CN104445436B - A kind of take copper water-supply pipe as the method that nano ferriferrous oxide prepared by raw material - Google Patents
A kind of take copper water-supply pipe as the method that nano ferriferrous oxide prepared by raw material Download PDFInfo
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Abstract
Take copper water-supply pipe as the method that nano ferriferrous oxide prepared by raw material, it relates to a kind of preparation method of nano ferriferrous oxide.The object of the invention is to solve the problem that iron salt coagulant compositions a large amount of in copper water-supply pipe cannot fully be utilized.Method: one, prepare copper water-supply pipe powder; Two, roasting; Three, acid leaching extraction; Four, centrifugation; Five, nanometer process, namely obtains nano ferriferrous oxide.Advantage: do easy, generates without harmful by-products, avoids copper water-supply pipe and recycles the problems such as the secondary pollution harm produced, reduce the preparation cost of nano ferriferrous oxide.The present invention is mainly used in utilizing copper water-supply pipe to prepare nano ferriferrous oxide for raw material.
Description
Technical field
The present invention relates to a kind of preparation method of nano ferriferrous oxide.
Background technology
In recent years, along with China's Small Towns water feeding system development and perfect, some problems also produce thereupon, seriously pollute surface water body as discharged a large amount of undressed copper water-supply pipe.China has formulated relevant laws and regulations to sludge water condition in waterworks and has disposed to the process managing samll cities and towns' copper water-supply pipe, to reduce the harm that it causes environment, mainly comprise modified to the method that its process is disposed, dehydration, sanitary landfill, direct discharge etc., but because it produces enormous amount, a large amount of medicament expense will be consumed use, labour cost or mechanical means expense, take a large amount of land resources, and the secondary pollution problem that the percolate in landfill place etc. produce also receives much concern, direct discharge then needs to carry out long term monitoring to jettisoning waters, environmental pollution etc. problem is inevitably caused to storage waters, effective solution is extremely urgent, it is how the problem being worth inquiring into by the disposal of effective for copper water-supply pipe environmental protection.
To the research of sludge water condition in waterworks process, oneself is extended to the disposal of microscopic theory and dehydrated sludge cake gradually by aspects such as processing technological flow, equipment application and the selections of sludge conditioning medicament and is fully utilized.Realizing recycling will be final, the best method of sludge disposal, for the recycling of mud as simply cultivated for gardens, bottom mud in lake absorption, abandoned mine filling etc., the usage quantity of these resource utilization methods to copper water-supply pipe has certain restriction, can not more than 20 tons as cultivated per hectare soil for gardens, after mud appropriateness is applied to soil, the flocculation reaction be similar in water treatment procedure can improve the flocculating degree of soil, improve the structure of soil, be beneficial to farming; The secondary pollution problems still needing to consider to exist as excessive in consumption.In the face of copper water-supply pipe generation huge every year, we then need to find copper water-supply pipe recycling more thoroughly method.And in the long run, reasonably, scientifically utilizing copper water-supply pipe to be the inexorable trend of environment protection, how recycling sludge is utilized that process is simplified, practical, commercialization, is a problem urgently to be resolved hurrily.
Utilizing status to copper water-supply pipe has greatly been increased as material of construction etc. such as brickmaking, cement processed, potting grains with mud, but the source of copper water-supply pipe mainly settling tank, wherein containing a large amount of iron salt coagulants etc., these a large amount of iron salt coagulant compositions are not fully utilized.
Summary of the invention
The object of the invention is to solve the problem that iron salt coagulant compositions a large amount of in copper water-supply pipe cannot fully be utilized, and to provide a kind of take copper water-supply pipe as the method that nano ferriferrous oxide prepared by raw material.
