CN101838041A - Preparation method of composite polysaccharide bioflocculant - Google Patents

Preparation method of composite polysaccharide bioflocculant Download PDF

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CN101838041A
CN101838041A CN 201010192583 CN201010192583A CN101838041A CN 101838041 A CN101838041 A CN 101838041A CN 201010192583 CN201010192583 CN 201010192583 CN 201010192583 A CN201010192583 A CN 201010192583A CN 101838041 A CN101838041 A CN 101838041A
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polysaccharide bioflocculant
bioflocculant
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CN101838041B (en
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庄汉忠
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Weihai Hanbang biological environmental protection Polytron Technologies Inc
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Abstract

The invention discloses a preparation method of a composite polysaccharide bioflocculant, comprising the following steps of: A10. alkalifying a polysaccharide bioflocculant with the viscosity of 3,000-10,000cps with aqueous alkali; A20. oxidizing an inorganic iron salt solution with an oxidant, wherein the content of iron in the solution after oxidization is 8.0-10.0 percent; and A30. adding the solution obtained in the step A20 into the solution obtained in the step A10 step by step to carry out composite reaction to obtain the composite polysaccharide bioflocculant, wherein the mass content of the composite polysaccharide bioflocculant in the solution obtained after the reaction is 0.43-4.7 percent, and the content of iron is 4.7-8.6 percent. The composite polysaccharide bioflocculant has not toxicity, no harm, no secondary pollution, high flocculation efficiency, wide application range as well as economy and practicability.

