CN103382491A - Preparation method of citric acid - Google Patents
Preparation method of citric acid Download PDFInfo
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- CN103382491A CN103382491A CN2013102758419A CN201310275841A CN103382491A CN 103382491 A CN103382491 A CN 103382491A CN 2013102758419 A CN2013102758419 A CN 2013102758419A CN 201310275841 A CN201310275841 A CN 201310275841A CN 103382491 A CN103382491 A CN 103382491A
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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 and fully utilize the field.
Background technology
China is large agricultural country, and agricultural resource is abundant, and the ultimate production of main farm produce, commodity amount are all at the forefront in the world, so deep processing of farm products is large rising industry.
China's maize sown area and ultimate production are only second to the U.S., occupy the second place of the world.Corn distributes very wide in China, 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, there is certain area in the west to Xinjiang and Qinghai-Tibet Platean.
Starch content in maize kernel reaches more than 70%, and two types of straight chain and amylopectin are arranged.Important purposes is respectively arranged, and 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 take W-Gum as raw material.The purposes of corn has been penetrated into the various piece of industrial or agricultural, and the quality of Maize Production has consisted of tremendous influence to national economy.
Citric acid is a kind of important organic acid, has another name called Citric Acid, and clear crystal often contains a part crystal water, and odorless has very strong tart flavour, and is soluble in water.Than soluble in hot water, this character is commonly used to identify and separation of citric acid its calcium salt in cold water.Control suitable temperature during crystallization and can obtain Citric Acid, usp, Anhydrous Powder.Due to the performance of physicals, chemical property, derivative, be to be widely used in the most important organic acids of industry such as food, medicine, daily use chemicals.
The citric acid industry of China has entered the world market earlier, has become world-class production and big export country through for many years effort and struggle.Citric acid is multiduty organic acid, and is very well sold and in short supply both at home and abroad at present.Be subjected in recent years the impact of various fermentation industry develop rapidlys and rising in price of raw materials etc., cause cost to rise, therefore anxious new raw material to be developed is to reduce production costs.
In recent years, the enterprise that produces in the world citric acid adopts direct fermentation mostly, and citric acid fermentation production divides fermentation and extracts two portions.
The fermentation of citric acid has solid state fermentation, liquid shallow tray fermentation and 3 kinds of methods of submerged fermentation.Solid state fermentation is take potato dry powder, the starch dregs of rice and amyloid agricultural byproducts as raw material.Liquid shallow tray fermentation is raw material mainly with molasses, its production method be will sterilization nutrient solution change over to one by one in the fermentation dish by pipeline, the access bacterial classification.
But, still need in the industrial fermentation of citric acid in the face of a lot of problems, what wherein rank first is the raw material problem.Our present main raw material is cassava and corn.The former is still the coarse fodder fermentation, and it has brought a series of intrinsic defectives, as the fluctuation of medium nutrient content; A large amount of impurity that do not participate in biochemical reaction waste the energy, and give and extract the many burdens of increase; The fermented liquid total sugar concentration is on the low side, has affected fermentation index and plant factor; The fermented liquid filter residue is worth very low, is difficult to comprehensive utilization etc.Maize raw material is half fine fodder fermentation at last also, in order to adjust nitrogenous source, also a certain proportion of Semen Maydis powder directly will be advanced tank.Owing to will pursuing high as far as possible liquefaction yield, total sugar concentration also can't be heightened, and causes our fermentation and acid, rests on so far lower level.The comprehensive utilization of maize raw material is also a large problem, except having utilized starch, rest part has all been made cheap feed.So, actual according to each factory, select the raw material that is more suitable for, improve resource utilization, be urgent problems very.
Glucose mother liquid is by in the 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,, impurity low because of its purity is many can't recrystallize, can only discharge.But glucose mother liquid concentration is the 70Be left and right, and sugar degree is 86% left and right, and directly discharging 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 further reduce the raw materials cost of citric acid production and produce the outfit facility investment, can comprehensively reclaim corn deep processing
In the byproduct resource, the production method of the citric acid of energy-conserving and environment-protective.
