CN115893604A - Purification method of starch wastewater - Google Patents
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- CN115893604A CN115893604A CN202211389711.3A CN202211389711A CN115893604A CN 115893604 A CN115893604 A CN 115893604A CN 202211389711 A CN202211389711 A CN 202211389711A CN 115893604 A CN115893604 A CN 115893604A
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Abstract
The invention discloses a purification method of starch wastewater, belonging to the technical field of organic wastewater treatment. Adding metal ions with more than divalent ions into starch wastewater, uniformly stirring, adjusting the pH of the starch wastewater to be neutral or alkaline to promote reaction to obtain a metal-starch complex solution, adding a magnetic seed into the metal-starch complex solution, and stirring to obtain a suspension containing magnetic floccules; and (3) placing the suspension containing the magnetic floccules in a magnetic field for sedimentation. The method realizes the high-efficiency sedimentation separation of organic matters in the starch wastewater by combining the metal ion coordination control with the magnetic agglomeration separation technical means, has the advantages of simple operation, high treatment efficiency, good purification effect and low cost, and is beneficial to industrial application.
Description
Technical Field
The invention relates to a purification method of starch wastewater, in particular to a method for realizing starch wastewater purification based on metal ion coordination regulation-magnetic agglomeration separation, and belongs to the technical field of wastewater purification.
Background
The starch wastewater is wastewater generated in the production process of starch or starch deep-processing products (starch sugar, glucose, starch derivatives and the like), and mainly comprises intermediate product washing water, equipment washing water, raw material soaking water and the like. According to the state of the art processes and technology, the production of six tons of waste water is produced approximately every 1 ton of starch produced, and the production of waste water is therefore undoubtedly very large for the entire starch manufacturing industry. The wastewater is not toxic, but if the wastewater is directly discharged into rivers, dissolved oxygen in the water is consumed, the propagation of algae and aquatic plants is promoted, the water quality is deteriorated, and fishes and other organisms die, so that not only is the groundwater in the rivers polluted, but also the living environment of people is greatly influenced.
The conventional methods for treating starch wastewater comprise: air flotation, adsorption, flocculant sedimentation and Fenton reagent oxidation. The traditional method has the defects of high requirement on the performance of operation management equipment, difficult control of operation conditions, difficult subsequent treatment and the like.
The 'starch wastewater treatment process selection', jiahaijiang and the like, environmental pollution treatment technology and equipment, volume 4, 2 nd phase 2 in 2003, and 2 months) disclose a method for treating starch wastewater by chemical flocculation, which selects lime and polyaluminium chloride as flocculating agents, adds PMA coagulant aid, takes a raw water sample as a mixed solution of hot water rinsing wastewater and potato cleaning wastewater, has COD =2.564g/L and pH =4.5, and can realize industrial operation when the total removal rate of the COD after flocculation treatment is 50-70 percent, but the simultaneous addition of 3 flocculating agents is too complex in coordination control and equipment cost, inconvenient to operate, high in cost and unreasonable in economy.
Disclosure of Invention
Aiming at the technical problems of the existing starch wastewater treatment method, the invention aims to provide the starch wastewater treatment method, which realizes the high-efficiency sedimentation separation of organic matters in the starch wastewater by utilizing the technical means of metal ion coordination regulation and magnetic agglomeration separation, has the advantages of simple operation, high treatment efficiency, good purification effect and low cost, and is beneficial to industrial application.
In order to achieve the technical purpose, the invention provides a purification method of starch wastewater, which comprises the following steps:
1) Adding metal ions with more than two valences into the starch wastewater, uniformly stirring, and then adjusting the pH of the starch wastewater to be neutral or alkaline to promote reaction to obtain a metal-starch complex solution;
2) Adding the magnetic seeds into the metal-starch complex solution, and stirring to obtain a suspension containing magnetic floccules;
3) And (3) placing the suspension containing the magnetic floccules in a magnetic field for sedimentation.