Description

The preparation method of composite polysaccharide bioflocculant
Technical field
The present invention relates to the preparation method of water conditioner, particularly relate to the preparation method of composite polysaccharide bioflocculant.
Background technology
Water is the indispensable precious resources of human survival, life and production, is the lifeblood of agricultural, the power of industry and the blood in city, for the development and prosperity of human society is being brought into play important support and guaranteeing role.Be accompanied by the progress and the expanding economy of science and technology, human demand to water also increases gradually, and inevitably produces the water environment pollution problem.The seriously polluted water crisis that causes of shortage of water resources and water not only destroys the eubiosis, causes the further aggravation of water resources imbalance between supply and demand, and can cause enormous economic loss.As seen, national economy is not only seriously being perplexed in the water crisis, and has become the important restraining factors of Chinese society Economic development.The problem that present China water surrounding faces is respectively: (one) discharge of major pollutant amount is considerably beyond water environment capacity.(2) rivers and lakes are generally polluted.(3) ecological water lacks, the water environment degradation aggravation.
Owing to water environmental problems a big chunk reason causes owing to production, sanitary wastewater directly discharge, therefore, production, sanitary wastewater are handled and recycle is the important measures of administering water environment pollution, and at water-treatment technology field, water conditioner is again the emphasis in this field.
Water conditioner is often referred to the chemical agent that is used for sewage disposal, and this chemical agent is used for eliminating and prevents that fouling, corrosion and bacterium algae from growing and carry out purification of water quality, to reach water saving and to prevent the purpose of pollution of waterhead.Water conditioner comprises flocculation agent, is used for removing the mechanical impurity of former water; Scale inhibitors is used to prevent fouling; Inhibiter is used for suppressing corrosion; Sterilant is used to stop harmful microbe to grow; Clean-out system is used to remove anvil cinder, old dirt, greasy dirt etc., and wherein, flocculation agent, flocculation agent have accounted for 3/4 of water conditioner total amount, has wherein accounted for 1/2 of flocculation agent, flocculation agent again as the polyacrylamide (PAM) of flocculation agent, and all the other 1/2 are inorganic polymer.
Yet, water conditioner at present commonly used, for example inorganic aluminate and polymkeric substance thereof and polyacrylamide are monomeric residual, and be more and more serious to the harm that HUMAN HEALTH and environment bring.Therefore, research and develop water conditioner efficient, nontoxic, harmless, non-secondary pollution, not only have realistic meaning, and have long-range strategic importance.In this respect, biological flocculant adds to have long main chain and more active gene in its molecule because its energy natural degradation does not have any harm to human body and environment, thereby is subjected to global scientific worker's favor.But, also be in starting stage of research and development at China's biological flocculant, sophisticated launch is not also arranged so far, subject matter is: the first, production cost is higher; The second, fine to some sewage flocculation effect, but then treatment effect is dissatisfied to other sewage.
Summary of the invention
In view of the problems referred to above that biological flocculant exists, the invention provides a kind of preparation method of composite polysaccharide bioflocculant, may further comprise the steps:
A10, be that the polysaccharide bioflocculant of 3000cps～10000cps carries out alkalinisation treatment with alkaline solution with viscosity, after the alkalinisation treatment in this solution the mass content of polysaccharide bioflocculant be 4.9%～9.9%, the mass content of alkali is 0.1%～1.0%;
A20, inorganic molysite solution is carried out oxidation with oxygenant, after the oxidation in this solution iron level be 8.0～10.0%;
A30, the solution that steps A 20 is obtained progressively join and carry out complex reaction in the solution that steps A 10 obtains and obtain composite polysaccharide bioflocculant, in this step, the proportioning of two kinds of solution is: in the steps A 10 gained solution in the quality of polysaccharide bioflocculant and the steps A 20 gained solution mass ratio of iron level be 1: 1～20, after complex reaction is finished in the gained solution mass content of polysaccharide bioflocculant be 0.43%～4.7%, iron level is 4.7%～8.6%.
In the aforesaid method, the concrete treating processes of steps A 10 is, it is 5～10% solution that polysaccharide bioflocculant is deployed into mass content, stir and be cooled to below 20 ℃, adding mass percent concentration then and be 20%～25% alkaline solution continues to stir and keeps temperature below 20 ℃ 1 hour, wherein, the mass ratio of polysaccharide bioflocculant and alkaline solution is 1: 0.02～0.1.
In the aforesaid method, alkaline solution is sodium hydroxide, potassium hydroxide or sodium carbonate solution.
In the aforesaid method, stir speed (S.S.) is 50～100 rev/mins.
In the aforesaid method, the concrete treating processes of steps A 20 is, the preparation iron level is 10% inorganic molysite solution earlier, regulate pH to 0.8～1.2 with the vitriol oil again, drip concentration then and be 30% oxidizing agent solution, continue to stir 30 minutes, the volumetric ratio of inorganic molysite solution and oxidizing agent solution is 10: 1, and whole oxidising process answers holding temperature below 30 ℃.
In the aforesaid method, the rate of addition of oxidizing agent solution is 1/30～1/60 of a per minute adding cubic capacity.
In the aforesaid method, inorganic molysite is ferrous sulfate or iron trichloride, and oxygenant is hydrogen peroxide or clorox.
In the aforesaid method, in the steps A 30, temperature is 20 ℃～60 ℃, and stir speed (S.S.) is 50～80 rev/mins, and the reaction times is 2～4 hours.