Take copper water-supply pipe as the method that nano ferriferrous oxide prepared by raw material, specifically complete according to the following steps: one, prepare copper water-supply pipe powder: first by copper water-supply pipe seasoning, be then ground to particle diameter and be less than 100 μm, namely obtain copper water-supply pipe powder; Two, roasting: copper water-supply pipe powder is put into box electrothermal oven, with 5 DEG C/min heat-up rate from room temperature to 400 ~ 900 DEG C, and at temperature is 400 ~ 900 DEG C roasting 1h, then naturally cool to room temperature, obtain copper water-supply pipe after roasting; Three, acid leaching extraction: be that copper water-supply pipe after roasting adds in acid by 1:20 by solid-to-liquid ratio, low whipping speed is 400r/min and acidleach temperature is acid leaching extraction 1h ~ 3h at 50 ~ 90 DEG C, then vacuum filtration machine is utilized to carry out vacuum filtration, be washing composition again with distilled water, in conjunction with vacuum filtration, solid residue is repeatedly washed, washing is to the filtrate obtained for the last time is neutrality, and the filtrate obtained by vacuum filtration merges, and is acid leaching extraction thing; Four, centrifugation: the pH value of acid leaching extraction thing is adjusted to 13 by the NaOH solution utilizing concentration to be 2mol/L, then carries out centrifugation, obtains red-brown precipitation thing, is the presoma of magnetic ferroferric oxide nanoparticle; Five, nanometer process: the presoma of magnetic ferroferric oxide nanoparticle is dissolved in ethylene glycol, add anhydrous sodium acetate again, be react 720min ~ 1800min in the water heating kettle of 180 DEG C in temperature, externally-applied magnetic field is utilized to carry out solid-liquid separation, then distilled water and ethanol is adopted to carry out cross washing to solid successively, wash 6 times altogether, be finally be dried to constant weight under the nitrogen protection of 50 DEG C in temperature, namely obtain nano ferriferrous oxide; The quality of the presoma of the magnetic ferroferric oxide nanoparticle described in step 5 and the volume ratio of ethylene glycol are 1g:(70mL ~ 80mL); Fe in the presoma of the magnetic ferroferric oxide nanoparticle described in step 5
3+be 5:1 with the mol ratio of anhydrous sodium acetate.
Advantage of the present invention:
One, the present invention take copper water-supply pipe as nano ferriferrous oxide prepared by raw material, by changing mud particle diameter, maturing temperature, acid leaching extraction temperature, acid leaching extraction time, making abstraction reaction more abundant, thus obtaining maximum iron extracted amount;
Two, the present invention take copper water-supply pipe as nano ferriferrous oxide prepared by raw material, by a simple step solvent structure nano ferriferrous oxide particle, easy and simple to handle, generate without harmful by-products, avoid copper water-supply pipe and recycle the problem such as secondary pollution harm produced, and take copper water-supply pipe as the preparation cost that nano ferriferrous oxide prepared by raw material reduces nano ferriferrous oxide;
Three, the present invention utilizes the magnetic of Z 250, realizes magnetic particle easily and is separated with water body, by various functional materialss of preparation such as the coated means of modification, and can realize cycling and reutilization, more can be widely used in every field.
Accompanying drawing explanation
Fig. 1 is the X-ray diffraction spectrogram of the nano ferriferrous oxide that test one obtains;
Fig. 2 is the x-ray photoelectron spectroscopy figure of the nano ferriferrous oxide that test one obtains;
Fig. 3 is the scanning electron microscopic picture of the nano ferriferrous oxide that test one obtains;
Fig. 4 is the extraction leaching content histogram of different maturing temperature inorganic iron component;
Fig. 5 is the extraction leaching content histogram of different acidleach temperature inorganic iron component;
Fig. 6 is the extraction leaching content histogram of different leaching time inorganic iron component;
Fig. 7 is the X-ray diffraction spectrogram of the nano ferriferrous oxide that test 14 obtains;
Fig. 8 is the X-ray diffraction spectrogram of the nano ferriferrous oxide that test 15 obtains;
Fig. 9 is test 16 Homogeneous phase mixing suspension liquid photo;
Figure 10 is photo after test 16 magnet is separated.