Based on that most organic matters in the starch wastewater contain polar groups, the starch wastewater has good hydrophilicity and is difficult to naturally settle, the technical scheme of the invention skillfully utilizes high-valence metal ions and organic matters containing a large number of polar groups to carry out self-assembly coordination to form metal-starch complexes, the metal-starch complexes have charges and certain colloid properties, not only can adsorb other organic matters in the starch wastewater by utilizing the metal-starch complexes, but also can adsorb the organic matters on loaded magnetic seed particles to form magnetic floccules with larger particle diameters, and the magnetic floccules can realize rapid settling separation under the combined action of an external magnetic field and a gravity field, thereby achieving the purification effect of the starch wastewater.
As a preferable mode, the divalent or higher metal ion includes at least one of iron ion, aluminum ion, and lead ion. Generally, only divalent or more metal ions can show stronger coordination capacity to organic matters containing polar groups in the starch wastewater, and different divalent or more metal ions show different coordination capacity, and the most preferable divalent or more metal ions are lead ions. The divalent or higher metal ions are provided by water-soluble salts of these divalent or higher metal ions, and may be commonly sulfates, nitrates, and the like.
As a preferable scheme, the COD content of the starch wastewater is 3000-5000 mg/L.
Preferably, the concentration of the divalent or higher metal ion added to the starch wastewater is 1.5 to 6gL. Generally speaking, the higher the adding concentration of the metal ions with the more than two valences in the starch wastewater is, the more beneficial the removal of COD in the starch wastewater is, but the different coordination abilities of the metal ions with the more than two valences to the organic matters containing polar groups in the starch wastewater are different, the best effect is lead ions, the best adding concentration is 1.5 g/L-2.5 g/L, the characteristics of low using amount and good COD removal effect are provided, the best adding concentration of iron ions is 3.5-4.2 g/L, and the best adding concentration of aluminum ions is 4.5-6 g/L.
As a preferable mode, the stirring in the step 1) is performed for 3 to 8min at a rate of 300 to 500 r/min. The metal ions and the polar group-containing organic matters in the starch wastewater are fully reacted through full stirring, and the self-assembly coordination reaction is favorably carried out.
As a preferable scheme, the pH value of the starch wastewater is adjusted to 7-11. Under neutral or alkaline conditions of pH 7-11, the coordination between the divalent or higher metal ions and the polar group-containing organic matter in the starch wastewater is significantly favored, but if the pH is under acidic conditions, the coordination assembly reaction effect of the metal ions on the polar group-containing organic matter in the starch wastewater is relatively poor, but if the pH is too high, the coordination assembly reaction effect between the divalent or higher metal ions and the polar group-containing organic matter in the starch wastewater may be deteriorated due to the participation of hydroxyl groups in coordination, and therefore, the pH of the starch wastewater is further preferably adjusted to 8-10.
Preferably, the magnetic seeds have a particle size of 80-90% by mass of a fraction smaller than 37 μm, wherein the magnetic seeds with a particle size of 200 nm-1 μm can sufficiently react with suspended particles, and the magnetic seeds with a particle size of 1 μm or more can accelerate sedimentation. The magnetic seeds comprise at least one of steel dust, iron powder and magnetite. The most preferred magnetic species is iron and steel dust, fe 2 O 3 The content of the zinc oxide is more than 90 percent, and the rest is Zn, ca, si, mn and the like. The iron content of the steel smoke dust is high, the steel smoke dust is mainly iron oxide, so that the steel smoke dust shows high magnetism, and meanwhile, the steel smoke dust has an amorphous porous structure and shows good adsorption performance on a metal-starch complex, so that the steel smoke dust can be utilizedThe dust adsorbs the metal-starch complex, which is beneficial to the generation of magnetic floccules.
As a preferable scheme, the magnetic seeds are subjected to magnetic separation pretreatment by adopting a magnetic field with the intensity of 0.2-0.3T. Removing nonmagnetic particles in the magnetic separation. Avoid the pollution to the environment caused by the non-magnetic particles which can not be recovered.