In order to address the above problem, the present invention by the following technical solutions: a kind of method of producing citric acid comprises the steps:
A, add fermention medium in fermentor tank, 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 that accesses in step b accounts for the 10%-20% of fermention medium cumulative volume, and leavening temperature is 34-38 ℃, and fermentation period is 70 hours, and in fermentor tank, the dissolved oxygen amount of unit volume is 20-30%.
Further improve:
The culturing step of described ferment-seeded substratum is as follows:
(1), preparation seed culture medium;
(2), aspergillus niger list bacterium colony cultivates, by carry out the streak culture aspergillus niger list bacterium that goes out on dull and stereotyped seed culture medium;
(3), aspergillus niger list bacterium colony activation, picking list colony inoculation activates in activation medium;
(4), the aspergillus niger after activating is inoculated into the 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, scraping bacterial classification 1-10 encircles in pure water after sterilization, the water that then will contain bacterial classification is poured in the seed culture medium for preparing in step (1);
(6), the seed culture medium that contains aspergillus niger strain in step (5) is poured into to ferment in fermentor tank obtain the ferment-seeded substratum.
Further improve:
Seed culture medium predominant quantity percentage composition described in the culturing step of ferment-seeded substratum (1) 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 improve:
Dull and stereotyped seed culture medium predominant quantity percentage composition described in the culturing step of ferment-seeded substratum (2) is as follows:
Wort: 10-30%;
Soybean protein hydrolyate: 5-30 ‰;
(NH
4)
2SO
4：1-10%；
Agar: 10-25%;
Surplus is water.
Further improve:
The pH of described dull and stereotyped seed culture medium is controlled at 7.5, and culture temperature is controlled at 30 ℃-40 ℃, and incubation time is 3-10 days.
Further improve:
Activation medium predominant quantity percentage composition described in the culturing step of described ferment-seeded substratum (3) is as follows:
Wort: 10-30%;
MnSO
4：2-4‰；
(NH
4)
2SO
4：1-10%；
Surplus is water.
Further improve:
The pH of described activation medium is controlled at 7.5, and culture temperature is controlled at 30 ℃-40 ℃, controls incubation time 3-10 days.
Further improve:
Inclined-plane seed culture medium predominant quantity percentage composition described in the culturing step of described ferment-seeded substratum (4) 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 improve:
The pH of described inclined-plane seed culture medium is controlled to be 7.5, and culture temperature is controlled at 30 ℃-40 ℃, controls incubation time 3-10 days.
The present invention adopts technique scheme, adopting glucose mother liquid is that raw material replaces the raw materials of glucose in known citric acid fermentation substratum, composition to lemon fermented substratum, performance, effect etc. be almost without any impact, with the citric acid of liquid glucose fermentative production, the quality guarantee arranged more more, can obviously reduce raw materials cost, the byproduct resource of corn deep processing process can also rationally be fully utilized, environmental contamination reduction and sewage disposal expense, the pressure of sewage disposal in the comprehensive process of alleviation corn.
Embodiment:
Embodiment, a kind of method of producing citric acid comprises the steps:
1, add fermention medium in fermentor tank, described fermention medium comprises the material of following weight part: the Portugal
Grape sugar mother liquor 7-20%, soybean protein hydrolyate 5-30 ‰, MnSO4 2-4 ‰, (NH)
2SO4 1-10%, surplus are water.
2, access ferment-seeded substratum in above-mentioned fermention medium, the volume that the access ferment-seeded is cultivated accounts for
The 10%-20% of fermention medium cumulative volume, leavening temperature are controlled at 34-38 ℃, and fermentation period is 70 hours, and the dissolved oxygen amount in fermentor tank in unit volume is controlled at 20-30%.
The culturing step of described ferment-seeded substratum is as follows:
1, preparation seed culture medium, the material of 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 ‰, and surplus is water, places the seed culture medium for preparing stand-by.