Embodiment
Embodiment one: present embodiment is a kind of take copper water-supply pipe as the method that nano ferriferrous oxide prepared by raw material, specifically complete according to the following steps: one, prepare copper water-supply pipe powder: first by copper water-supply pipe seasoning, then be ground to particle diameter and be less than 100 μm, namely obtain copper water-supply pipe powder; Two, roasting: copper water-supply pipe powder is put into box electrothermal oven, with 5 DEG C/min heat-up rate from room temperature to 400 ~ 900 DEG C, and at temperature is 400 ~ 900 DEG C roasting 1h, then naturally cool to room temperature, obtain copper water-supply pipe after roasting; Three, acid leaching extraction: be that copper water-supply pipe after roasting adds in acid by 1:20 by solid-to-liquid ratio, low whipping speed is 400r/min and acidleach temperature is acid leaching extraction 1h ~ 3h at 50 ~ 90 DEG C, then vacuum filtration machine is utilized to carry out vacuum filtration, be washing composition again with distilled water, in conjunction with vacuum filtration, solid residue is repeatedly washed, washing is to the filtrate obtained for the last time is neutrality, and the filtrate obtained by vacuum filtration merges, and is acid leaching extraction thing; Four, centrifugation: the pH value of acid leaching extraction thing is adjusted to 13 by the NaOH solution utilizing concentration to be 2mol/L, then carries out centrifugation, obtains red-brown precipitation thing, is the presoma of magnetic ferroferric oxide nanoparticle; Five, nanometer process: the presoma of magnetic ferroferric oxide nanoparticle is dissolved in ethylene glycol, add anhydrous sodium acetate again, be react 720min ~ 1800min in the water heating kettle of 180 DEG C in temperature, externally-applied magnetic field is utilized to carry out solid-liquid separation, then distilled water and ethanol is adopted to carry out cross washing to solid successively, wash 6 times altogether, be finally be dried to constant weight under the nitrogen protection of 50 DEG C in temperature, namely obtain nano ferriferrous oxide; The quality of the presoma of the magnetic ferroferric oxide nanoparticle described in step 5 and the volume ratio of ethylene glycol are 1g:(70mL ~ 80mL); Fe in the presoma of the magnetic ferroferric oxide nanoparticle described in step 5
3+be 5:1 with the mol ratio of anhydrous sodium acetate.
Present embodiment take copper water-supply pipe as nano ferriferrous oxide prepared by raw material, by changing mud particle diameter, maturing temperature, acid leaching extraction temperature, acid leaching extraction time, making abstraction reaction more abundant, thus obtaining maximum iron extracted amount.
Present embodiment take copper water-supply pipe as nano ferriferrous oxide prepared by raw material, by a simple step solvent structure nano ferriferrous oxide particle, easy and simple to handle, generate without harmful by-products, avoid copper water-supply pipe and recycle the problem such as secondary pollution harm produced, and take copper water-supply pipe as the preparation cost that nano ferriferrous oxide prepared by raw material reduces nano ferriferrous oxide.
Present embodiment utilizes the magnetic of Z 250, realizes magnetic particle easily and is separated with water body, by various functional materialss of preparation such as the coated means of modification, and can realize cycling and reutilization, more can be widely used in every field.
Embodiment two: the difference of present embodiment and embodiment one is: the copper water-supply pipe described in step one is water purification plant's clarifier sludge.Other are identical with embodiment one.
Embodiment three: one of present embodiment and embodiment one or two difference is: the hydrochloric acid of to be concentration the be 2mol/L of the acid described in step 3.Other are identical with embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three difference is: the particle diameter of the nano ferriferrous oxide described in step 5 is 150nm ~ 250nm.Other are identical with embodiment one to three.