Preferably, the concentration of the magnetic seeds added to the metal-organic complex solution is 10 to 40g/L. When the adding concentration of the magnetic seeds in the metal organic complex solution is about 10g/L, the settling time can reach better settling effect only within 32min, and when the adding concentration of the magnetic seeds in the metal organic complex solution is more than 20g/L, such as iron-starch complex and lead-starch complex, the settling time can reach better settling effect only within 8min, and for aluminum-starch complex, the settling time can reach better settling effect only within more than 32min, so the adding concentration of the magnetic seeds in the metal organic complex solution is preferably 20-40 g/L, and further preferably 30-40 g/L.
As a preferable scheme, the stirring speed in the step 2) is 300-500 r/min, and the stirring time is 3-8 min. The adsorption of the magnetic species to the metal-organic complex can be promoted by the preferred stirring conditions.
Preferably, the magnetic field strength is 0.3 to 0.5T.
Compared with the prior art, the technical scheme of the invention has the following beneficial technical effects:
1) The technical scheme of the invention utilizes high-valence metal ions to coordinate and complex organic matters in the starch wastewater to convert the organic matters into metal organic complexes, and on the basis, magnetic seeds are adopted to rapidly and efficiently adsorb and promote the metal organic complexes to form magnetic floccules, so that the magnetic floccules are rapidly settled and separated under the combined action of an external magnetic field and a gravitational field, the method can reduce the chemical oxygen demand of the high-concentration starch wastewater with the COD content of 3500mg/L by over 90 percent, and the method has the advantages of simple operation, high treatment efficiency, good purification effect, low cost and the like.
2) The invention can adopt the steel smoke dust as the magnetic seed, has low use cost and better adsorption and agglomeration effects, can realize the reutilization of industrial waste, and achieves the purpose of treating waste by waste.
Drawings
FIG. 1 is a graph showing the effect of different pH values on the removal rate of COD in starch wastewater in examples 1 to 3.
FIG. 2 is a graph showing the effect of different metal ions on the COD removal rate of starch wastewater in different amounts in examples 1-3.
FIG. 3 is an XRD pattern of different metal ion-starch complexes of examples 1-3.
FIG. 4 shows IR spectra of different metal ion-starch complexes of examples 1 to 3.
FIG. 5 is a particle size analysis of different metal ion-starch complexes of examples 1 to 3.
FIG. 6 shows the result of laser particle size analysis of steel dust.
FIG. 7 shows the effect of different amounts of iron and steel dusts on the settling effect of different organometallic complexes in examples 1 to 3.
Detailed Description
The following specific examples are intended to illustrate the invention in further detail, but not to limit the scope of the claims.
The COD content of the starch wastewater in the following specific examples was 3500mg/L.
In the following examples, the steel dust particle size satisfies 85% of the mass percentage content of the particle size fraction smaller than 37 μm, and the magnetic separation pretreatment is performed by using a 0.3T magnetic field.
Example 1
1. The ferric sulfate solution with the concentration of 5g/L is taken to react with the organic starch wastewater, the pH value of the solution is changed (2, 4,6,8, 10 and 12) to determine the influence of the pH value on the removal rate of COD in the starch wastewater, and the influence can be seen in figure 1: the removal rate of COD is low under the acidic condition, the removal rate of COD is increased and then reduced along with the increase of pH, and the removal rate reaches the highest when the pH of the solution is = 10.
2. The pH of the mixed solution was stabilized at 10, and the amount of ferric sulfate was increased to ensure that the concentration of ferric ions in the solution system was (1.3 g/L,2.1g/L,2.6g/L,3.3g/L,4.2 g/L), as can be observed in FIG. 2: the COD removal rate is increased along with the increase of the dosage of the iron ions, and the COD removal rate can reach 90 percent when the dosage of the iron ions is 4.2 g/L.
3. The use amount of the iron ions is determined to be 4.2g/L, the reaction time is gradually increased, the change of the sedimentation height of the precipitate obtained after the iron ions and the starch organic waste liquid are reacted along with the time can be observed, and after 32 minutes, the Fe-starch particles are only sedimented by 8cm.