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 is mainly to carry 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 elements and Carbon and nitrogen sources, rules on dull and stereotyped seed culture medium, 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 is controlled at 7.5, and culture temperature is controlled at 30 ℃-40 ℃, and incubation time is 3-10 days.
3, aspergillus niger list bacterium colony activation, picking list colony inoculation activates in activation medium.Activation medium is except the necessary carbon source that thalli growth is provided, 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 is controlled at 30 ℃-40 ℃, controls incubation time at 3-10 days.
4, the aspergillus niger after activating is inoculated into the inclined-plane seed culture medium.The inclined-plane seed culture medium is perfect medium, wherein contains organic and inorganic nutrients source, carbon source for example, and nitrogenous source and other micro-nutrients are mainly used in going down to posterity of seed, store.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 is controlled at 30 ℃-40 ℃, controls incubation time at 3-10 days.
Bacterial classification is cultivated in the inclined-plane seed culture medium good after, bacterial classification presents black on substratum, the mycelium of white can appear in crude sense on the substratum upper strata.
5, treat that spawn culture is good after, with transfering loop scraping bacterial classification, scraping bacterial classification 1-10 encircles in pure water after sterilization, then water is poured in the seed culture medium that configures.
It is 30m that above-mentioned seed culture medium is put into volume
3Vertical digester, control simultaneously temperature at 30-40 ℃, incubation time is 1-4 days, control pH at 6.5-8.5, aspergillus niger is cultivated suitable product acid in seed culture medium, acid production rate can obtain the ferment-seeded substratum after reaching 1.1-3.1g/dL, then can be inoculated in fermention medium.
It is mainly quantity for enlarging black-koji mould that ferment-seeded is cultivated, and making in the fermentation in later stage has enough bacterium to ferment.Generally, cultivate after about 20 hours to 30 hours in the ferment-seeded substratum and just can be inoculated into fermention medium, this moment, biomass was all proper with product acid.
Below that the present invention adopts the fermention medium production citric acid of glucose mother liquid preparation as follows with the technical indicator contrast of the fermention medium fermentation production of citric acid that adopts known employing glucose preparation:
| 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% |
Compare with existing known method, citric acid per ton can reduce costs 900 yuan, can increase by 1,000 ten thousand yuan of profits the whole year.Fully utilize simultaneously the waste liquor of discharging in the glucose production system, reduced the liquid waste disposal expense, year saved sewage disposal expense 500,000 yuan.Can also reduce 3,600 ten thousand yuan of the investment construction expenses of the required supporting liquid sugar of known technology production equipment.
Adopting glucose mother liquid of the present invention is that raw material replaces the raw materials of glucose in known citric acid fermentation substratum, and to the composition of lemon fermented substratum, performance, effect etc. are almost without any impact.
Test and rig-site utilization experiment showed, due to residual in glucose mother liquid after deliberation a small amount of polysaccharide, when bacterial classification just changes ferment tank over to, may not too adapt to, and therefore, can observe in the early stage of fermentation the sour slower situation of producing.But in the middle and later periods of fermentation, the raising that the generation speed of citric acid can be slowly also can reach at last the product acid that other substratum can reach and measure.Product and net result to fermentation can not have a negative impact.
Adopt the citric acid quality product of substratum fermentative production of glucose mother liquid of the present invention preparation as follows:
The 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% |
Adopt glucose mother liquid of the present invention to produce the method for citric acid, can rationally fully utilize the byproduct resource of corn deep processing process, environmental contamination reduction and sewage disposal expense, can obviously reduce raw materials cost, reduce the support equipment investment, reduce the pressure of sewage disposal in the corn comprehensive process, its product is impure few, with the citric acid of liquid glucose fermentative production, the quality guarantee is arranged more more.
Claims (10)
1. a method of producing citric acid, is characterized in that: comprise the steps:
A, add fermention medium in fermentor tank, 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.