Adopt following verification experimental verification effect of the present invention
Test one: a kind of take copper water-supply pipe as the method that nano ferriferrous oxide prepared by raw material, specifically complete according to the following steps: one, prepare copper water-supply pipe powder: first by copper water-supply pipe seasoning, then be ground to particle diameter and be less than 100 μm, namely obtain copper water-supply pipe powder; Two, roasting: copper water-supply pipe powder is put into box electrothermal oven, with 5 DEG C/min heat-up rate from room temperature to 500 DEG C, and at temperature is 500 DEG C roasting 1h, then naturally cool to room temperature, obtain copper water-supply pipe after roasting; Three, acid leaching extraction: be that copper water-supply pipe after roasting adds in acid by 1:20 by solid-to-liquid ratio, low whipping speed is 400r/min and acidleach temperature is acid leaching extraction 3h at 90 DEG C, then vacuum filtration machine is utilized to carry out vacuum filtration, be washing composition again with distilled water, in conjunction with vacuum filtration, solid residue is repeatedly washed, washing is to the filtrate obtained for the last time is neutrality, and the filtrate obtained by vacuum filtration merges, and is acid leaching extraction thing; Four, centrifugation: the pH value of acid leaching extraction thing is adjusted to 13 by the NaOH solution utilizing concentration to be 2mol/L, then carries out centrifugation, obtains red-brown precipitation thing, is the presoma of magnetic ferroferric oxide nanoparticle; Five, nanometer process: the presoma of magnetic ferroferric oxide nanoparticle is dissolved in ethylene glycol, add anhydrous sodium acetate again, be react 1440min in the water heating kettle of 180 DEG C in temperature, externally-applied magnetic field is utilized to carry out solid-liquid separation, then distilled water and ethanol is adopted to carry out cross washing to solid successively, wash 6 times altogether, be finally be dried to constant weight under the nitrogen protection of 50 DEG C in temperature, namely obtain nano ferriferrous oxide; The quality of the presoma of the magnetic ferroferric oxide nanoparticle described in step 5 and the volume ratio of ethylene glycol are 1g:75mL; Fe in the presoma of the magnetic ferroferric oxide nanoparticle described in step 5
3+be 5:1 with the mol ratio of anhydrous sodium acetate.
Copper water-supply pipe described in this testing sequence one is water purification plant's clarifier sludge.
The hydrochloric acid of to be concentration the be 2mol/L of the acid described in this testing sequence three.
The particle diameter of the nano ferriferrous oxide described in this testing sequence five is 150nm ~ 250nm.
Fig. 1 is the X-ray diffraction spectrogram of the nano ferriferrous oxide that test one obtains, as can be seen from Figure 1, in 2 θ=30.1 °, the diffraction peak at 35.3 °, 43.1 °, 57.1 ° and 62.6 ° places is (220), (311), (400), (511) and (440) crystallographic plane diffraction peak of ferriferrous oxide nano-particle, illustrate that this material is Z 250, and ferriferrous oxide nano-particle is face-centred cubic structure.
Fig. 2 is the x-ray photoelectron spectroscopy figure of the nano ferriferrous oxide that test one obtains, its chemical constitution can be significantly found out from Fig. 2, the fignal center occurred in 284.6 and 532.5eV place in figure is respectively C1s and O1s peak, and the fignal center occurred at 710 ~ 740eV is then Fe2p peak.
Fig. 3 is the scanning electron microscopic picture of the nano ferriferrous oxide that test one obtains, and the nano ferriferrous oxide testing two preparations is as seen from Figure 3 that particle diameter is at 150 ~ 250nm spheroidal particle.
Test two: this test with test one difference is: in step 2, copper water-supply pipe powder is put into box electrothermal oven, with 5 DEG C/min heat-up rate from room temperature to 400 DEG C, and at temperature is 400 DEG C roasting 1h, then naturally cool to room temperature, obtain copper water-supply pipe after roasting.Other are identical with test one.
Test three: this test with test one difference is: in step 2, copper water-supply pipe powder is put into box electrothermal oven, with 5 DEG C/min heat-up rate from room temperature to 600 DEG C, and at temperature is 600 DEG C roasting 1h, then naturally cool to room temperature, obtain copper water-supply pipe after roasting.Other are identical with test one.