The present invention, adopt advanced efficient enzyme process synthetic technology and cyclic regeneration technology, with Chinese invention patent CN101392280A, a kind of Enzymology method for preparing polysaccharide bioflocculant is converted into large-scale industrial production, production cost is significantly reduced, reach the complete receptible level of domestic and international client; And adopt composite method, utilize inorganic molysite, especially ferrous sulfate, low price and good charge neutrality are taken off bridge formation, the net of steady effect and polysaccharide bioflocculant excellence and are caught, roll up the effect of sweeping, both are composite, realize both chemically with function on combination, complementation, and along with the raising of product flocculating effect, the actual motion expense and the facility investment of sewage disposal also will significantly reduce, and the more important thing is that this compound product is a biological environmental production product really nontoxic, harmless, non-secondary pollution.Specifically, the present invention has the following advantages:
(1), flocculation efficiency height: because powerful bridge formation, volume that the present invention utilizes the good electric neutralization of inorganic molysite to take off steady characteristic and polysaccharide bioflocculant are swept effect, it is big and solid to make this patent product demonstrate the flocculation particle in sewage disposal, flocculation forms fast, and the also fast and mud compression performance of sedimentation speed is good than independent user also.The macromethod data presentation, its turbidity removal, the effect of decolouring, falling COD significantly are better than inorganic molysite, aluminium salt and their polymkeric substance.In addition, its effect (seeing application example for details) that some sewage are also had remarkable dephosphorization, denitrogenate.
(2), the scope of application is extensive: this patent product is to river sewage, the various industrial sewage of city domestic sewage, pollution, gourmet powder waste water for example, especially dyeing waste water comprises that extremely unmanageable active dye wastewater and the former water of tap water all have extremely good flocculating effect.
(3), economical and practical: the polysaccharide bioflocculant system that the art of this patent adopted adopts the Enzymology method and the cyclic regeneration technology of high yield, and has carried out big standard suitability for industrialized production, and cost can significantly reduce, and the price of the ferrous sulfate in the product own is very cheap.The aspect is owing to efficient, so their consumption significantly reduced when also using more separately in addition.As seen, this patent is realized the complementary effect of two kinds of compound substances aspect function and cost.
(4), nontoxic, harmless, non-secondary pollution: among the present invention, polysaccharide bioflocculant adopts abacterial Production by Enzymes and ultra-filtration membrane purifying, based on very high purity, but and natural degradation; And the ferrous sulfate actual amount significantly reduces when using separately, and the iron after compound has been converted into safer biological iron.As seen this patent product there is no any harm to water quality, edatope and HUMAN HEALTH in sewage treatment process.
Embodiment
Below in conjunction with specific embodiment the present invention is made detailed explanation.
To 10000cps, its preparation method adopts Chinese invention patent CN101392280A to employed polysaccharide bioflocculant range of viscosities from 3000cps among the present invention, and a kind of Enzymology method for preparing polysaccharide bioflocculant carries out.
Embodiment one:
A10, polysaccharide bioflocculant is carried out alkalinisation treatment.
Concrete grammar, adding mass percentage content in the there-necked flask of 1000ml is 10%, viscosity is the polysaccharide bioflocculant 500ml (polysaccharide bioflocculant that is equivalent to 50 gram dry weights of 3000cps, the content that is solute is 50 grams), there-necked flask is placed 20 ℃ or following water-bath and stir with the speed of stirrer with 50～100 rev/mins, the back that stirs slowly drips concentration to be that 20% NaOH solution 5ml (dripping off about 15 minutes) continues stirring 1 hour more standby, in this process, remain solution temperature at 20 ℃ or following, the mass content of polysaccharide bioflocculant is 9% in the resulting solution, the mass content of alkali is 0.8%, wherein the mass content of the mass content of polysaccharide bioflocculant and alkali can change with the add-on of NaOH solution, be 1 promptly by the mass ratio of adjusting polysaccharide bioflocculant and alkaline solution: thus 0.02～0.1 to make the mass content of polysaccharide bioflocculant be 4.9%～9.9%, and the mass content of alkali is 0.1%～1.0%;
A20, copperas solution is carried out oxide treatment.
Concrete grammar is that other gets the there-necked flask of a 1000ml, adds FeSO 47H 2O 250 gram and pure water 250ml put heat temperature raising to 30 in the water-bath～40 ℃, make FeSO with 50 rev/mins speed stirrings 47H 2O fully dissolves, and adds pure water again to cubic capacity 500ml, and iron level this moment (IronContent) is 10%, further regulates pH to 0.8～1.2 with a small amount of vitriol oil, and slowly dripping concentration with the speed of 1～3ml/ branch then is 30% H 2O 2Solution 50ml, and stir with 50～100 rev/mins speed simultaneously, continuing again after waiting to drip off to stir 30 minutes, temperature of reaction should be controlled at below 30 ℃ in the above-mentioned oxidising process.Finally obtaining cubic capacity is the copperas solution through peroxidation of 550ml, and the iron level in this solution is 9.0%.The variation of the amount by adding pure water can be adjusted the iron level in this solution, and setting range is 8.0～10.0%.
A30, complex reaction.
Concrete grammar is, progressively add the polysaccharide bioflocculant 50ml after the alkalization that steps A 10 obtains among the copperas solution 550ml after the oxidation that steps A 20 is obtained, under 25～30 ℃ of room temperatures with 50～100 rev/mins speed continuously stirring 2 hours, make composite polysaccharide bioflocculant 600ml, wherein iron level is 8.3%, and the mass content of polysaccharide bioflocculant is 0.83%.
Embodiment two:
The difference of present embodiment and embodiment one is, is that the polysaccharide bioflocculant replacement viscosity of 5000cps is the polysaccharide bioflocculant of 3000cps with viscosity, and other raw materials are all identical with embodiment one with working method.The mass content of iron is 8.3% among the composite polysaccharide bioflocculant 600ml that finally obtains, and the mass content of polysaccharide bioflocculant is 0.83%.