2. a kind of method of producing citric acid according to claim 1, it is characterized in that: the volume of the ferment-seeded substratum that accesses in step b accounts for the 10%-20% of fermention medium cumulative volume, leavening temperature is 34-38 ℃, fermentation period is 70 hours, and in fermentor tank, the dissolved oxygen amount of unit volume is 20-30%.
3. a kind of method of producing citric acid according to claim 1, it is characterized in that: the culturing step of described ferment-seeded substratum is as follows:
(1), preparation seed culture medium;
(2), aspergillus niger list bacterium colony cultivates, by carry out the streak culture aspergillus niger list bacterium that goes out on dull and stereotyped seed culture medium;
(3), aspergillus niger list bacterium colony activation, picking list colony inoculation activates in activation medium;
(4), the aspergillus niger after activating is inoculated into the 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, scraping bacterial classification 1-10 encircles in pure water after sterilization, the water that then will contain bacterial classification is poured in the seed culture medium for preparing in step (1);
(6), the seed culture medium that contains aspergillus niger strain in step (5) is poured into to ferment in fermentor tank obtain the ferment-seeded substratum.
4. a kind of method of producing citric acid according to claim 3, is characterized in that: fermentation
Seed culture medium predominant quantity percentage composition described in the culturing step of seed culture medium (1) 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.
5. a kind of method of producing citric acid according to claim 3, is characterized in that: ferment and plant
Dull and stereotyped seed culture medium predominant quantity percentage composition described in the culturing step of sub-substratum (2) is as follows:
Wort: 10-30%;
Soybean protein hydrolyate: 5-30 ‰;
(NH
4)
2SO
4：1-10%；
Agar: 10-25%;
Surplus is water.
6. a kind of method of producing citric acid according to claim 5, is characterized in that: described flat
The pH of plate seed culture medium is controlled at 7.5, and culture temperature is controlled at 30 ℃-40 ℃, and incubation time is 3-10 days.
7. a kind of method of producing citric acid according to claim 3, it is characterized in that: the activation medium predominant quantity percentage composition described in the culturing step of described ferment-seeded substratum (3) is as follows:
Wort: 10-30%;
MnSO
4：2-4‰；
(NH
4)
2SO
4：1-10%；
Surplus is water.
8. a kind of method of producing citric acid according to claim 7, it is characterized in that: the pH of described activation medium is controlled at 7.5, and culture temperature is controlled at 30 ℃-40 ℃, controls incubation time 3-10 days.
9. a kind of method of producing citric acid according to claim 3, it is characterized in that: the inclined-plane seed culture medium predominant quantity percentage composition described in the culturing step of described ferment-seeded substratum (4) is as follows:
Wort: 10-30%;
(NH
4)
2SO
4：1-10%；
FeCl
2：0.01-0.1‰；
Agar: 10-25%;
Surplus is water.
10. a kind of method of producing citric acid according to claim 9, it is characterized in that: the pH of described inclined-plane seed culture medium is controlled to be 7.5, and culture temperature is controlled at 30 ℃-40 ℃, controls incubation time 3-10 days.
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|---|---|---|---|
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|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104561140A (en) * | 2013-10-23 | 2015-04-29 | 中粮营养健康研究院有限公司 | Method for preparing 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 |
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| 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)
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| 朱亨政等: "葡萄糖母液摇瓶发酵生产柠檬酸", 《微生物学通报》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104561140A (en) * | 2013-10-23 | 2015-04-29 | 中粮营养健康研究院有限公司 | Method for preparing citric acid by fermentation |
| 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 |
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|---|---|
| CN103382491B (en) | 2015-05-20 |
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Effective date of registration: 20170509 Address after: 262700 Shouguang Development Zone, Weifang, Shandong, Shandong Patentee after: Shouguang golden Far East Starch Co. Ltd. Address before: 262700 Shandong city in Weifang Province, Shouguang City emerging Street No. 150 Patentee before: Shandong Shouguang Juneng Group Golden Corn Co., Ltd. |