Test four: this test with test one difference is: in step 2, copper water-supply pipe powder is put into box electrothermal oven, with 5 DEG C/min heat-up rate from room temperature to 700 DEG C, and at temperature is 700 DEG C roasting 1h, then naturally cool to room temperature, obtain copper water-supply pipe after roasting.Other are identical with test one.
Test five: this test with test one difference is: in step 2, copper water-supply pipe powder is put into box electrothermal oven, with 5 DEG C/min heat-up rate from room temperature to 800 DEG C, and at temperature is 800 DEG C roasting 1h, then naturally cool to room temperature, obtain copper water-supply pipe after roasting.Other are identical with test one.
Test six: this test with test one difference is: in step 2, copper water-supply pipe powder is put into box electrothermal oven, with 5 DEG C/min heat-up rate from room temperature to 900 DEG C, and at temperature is 900 DEG C roasting 1h, then naturally cool to room temperature, obtain copper water-supply pipe after roasting.Other are identical with test one.
The extracted amount that the presoma 341.3mg/g (ironic hydroxide/copper water-supply pipe) of magnetic ferroferric oxide nanoparticle obtained according to step 4 and the copper water-supply pipe described in step one calculate inorganic iron component is 178.6mg/g (Fe
3+/ copper water-supply pipe), the extraction leaching content of the inorganic iron component of test one to six as shown in Figure 4, Fig. 4 is the extraction leaching content histogram of different maturing temperature inorganic iron component, as shown in Figure 4, the extraction leaching content of inorganic iron component reaches maximum when maturing temperature is 500 DEG C, increase along with temperature afterwards and reduce, when illustrating that maturing temperature is 500 DEG C, the extraction leaching content of inorganic iron component is the highest.
Test seven: this test with test a difference and be: be that copper water-supply pipe after roasting adds in acid by 1:20 by solid-to-liquid ratio in step 3, low whipping speed is 400r/min and acidleach temperature is acid leaching extraction 3h at 50 DEG C, then vacuum filtration machine is utilized to carry out vacuum filtration, be washing composition again with distilled water, in conjunction with vacuum filtration, solid residue is repeatedly washed, washing is to the filtrate obtained for the last time is neutrality, and the filtrate obtained by vacuum filtration merges, and is acid leaching extraction thing.Other are identical with test one.
Test eight: this test with test a difference and be: be that copper water-supply pipe after roasting adds in acid by 1:20 by solid-to-liquid ratio in step 3, low whipping speed is 400r/min and acidleach temperature is acid leaching extraction 3h at 60 DEG C, then vacuum filtration machine is utilized to carry out vacuum filtration, be washing composition again with distilled water, in conjunction with vacuum filtration, solid residue is repeatedly washed, washing is to the filtrate obtained for the last time is neutrality, and the filtrate obtained by vacuum filtration merges, and is acid leaching extraction thing.Other are identical with test one.
Test nine: this test with test a difference and be: be that copper water-supply pipe after roasting adds in acid by 1:20 by solid-to-liquid ratio in step 3, low whipping speed is 400r/min and acidleach temperature is acid leaching extraction 3h at 70 DEG C, then vacuum filtration machine is utilized to carry out vacuum filtration, be washing composition again with distilled water, in conjunction with vacuum filtration, solid residue is repeatedly washed, washing is to the filtrate obtained for the last time is neutrality, and the filtrate obtained by vacuum filtration merges, and is acid leaching extraction thing.Other are identical with test one.
Test ten: this test with test a difference and be: be that copper water-supply pipe after roasting adds in acid by 1:20 by solid-to-liquid ratio in step 3, low whipping speed is 400r/min and acidleach temperature is acid leaching extraction 3h at 80 DEG C, then vacuum filtration machine is utilized to carry out vacuum filtration, be washing composition again with distilled water, in conjunction with vacuum filtration, solid residue is repeatedly washed, washing is to the filtrate obtained for the last time is neutrality, and the filtrate obtained by vacuum filtration merges, and is acid leaching extraction thing.Other are identical with test one.