Embodiment three:
The difference of present embodiment and embodiment one be with viscosity be the polysaccharide bioflocculant of 10000cps to replace viscosity be the polysaccharide bioflocculant of 3000cps, other desired raw materials and working method are all identical with embodiment 1.The mass content of iron is 8.3% among the composite polysaccharide bioflocculant 600ml that finally obtains, and the mass content of polysaccharide bioflocculant is 0.83%.
Product after the polysaccharide bioflocculant of above-mentioned three kinds of different viscosity and iron are compound, equal quality there is no significant difference to the flocculating effect of same sewage, and therefore, in 3000cps～10, the polysaccharide bioflocculant in the 000cps range of viscosities all can use.
Embodiment four:
The difference of present embodiment and embodiment one is, replaces hydrogen peroxide that ferrous sulfate is carried out oxidation with clorox, and other raw materials are all identical with embodiment one with method.Product and embodiment one product equal no significant difference aspect quality and flocculating effect of present embodiment preparation, the prompting clorox is effectively same in the technology of the present invention.
Embodiment five:
Among the embodiment one, the mass ratio of polysaccharide bioflocculant and iron is 1: 10, in this example this ratio is changed into 1: 1.Detailed process is:
Press the alkalization polysaccharide bioflocculant of embodiment one method preparation, get among copperas solution (mass content 9.0%) 222ml after this flocculant solution of 200ml joins the oxidation of embodiment one preparation, under 25～30 ℃ of room temperatures with 50～100 rev/mins speed continuously stirring 2 hours, obtain the 422ml composite polysaccharide bioflocculant, wherein iron level is 4.7%, and the polysaccharide bioflocculant mass content is 4.7%.Present embodiment is compared with embodiment one, and polysaccharide bioflocculant content obviously increases, thereby more suitable to the less sewage disposal of particle that is difficult to flocculate or flocculate.
Embodiment six:
In the present embodiment, change the mass ratio of polysaccharide bioflocculant and iron into 1: 20, detailed process is as follows:
Press the alkalization polysaccharide bioflocculant of embodiment 1 method preparation, getting the 50ml mass content and be 10% solution is added on by among copperas solution (mass content 9.0%) 1111ml after the oxidation of embodiment 1 preparation, room temperature (25 ℃～30 ℃) continuously stirring (50～100 rev/mins) 2 hours, the products obtained therefrom cubic capacity was 1161ml.Wherein iron level is 8.6%, and polysaccharide bioflocculant content is 0.43%.
Composite polysaccharide bioflocculant of the present invention can be applicable to the coagulating treatment of multiple sewage, now illustrates as follows:
Application examples one: the application of iron content composite polysaccharide bioflocculant in river sewage is handled.
Use composite polysaccharide bioflocculant of the present invention part tributary, river bend, Shenzhen river sewage is carried out coagulating sedimentation.Method system adopts 2R4-6 coagulation test stirrer (profit water and wastewater industry Technology Dev Company Ltd. makes in the Shenzhen), the iron content composite polysaccharide bioflocculant 1～2ml and coagulant aids (calcium oxide) 0.1 gram that in 1L water, add embodiment 1 preparation, the start-up operation program, during beginning quick (400 rev/mins), stirred 1～1.5 minute, (20～30 rev/mins) stirred 2 minutes then at a slow speed, static afterwards 30 minutes; Get supernatant liquor and measure photoabsorption (0D), turbidity, chemical oxygen demand (COD) (COD) and total nitrogen and total phosphorus.Method system is according to " water and the effluent monitoring analytical procedure " of State Environmental Protection Administration's establishment.Gained result such as subordinate list 1.
Subordinate list 1, composite polysaccharide bioflocculant are to the flocculating effect of Shenzhen's part river sewage.
Except that adding the iron content composite polysaccharide bioflocculant, still add coagulant aids (calcium oxide) 0.1 gram.
The result shows that compound bio flocculation agent of the present invention is remarkable especially to decolouring, the turbidity removal effect of river sewage.Its clearance reaches 90%～99.2%, and phosphor-removing effect is also quite satisfied, and clearance reaches 74.5%～98.2%, in addition, to denitrogenating and falling COD certain effect is arranged also.
Application examples two: composite polysaccharide bioflocculant is to the domestic sewage treating effect
Adopt polysaccharide bioflocculant of the present invention that Shenzhen's part sanitary sewage is carried out coagulation and sedimentation experiment.Method is identical with application examples one.Result such as subordinate list 2:
Subordinate list 2, composite polysaccharide bioflocculant are to the flocculating effect of Shenzhen's part sanitary sewage
Except that adding ferruginous composite polysaccharide bioflocculant, still add coagulant aids (calcium oxide) 0.1 gram.
Subordinate list 2 shows that further polysaccharide bioflocculant of the present invention has the flocculating effect same with river sewage to city domestic sewage.
Application examples three: composite polysaccharide bioflocculant is in some Application in Industrial Wastewater Treatment.
Adopt composite polysaccharide bioflocculant of the present invention to some trade effluent, for example comprehensive trade effluent, dyeing waste water, leather waste water carry out coagulating sedimentation.Result such as subordinate list 3:
Table 3, composite polysaccharide bioflocculant are to the flocculating effect of some trade effluent
Figure GSA00000134175900102
Except that adding ferruginous composite polysaccharide bioflocculant, still add coagulant aids (calcium oxide) 0.1～0.2 gram.
Subordinate list 3 shows that this composite polysaccharide bioflocculant is all satisfied to the treatment effect of described several trade effluents.
The present invention is not limited to above-mentioned preferred forms, and anyone should learn the structural changes of making under enlightenment of the present invention, and every have identical or close technical scheme with the present invention, all falls within protection scope of the present invention.