4. As can be seen from the X-ray diffraction pattern (FIG. 3) of the iron-starch complex, the diffraction peaks of gamma-FeOOH are observed near 17.03 DEG and 24.10 DEG in the Fe-starch complex pattern.
5. Iron-starch complex particle size analysis results fig. 5 shows that d (0.1) =4.766 μm, d (0.5) =32.086 μm, d (0.9) =88.670 μm for iron-starch complexes, i.e. 10% of the particles have a particle size of 4.766 μm or less, 50% of the particles have a particle size of 32.086 μm or less, 90% of the particles have a particle size of 88.670 μm or less, and the volume average particle size is 40.452 μm.
6. Taking 50ml of starch wastewater in a beaker, adding 4.2g/L of iron ions, stirring for 5min, then adjusting the pH to 10, stirring for 5min, adding a certain amount of steel smoke dust, stirring for 5min again, uniformly mixing, transferring the solution to a settling tube, stably placing the settling tube in a magnet with the magnetic field intensity of 0.3T, and taking the using amounts of the steel smoke dust to be 10, 20, 30 and 40g/L respectively; settling times were 1,2, 4, 8, 16 and 32min. As shown in the figure 6 and the figure 7, the addition of the iron and steel smoke dust obviously improves the sedimentation effect of Fe-starch complex particles, when the dosage of the iron and steel smoke dust is 20g/L, the sedimentation can be basically completed within 8min, the thickness of the sedimentation layer is 25cm, and the COD measurement result shows that the COD content in the supernatant is reduced to 35.16mg/L from 186mg/L when the iron and steel smoke dust is not added, and the upper layer solution is colorless and transparent.
7. The dosage of iron ions is 4.2g/L, the pH =10, the dosage of the steel dust is 20g/L, and turbidity measurement is carried out when the steel dust is settled for 8min and 16 min. The test results show that: the turbidity of the steel fume dust added and the steel fume dust added in 8min are 2358.71 and 11.121 respectively, and the turbidity of the steel fume dust added in 16min is 1920.03 and 6.684 respectively. In the condition of natural sedimentation without adding iron dust, the turbidity of the iron ion-starch precipitate is higher, which is mainly because the natural sedimentation speed is slower and a large amount of suspended matters still exist during sampling. After the iron and steel dust is added, the turbidity of the Fe-starch complex is obviously reduced at 8min.
Example 2
1. The influence of the pH value on the COD removal rate of the starch wastewater is determined by taking an aluminum sulfate octadecahydrate solution with the concentration of 8g/L to react with the organic starch wastewater and changing the pH value of the solution (2, 4,6,8, 10, 12) as shown in figure 1: the removal rate of COD is low under the acidic condition, the removal rate of COD is increased and then reduced along with the increase of pH, and the removal rate reaches the highest when the pH of the solution is = 10.
2. The pH of the mixed solution is stabilized at 10, the dosage of aluminum sulfate octadecahydrate is increased to ensure that the concentration of aluminum ions in the solution system is (1.1, 2.2,3.3,4.4, 5.65g/L), the COD removal rate is observed to increase along with the increase of the dosage of the aluminum ions, and the COD removal rate can reach 90 percent when the dosage of the aluminum ions is 5.65 g/L.
3. The dosage of the aluminum ions is 5.65g/L, the reaction time is gradually increased, the change of the sedimentation height of the precipitate obtained after the metal ions and the starch organic waste liquid are acted with time is observed, and after 32 minutes, the Al-starch particles are only settled by 3cm.
4. According to the X-ray diffraction pattern of the aluminum ion-starch complex, as can be seen from fig. 3, in the pattern of the Al-starch complex, diffraction peaks near 14.54 °, 28.41 °, 38.21 °, 49.39 ° and 64.64 ° are consistent with gamma-AlOOH.
Fig. 5 shows that d (0.1) =14.459 μm, d (0.5) =48.499 μm, d (0.9) =132.707 μm, and the volume average particle size of the Al-starch complex is 63.268 μm. The Al-starch complex has the largest volume average particle size, but the slowest sedimentation speed and the thickest sedimentation layer, which are probably caused by higher potential, more stable system and large space structure of coordination assemblies formed by the Al-starch complex and starch.