The extracted amount that the presoma 341.3mg/g (ironic hydroxide/copper water-supply pipe) of magnetic ferroferric oxide nanoparticle obtained according to step 4 and the copper water-supply pipe described in step one calculate inorganic iron component is 178.6mg/g (Fe
3+/ copper water-supply pipe), the extraction leaching content of the inorganic iron component of test one, seven to ten as shown in Figure 5, Fig. 5 is the extraction leaching content histogram of different acidleach temperature inorganic iron component, as shown in Figure 5, along with the rising of acidleach temperature, the extraction leaching content of inorganic iron component constantly raises, and when acidleach temperature is 90 DEG C, the extraction leaching content of inorganic iron component is the highest.
Test 11: this test with test one difference is: be that copper water-supply pipe after roasting adds in acid by 1:20 by solid-to-liquid ratio in step 3, low whipping speed is 400r/min and acidleach temperature is acid leaching extraction 1.5h at 90 DEG C, then vacuum filtration machine is utilized to carry out vacuum filtration, be washing composition again with distilled water, in conjunction with vacuum filtration, solid residue is repeatedly washed, washing is to the filtrate obtained for the last time is neutrality, and the filtrate obtained by vacuum filtration merges, and is acid leaching extraction thing.Other are identical with test one.
Test 12: this test with test one difference is: be that copper water-supply pipe after roasting adds in acid by 1:20 by solid-to-liquid ratio in step 3, low whipping speed is 400r/min and acidleach temperature is acid leaching extraction 2.0h at 90 DEG C, then vacuum filtration machine is utilized to carry out vacuum filtration, be washing composition again with distilled water, in conjunction with vacuum filtration, solid residue is repeatedly washed, washing is to the filtrate obtained for the last time is neutrality, and the filtrate obtained by vacuum filtration merges, and is acid leaching extraction thing.Other are identical with test one.
Test 13: this test with test one difference is: be that copper water-supply pipe after roasting adds in acid by 1:20 by solid-to-liquid ratio in step 3, low whipping speed is 400r/min and acidleach temperature is acid leaching extraction 2.5h at 90 DEG C, then vacuum filtration machine is utilized to carry out vacuum filtration, be washing composition again with distilled water, in conjunction with vacuum filtration, solid residue is repeatedly washed, washing is to the filtrate obtained for the last time is neutrality, and the filtrate obtained by vacuum filtration merges, and is acid leaching extraction thing.Other are identical with test one.
The extracted amount that the presoma 341.3mg/g (ironic hydroxide/copper water-supply pipe) of magnetic ferroferric oxide nanoparticle obtained according to step 4 and the copper water-supply pipe described in step one calculate inorganic iron component is 178.6mg/g (Fe
3+/ copper water-supply pipe), as shown in Figure 6, Fig. 6 is the extraction leaching content histogram of different leaching time inorganic iron component to the extraction leaching content of the inorganic iron component of test one, 10 one to ten three, as shown in Figure 6, reaction times, when reaching 3h, the extraction leaching content of inorganic iron component reached balance.