Claims (8)

1. the preparation method of composite polysaccharide bioflocculant is characterized in that may further comprise the steps:
A10, be that the polysaccharide bioflocculant of 3000cps～10000cps carries out alkalinisation treatment with alkaline solution with viscosity, after the alkalinisation treatment in this solution the mass content of polysaccharide bioflocculant be 4.9%～9.9%, the mass content of alkali is 0.1%～1.0%;
A20, inorganic molysite solution is carried out oxidation with oxygenant, after the oxidation in this solution iron level be 8.0～10.0%;
A30, the solution that steps A 20 is obtained progressively join and carry out complex reaction in the solution that steps A 10 obtains and obtain composite polysaccharide bioflocculant, in this step, the proportioning of two kinds of solution is: in the steps A 10 gained solution in the quality of polysaccharide bioflocculant and the steps A 20 gained solution mass ratio of iron level be 1: 1～20, after complex reaction is finished in the gained solution mass content of polysaccharide bioflocculant be 0.43%～4.7%, iron level is 4.7%～8.6%.
2. the preparation method of composite polysaccharide bioflocculant as claimed in claim 1, the concrete treating processes that it is characterized in that steps A 10 is, it is 5～10% solution that polysaccharide bioflocculant is deployed into mass content, stirring also is cooled to 20 ℃ or following, adding mass percent concentration then and be 20%～25% alkaline solution continues to stir and keeps 20 ℃ of temperature or following 1 hour, wherein, the mass ratio of polysaccharide bioflocculant and alkaline solution is 1: 0.02～0.1.
3. the preparation method of composite polysaccharide bioflocculant as claimed in claim 2 is characterized in that alkaline solution is sodium hydroxide, potassium hydroxide or sodium carbonate solution.
4. the preparation method of composite polysaccharide bioflocculant as claimed in claim 2 is characterized in that stir speed (S.S.) is 50～100 rev/mins.
5. the preparation method of composite polysaccharide bioflocculant as claimed in claim 1, the concrete treating processes that it is characterized in that steps A 20 is, the preparation iron level is 10% inorganic molysite solution earlier, regulate pH to 0.8～1.2 with the vitriol oil again, drip concentration then and be 30% oxidizing agent solution, continue to stir 30 minutes, the volumetric ratio of inorganic molysite solution and oxidizing agent solution is 10: 1, and whole oxidising process answers holding temperature below 30 ℃.
6. the preparation method of composite polysaccharide bioflocculant as claimed in claim 1, the rate of addition that it is characterized in that oxidizing agent solution be per minute add cubic capacity 1/30～1/60.
7. the preparation method of composite polysaccharide bioflocculant as claimed in claim 5 is characterized in that inorganic molysite is ferrous sulfate or iron trichloride, and oxygenant is hydrogen peroxide or clorox.
8. the preparation method of composite polysaccharide bioflocculant as claimed in claim 1 is characterized in that in the steps A 30, and temperature is 20 ℃～60 ℃, and stir speed (S.S.) is 50～80 rev/mins, and the reaction times is 2～4 hours.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105621568A (en) * 2015-12-29 2016-06-01 哈尔滨工业大学 Preparation method of ferric salt solution
NO20170373A1 (en) * 2017-03-14 2018-09-17 M Vest Water As Product, method and application for removal of pollution in water

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CN1490256A (en) * 2003-08-27 2004-04-21 中国科学院沈阳应用生态研究所 Economic inorganic-organic composite flocculant
CN1515507A (en) * 2003-01-08 2004-07-28 中国科学院沈阳应用生态研究所 Ecological safety composite type iron system high-effective flocculating agent

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105621568A (en) * 2015-12-29 2016-06-01 哈尔滨工业大学 Preparation method of ferric salt solution
NO20170373A1 (en) * 2017-03-14 2018-09-17 M Vest Water As Product, method and application for removal of pollution in water
NO344503B1 (en) * 2017-03-14 2020-01-20 M Vest Water As Product, method and application for removal of contaminants in water

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