6. Taking 50ml of starch wastewater in a beaker, adding 5.65g/L of aluminum ions, stirring for 5min, adjusting the pH value to 10, stirring for 5min, adding a certain amount of steel smoke dust, stirring for 5min, uniformly mixing, transferring the solution to a settling tube, stably placing the settling tube in a magnet with the magnetic field intensity of 0.3T, and respectively taking 10g/L, 20g/L, 30g/L and 40g/L of the steel smoke dust; settling times were 1,2, 4, 8, 16 and 32min. As can be seen from FIGS. 6 and 7, the addition of the iron and steel dust can improve the sedimentation performance of the Al-starch complex particles to a certain extent, but when the amount of the iron and steel dust is low, the sedimentation rate of the Al-starch particles is still slow, and the sedimentation rate gradually increases with the increase of the amount of the iron and steel dust, but the increase is slow. When the using amount of the steel dust reaches 40g/L, rapid sedimentation still cannot be realized within a short time, and when the using amount of the steel dust reaches 32min, the thickness of a sedimentation layer is still 30cm. This may be associated with an excessive amount of aluminium ions with which the steel fumes do not work adequately.
7. The dosage of aluminum ions is 5.65g/L, the pH =10, and the dosage of steel smoke dust is 40g/L. Turbidity measurements were performed at 8min and 16min of settling. The test results show that: the turbidity of the steel fume dust without adding steel fume dust at 8min and the turbidity of the steel fume dust with adding steel fume dust are 2126.8 and 3268.72 respectively, and the turbidity of the steel fume dust with adding steel fume dust at 16min is 2101.72 and 2096.34 respectively. Under the condition of no steel dust natural sedimentation, the turbidity of the aluminum ion-starch complex is higher, which is mainly because the natural sedimentation speed is slower and a large amount of suspended matters still exist during sampling. After the steel dust is added, the turbidity of the Al-starch precipitate is even increased within 2min, and is not obviously reduced within 8min.
Example 3
1. The effect of pH value on COD removal rate of starch wastewater is determined by reacting 2g/L lead nitrate solution with organic starch wastewater and changing pH of the solution (2, 4,6,8, 10, 12) as shown in FIG. 1: the removal rate of COD is low under the acidic condition, the removal rate of COD is increased and then reduced along with the increase of pH, and the removal rate reaches the highest when the pH of the solution is = 10.
2. The pH of the mixed solution was stabilized at 10, the amount of lead nitrate used was increased so that the lead ion concentration in the solution system was (0.5, 1.0,1.5,2.0,2.5 g/L), and it was observed that the COD removal rate increased with the increase in the amount of lead ions, and the COD removal rate reached 90% at a lead ion amount of 2.5 g/L.
3. The dosage of the lead ions is 2.5g/L, the reaction time is gradually increased, and the change of the sedimentation height of the precipitate obtained after the lead ions and the starch organic waste liquid are reacted with each other along with the time is observed. After 32 minutes, the Pb-starch complex particles settled by only 5cm.
4. As can be seen from FIG. 3, in the spectrum of the Pb-starch complex, near 24.28 ℃ and 53.88 ℃ are (PbCO) 3 ) 2 ·Pb(OH) 2 Diffraction peaks of (1) at around 34.20 DEG and 26.61 DEG are Pb 3 O 4 Diffraction peak of (1), pb at 30.36 DEG 2 O 3 Possibly because of decomposition of lead hydroxide and CO during crystallization of the Pb-starch complex 2 A reaction takes place.
The results of particle size analysis of Pb-starch complex in FIG. 5 show that the Pb-starch precipitate has d (0.1) = 1.740. Mu.m, d (0.5) = 8.221. Mu.m, d (0.9) = 73.555. Mu.m, and a volume average particle size of 26.951. Mu.m, and it can be seen that the Pb-starch precipitate distribution diagram has two peaks, a wide particle size distribution, and a large amount of fine particles, which is consistent with the poor solid-liquid separation effect of Pb-starch precipitate in the sedimentation test.