Test 14: a kind of take copper water-supply pipe as the method that nano ferriferrous oxide prepared by raw material, specifically complete according to the following steps: one, prepare copper water-supply pipe powder: first by copper water-supply pipe seasoning, then be ground to particle diameter and be less than 100 μm, namely obtain copper water-supply pipe powder; Two, roasting: copper water-supply pipe powder is put into box electrothermal oven, with 5 DEG C/min heat-up rate from room temperature to 500 DEG C, and at temperature is 500 DEG C roasting 1h, then naturally cool to room temperature, obtain copper water-supply pipe after roasting; Three, acid leaching extraction: be that copper water-supply pipe after roasting adds in acid by 1:20 by solid-to-liquid ratio, low whipping speed is 400r/min and acidleach temperature is acid leaching extraction 3h at 90 DEG C, then vacuum filtration machine is utilized to carry out vacuum filtration, be washing composition again with distilled water, in conjunction with vacuum filtration, solid residue is repeatedly washed, washing is to the filtrate obtained for the last time is neutrality, and the filtrate obtained by vacuum filtration merges, and is acid leaching extraction thing; Four, centrifugation: the pH value of acid leaching extraction thing is adjusted to 13 by the NaOH solution utilizing concentration to be 2mol/L, then carries out centrifugation, obtains red-brown precipitation thing; Five, the dissolving with hydrochloric acid red-brown precipitation thing utilizing concentration to be 2mol/L, then concentrate, obtain iron(ic) chloride, be the presoma of magnetic ferroferric oxide nanoparticle; Six, nanometer process: the presoma of magnetic ferroferric oxide nanoparticle is dissolved in ethylene glycol, add anhydrous sodium acetate again, be react 1440min in the water heating kettle of 180 DEG C in temperature, externally-applied magnetic field is utilized to carry out solid-liquid separation, then distilled water and ethanol is adopted to carry out cross washing to solid successively, wash 6 times altogether, be finally be dried to constant weight under the nitrogen protection of 50 DEG C in temperature, namely obtain nano ferriferrous oxide; The quality of the presoma of the magnetic ferroferric oxide nanoparticle described in step 6 and the volume ratio of ethylene glycol are 1g:75mL; Fe in the presoma of the magnetic ferroferric oxide nanoparticle described in step 6
3+be 5:1 with the mol ratio of anhydrous sodium acetate.
Copper water-supply pipe described in this testing sequence one is water purification plant's clarifier sludge.
The hydrochloric acid of to be concentration the be 2mol/L of the acid described in this testing sequence three.
Fig. 7 is the X-ray diffraction spectrogram of the nano ferriferrous oxide that test 14 obtains, as can see from Figure 7 except the oxidation peak of Z 250 also has the assorted peak of a lot of ferric oxide, illustrate that this material is containing some Z 250 crystal, but Z 250 crystallinity not test a gained magnetic ferroferric oxide nanoparticle good.
Test 15: this test with the difference of test 14 is: the sulfuric acid dissolution red-brown precipitation thing utilizing concentration to be 2mol/L in step 5, then concentrates, and obtains ferric sulfate, is the presoma of magnetic ferroferric oxide nanoparticle.Other are identical with test 14.
Fig. 8 is the X-ray diffraction spectrogram of the nano ferriferrous oxide that test 15 obtains, as can see from Figure 8 the oxidation peak intensity of Z 250 and Fig. 1 more relatively low, alike with the diffraction peak location comparison in Fig. 7, though this material of same explanation is containing some Z 250, Z 250 crystallinity does not test the good of gained in.
Test 16: magnetometric analysis: add in 20mL distilled water by the nano ferriferrous oxide of 0.1g test one preparation, ultrasonic disperse 5min, be uniformly mixed suspension liquid, strong magnet is placed on Reagent Tube side, can carry out solid-liquid separation.
Fig. 9 is test 16 Homogeneous phase mixing suspension liquid photo, Figure 10 is photo after magnet is separated, known by Fig. 9 and Figure 10, the nano ferriferrous oxide of test one preparation fully can be separated with distilled water, proves that nano ferriferrous oxide prepared by the present invention fully can be separated with distilled water.
