation
The seed culture medium predominant quantity percentage composition described in culturing step (1) of seed culture medium is as follows:
Glucose mother liquid: 7-20%;
Soybean protein hydrolyate: 0.45-9 ‰;
MnSO
4：2-4‰；
MgSO
4：1-2‰；
Surplus is water.
3. a kind of method of producing citric acid according to claim 2, is characterized in that: fermentation kind
Dull and stereotyped seed culture medium predominant quantity percentage composition described in the culturing step (2) of sub-substratum is as follows:
Wort: 10-30%;
Soybean protein hydrolyate: 5-30 ‰;
(NH
4)
2SO
4：1-10%；
Agar: 10-25%;
Surplus is water.
4. a kind of method of producing citric acid according to claim 3, is characterized in that: described flat
The pH of plate seed culture medium controls 7.5, and culture temperature controls at 30 DEG C-40 DEG C, and incubation time is 3-10 days.
5. a kind of method of producing citric acid according to claim 4, is characterized in that: the activation medium predominant quantity percentage composition described in culturing step (3) of described ferment-seeded substratum is as follows:
Wort: 10-30%;
MnSO
4：2-4‰；
(NH
4)
2SO
4：1-10%；
Surplus is water.
6. a kind of method of producing citric acid according to claim 5, it is characterized in that: the pH of described activation medium controls 7.5, culture temperature controls at 30 DEG C-40 DEG C, controls incubation time 3-10 days.
7. a kind of method of producing citric acid according to claim 6, is characterized in that: the inclined-plane seed culture medium predominant quantity percentage composition described in culturing step (4) of described ferment-seeded substratum is as follows:
Wort: 10-30%;
(NH
4)
2SO
4：1-10%；
FeCl
2：0.01-0.1‰；
Agar: 10-25%;
Surplus is water.
8. a kind of method of producing citric acid according to claim 7, is characterized in that: the pH of described inclined-plane seed culture medium controls to be 7.5, and culture temperature controls at 30 DEG C-40 DEG C, controls incubation time 3-10 days.
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|---|---|---|---|
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|---|---|---|---|
| CN201310275841.9A CN103382491B (en) | 2013-07-03 | 2013-07-03 | Preparation method of citric acid |
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| CN103382491B true CN103382491B (en) | 2015-05-20 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104561140B (en) * | 2013-10-23 | 2018-03-06 | 中粮营养健康研究院有限公司 | A kind of method of preparation of citric acid by fermentation |
| CN107221723A (en) * | 2017-05-19 | 2017-09-29 | 合肥尚强电气科技有限公司 | A kind of method that biological fermentation process reclaims lead in lead accumulator |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3622455A (en) * | 1967-12-19 | 1971-11-23 | Mitsui Sugar Co | Process for the production of citric acid by fermentation |
| CN102443611A (en) * | 2010-10-13 | 2012-05-09 | 中粮生物化学（安徽）股份有限公司 | Production method of citric acid |
-
2013
- 2013-07-03 CN CN201310275841.9A patent/CN103382491B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3622455A (en) * | 1967-12-19 | 1971-11-23 | Mitsui Sugar Co | Process for the production of citric acid by fermentation |
| CN102443611A (en) * | 2010-10-13 | 2012-05-09 | 中粮生物化学（安徽）股份有限公司 | Production method of citric acid |
Non-Patent Citations (2)
| Title |
|---|
| 影响葡萄糖母液发酵柠檬酸的因素初探;王岁楼等;《郑州粮食学院学报》;19950330;第16卷(第1期);第46页第1段至第47页第1段，第48页第1段至第4段，表2、6-9 * |
| 葡萄糖母液摇瓶发酵生产柠檬酸;朱亨政等;《微生物学通报》;19840828(第4期);第156页左栏第2-8段，第156页右栏第5段至第158页右栏第1段，表1-4 * |
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