6. Taking 50ml of starch wastewater in a beaker, adding 2.5g/L of lead ions, stirring for 5min, adjusting the pH value to 10, stirring for 5min, adding a certain amount of steel smoke dust, stirring for 5min, uniformly mixing, transferring the solution to a settling tube, stably placing the settling tube in a magnet with the magnetic field intensity of 0.3T, and respectively taking 10g/L, 20g/L, 30g/L and 40g/L of the steel smoke dust; settling times were taken at 1,2, 4, 8, 16 and 32min. The effect of the magnetic sedimentation of the Pb-starch complex particles is similar to that of the Fe-starch complex particles. After the iron and steel dust is added, the sedimentation effect of the Pb-starch complex particles is obviously improved, and the effect is more obvious along with the increase of the using amount of the iron and steel dust. When the using amount of the steel dust is 30g/L, the thickness of the sedimentation layer can be reduced to 23cm within 8min.
7. The dosage of lead ions is 2.5g/L, the pH =10, the dosage of steel dust is 30g/L, and turbidity measurement is carried out when the steel dust is settled for 8min and 16 min. The test results show that: the turbidity of the steel dust added and the turbidity of the steel dust added are 1727.35 and 10.47 respectively at 8min and 911.53 and 7.957 respectively at 16 min. Under the condition of no steel dust natural sedimentation, the turbidity of the lead ion-starch complex is higher, which is mainly because the natural sedimentation speed is slower and a large amount of suspended matters still exist during sampling. The turbidity of Pb-starch sediment is obviously reduced after the iron and steel dust is added in 8min.
Generally speaking, the crystallization of three metal ion-starch complexes of lead, iron and aluminum is incomplete, impurity interference exists, and the three metal ion-starch complexes are fine in particle size, so that the precipitation performance is poor under natural conditions, and solid-liquid separation is difficult. Compared with the method without adding steel smoke dust, the sedimentation effect of the three metal ion-starch complexes is improved to a certain extent along with the addition of the steel smoke dust, and the purposes of rapid sedimentation and sedimentation layer compression are achieved. The improvement degree of the sedimentation effect of the iron and steel dust on different metal ion-starch complex particles is Fe 3+ ＞Pb 2+ ＞Al 3+ 。
Claims (10)
1. A purification method of starch wastewater is characterized in that: the method comprises the following steps:
1) Adding metal ions with more than two valences into the starch wastewater, uniformly stirring, and then adjusting the pH of the starch wastewater to be neutral or alkaline to promote reaction to obtain a metal-starch complex solution;
2) Adding the magnetic seeds into the metal-starch complex solution, and stirring to obtain a suspension containing magnetic floccules;
3) And (3) placing the suspension containing the magnetic floccules in a magnetic field for sedimentation.
2. The method for purifying starch wastewater according to claim 1, wherein: the metal ion with the divalent or higher valence includes at least one of iron ion, aluminum ion and lead ion.
3. The method for purifying starch wastewater according to claim 1 or 2, wherein: the addition concentration of the divalent or higher metal ions in the starch wastewater is 1.5-6 gL.
4. The method for purifying starch wastewater according to claim 1, wherein: the COD content of the starch wastewater is 3000-5000 mg/L.
5. The method for purifying starch wastewater according to claim 1, wherein: and adjusting the pH value of the starch wastewater to 7-11.
6. The method for purifying starch wastewater according to claim 1, wherein: the granularity of the magnetic seeds meets the requirement that the mass percentage content of the grain size smaller than 37 mu m is 80-90%.
7. The method for purifying starch wastewater according to claim 1 or 6, wherein: the magnetic seeds comprise at least one of steel dust, iron powder and magnetite.
8. The method for purifying starch wastewater according to claim 1, 4 or 6, wherein:
the adding concentration of the magnetic seeds in the metal-starch complex solution is 10-40 g/L.
9. The method for purifying starch wastewater according to claim 1, wherein: the magnetic field intensity is 0.3-0.5T.
10. The method for purifying starch wastewater according to claim 1, wherein: the settling time is more than 8min.
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