Claims (1)
1. one kind is the method that nano ferriferrous oxide prepared by raw material with copper water-supply pipe, it is characterized in that a kind of method with copper water-supply pipe being nano ferriferrous oxide prepared by raw material completes according to the following steps: one, prepare copper water-supply pipe powder: first by copper water-supply pipe seasoning, then be ground to particle diameter and be less than 100 μm, namely obtain copper water-supply pipe powder; Two, roasting: copper water-supply pipe powder is put into box electrothermal oven, with 5 DEG C/min heat-up rate from room temperature to 400 ~ 900 DEG C, and at temperature is 400 ~ 900 DEG C roasting 1h, then naturally cool to room temperature, obtain copper water-supply pipe after roasting; Three, acid leaching extraction: be that copper water-supply pipe after roasting adds in acid by 1:20 by solid-to-liquid ratio, low whipping speed is 400r/min and acidleach temperature is acid leaching extraction 1h ~ 3h at 50 ~ 90 DEG C, then vacuum filtration machine is utilized to carry out vacuum filtration, be washing composition again with distilled water, in conjunction with vacuum filtration, solid residue is repeatedly washed, washing is to the filtrate obtained for the last time is neutrality, and the filtrate obtained by vacuum filtration merges, and is acid leaching extraction thing; Four, centrifugation: the pH value of acid leaching extraction thing is adjusted to 13 by the NaOH solution utilizing concentration to be 2mol/L, then carries out centrifugation, obtains red-brown precipitation thing, is the presoma of magnetic ferroferric oxide nanoparticle; Five, nanometer process: the presoma of magnetic ferroferric oxide nanoparticle is dissolved in ethylene glycol, add anhydrous sodium acetate again, be react 720min ~ 1800min in the water heating kettle of 180 DEG C in temperature, externally-applied magnetic field is utilized to carry out solid-liquid separation, then distilled water and ethanol is adopted to carry out cross washing to solid successively, wash 6 times altogether, be finally be dried to constant weight under the nitrogen protection of 50 DEG C in temperature, namely obtain nano ferriferrous oxide; The quality of the presoma of the magnetic ferroferric oxide nanoparticle described in step 5 and the volume ratio of ethylene glycol are 1g:(70mL ~ 80mL); Fe in the presoma of the magnetic ferroferric oxide nanoparticle described in step 5
3+be 5:1 with the mol ratio of anhydrous sodium acetate;
Copper water-supply pipe described in step one is water purification plant's clarifier sludge;
The hydrochloric acid of to be concentration the be 2mol/L of the acid described in step 3;
The particle diameter of the nano ferriferrous oxide described in step 5 is 150nm ~ 250nm.
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|---|---|---|---|---|
| CN101885512A (en) * | 2010-01-05 | 2010-11-17 | 河北医科大学 | Hydrothermal synthesis process of magnetic ferroferric oxide nanometer ultrafine particles in non-N2 atomosphere |
| CN102358648A (en) * | 2011-09-20 | 2012-02-22 | 卢玉柱 | Technology for recycling of sludge obtained after neutralizing treatment of steel and iron pickling wastewater and recycling ferroferric oxide |
| CN102826614A (en) * | 2012-08-31 | 2012-12-19 | 长春工程学院 | Method for preparing iron oxide black by recovering iron in sludge water from biological iron and manganese removal water plant |
| CN103451422A (en) * | 2013-09-03 | 2013-12-18 | 天津城建大学 | Method for preparing iron oxide for iron making by using steel acid-washing wastewater sludge |
| CN103787424A (en) * | 2014-01-24 | 2014-05-14 | 东北师范大学 | Method for preparing nano Fe3O4 by using underground water plant iron mud as raw material |
-
2014
- 2014-12-04 CN CN201410735007.8A patent/CN104445436B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101885512A (en) * | 2010-01-05 | 2010-11-17 | 河北医科大学 | Hydrothermal synthesis process of magnetic ferroferric oxide nanometer ultrafine particles in non-N2 atomosphere |
| CN102358648A (en) * | 2011-09-20 | 2012-02-22 | 卢玉柱 | Technology for recycling of sludge obtained after neutralizing treatment of steel and iron pickling wastewater and recycling ferroferric oxide |
| CN102826614A (en) * | 2012-08-31 | 2012-12-19 | 长春工程学院 | Method for preparing iron oxide black by recovering iron in sludge water from biological iron and manganese removal water plant |
| CN103451422A (en) * | 2013-09-03 | 2013-12-18 | 天津城建大学 | Method for preparing iron oxide for iron making by using steel acid-washing wastewater sludge |
| CN103787424A (en) * | 2014-01-24 | 2014-05-14 | 东北师范大学 | Method for preparing nano Fe3O4 by using underground water plant iron mud as raw material |
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| CN104445436A (en) | 2015-03-25 |
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