CN105174325A - Method for preparing furfural wastewater treating agent by means of furfural residues - Google Patents
Method for preparing furfural wastewater treating agent by means of furfural residues Download PDFInfo
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- CN105174325A CN105174325A CN201510626267.6A CN201510626267A CN105174325A CN 105174325 A CN105174325 A CN 105174325A CN 201510626267 A CN201510626267 A CN 201510626267A CN 105174325 A CN105174325 A CN 105174325A
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- furfural
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- charing
- furfural dregs
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- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 title claims abstract description 232
- 239000002351 wastewater Substances 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 26
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 24
- 238000004065 wastewater treatment Methods 0.000 claims abstract description 22
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Chemical compound CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims description 22
- 238000000855 fermentation Methods 0.000 claims description 19
- 230000004151 fermentation Effects 0.000 claims description 19
- 239000002245 particle Substances 0.000 claims description 18
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 13
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 12
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 12
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000000706 filtrate Substances 0.000 claims description 12
- 238000009413 insulation Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000000047 product Substances 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 8
- 238000006424 Flood reaction Methods 0.000 claims description 6
- 239000001888 Peptone Substances 0.000 claims description 6
- 108010080698 Peptones Proteins 0.000 claims description 6
- 239000004952 Polyamide Substances 0.000 claims description 6
- 238000007605 air drying Methods 0.000 claims description 6
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 6
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 6
- 238000001125 extrusion Methods 0.000 claims description 6
- 238000007654 immersion Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 6
- 239000013618 particulate matter Substances 0.000 claims description 6
- 235000019319 peptone Nutrition 0.000 claims description 6
- 229920002647 polyamide Polymers 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 239000010802 sludge Substances 0.000 claims description 6
- 239000011780 sodium chloride Substances 0.000 claims description 6
- 239000004408 titanium dioxide Substances 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- AIUDWMLXCFRVDR-UHFFFAOYSA-N dimethyl 2-(3-ethyl-3-methylpentyl)propanedioate Chemical class CCC(C)(CC)CCC(C(=O)OC)C(=O)OC AIUDWMLXCFRVDR-UHFFFAOYSA-N 0.000 claims description 3
- 229940066779 peptones Drugs 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims 1
- 239000002699 waste material Substances 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 5
- 229920005610 lignin Polymers 0.000 abstract description 2
- 238000012986 modification Methods 0.000 abstract description 2
- 230000004048 modification Effects 0.000 abstract description 2
- 125000004423 acyloxy group Chemical group 0.000 abstract 1
- 238000010000 carbonizing Methods 0.000 abstract 1
- -1 methacryloyl Chemical group 0.000 abstract 1
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000001704 evaporation Methods 0.000 description 4
- 239000002893 slag Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 150000001299 aldehydes Chemical class 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000010170 biological method Methods 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 description 1
- 239000005695 Ammonium acetate Substances 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 241000521257 Hydrops Species 0.000 description 1
- 239000000020 Nitrocellulose Substances 0.000 description 1
- 206010030113 Oedema Diseases 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229940043376 ammonium acetate Drugs 0.000 description 1
- 235000019257 ammonium acetate Nutrition 0.000 description 1
- HIVLDXAAFGCOFU-UHFFFAOYSA-N ammonium hydrosulfide Chemical compound [NH4+].[SH-] HIVLDXAAFGCOFU-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 239000001175 calcium sulphate Substances 0.000 description 1
- 235000011132 calcium sulphate Nutrition 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethanethiol Chemical compound CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 230000002906 microbiologic effect Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000009280 upflow anaerobic sludge blanket technology Methods 0.000 description 1
Abstract
The invention discloses a method for preparing a furfural wastewater treating agent by means of furfural residues, and belongs to the technical field of wastewater treatment. The method comprises the steps that firstly, the furfural residues are neutralized with a sodium hydroxide solution, and part of substances such as lignin are removed, so that the gaps of the furfural residues are developed; secondly, modification is performed on the furfural residues by adding substances such as methacryloyl acyloxy propyl trimethoxy silane and diacetone alcohol to enable the furfual residues to simultaneously achieve the high acidity resistance, then carbonizing and fermenting are performed, and the furfural wastewater treating agent is prepared. The method is easy to operate and practicable, the furfural wastewater treating agent takes the furfural residues as the raw mateirls, comprehensive utilization of waste is achieved, the operation cost is reduced, operation is easy and reliable, secondary pollution cannot be caused, the final measured COD removing rate of furfural wastewater is above 90 percent, and the BOD removing rate is above 98.7 percent.
Description
Technical field
The invention discloses a kind of method utilizing furfural dregs to prepare furfural waste-water treatment agent, belong to technical field of waste water processing.
Background technology
Furfural has another name called furtural, is one of main raw material in synthetic organic chemical manufacturing industry, and its purposes widely, can be used for making synthetic resins, by reactions such as hydrogenation, oxidation, condensations to produce a large amount of derivative.It is also excellent solvent, can be used for refining petroleum, bright stock, refines grease and dissolves nitrocellulose etc., or the raw material of pharmacy and multiple organic synthesis and reagent.It is a kind of important basic organic chemical industry raw material.World's furfural production ability is about 500,000 tons/a, and China's output is 350,000 tons/a.In furfural production process, produce with a large amount of furfuraldehyde waste slag, furfural product per ton discharges more than 10 tons residues, China discharges nearly 30,000,000 tons of furfuraldehyde waste slag every year, cause the wasting of resources, and produce a large amount of waste water in furfural production process, produce the furfural production device discharge acid-bearing wastewater about 1.5 ten thousand tons of 1000 tons per year.Waste water mainly comes from liquid under mao aldehyde distillation tower, and temperature is high, and along with steam, belongs to air water miscellany.Cooled water sample stench, pale yellow transparent, pH value is approximately 4, COD and is about 10000 ~ 20000mg/L, and BOD is approximately 2500 ~ 3000mg/L, and biodegradability is poor, if do not process this waste water, directly outer row, must cause serious environmental pollution.
Furfural waste-water has the features such as highly acidity, high density, corrodibility is strong, biodegradability is poor, be difficult to reach desirable treatment effect with single treatment process, in practice, many employing built-up type treatment process, comprise the kinds of processes of biological method, phase transfer method, double-effect evaporation method.
First biological method refers to and first hair aldehyde base product 80 ~ 90 DEG C of furfural waste-waters is out cooled to less than 45 DEG C, uses alkali lye adjust ph, then regulates concentration according to content organic in waste water, adds nutritive salt in proportion.Waste water after deployed squeezes into UASB reactor through water pump, and waste water is through microbiological anaerobic biochemical treatment, and organic impurity is progressively degraded, but the method is difficult to continuous operation, easily produces odor pollution; The phase transfer method of next refers to and is loaded in phase transition post by multifunctional macromolecule polymkeric substance, and waste water is after this device, and acetic acid and other impurity transfer to solid phase immediately, exports as clear as crystal neutral water, returns boiler use as softening water.High molecular polymer ammonia separation and regenerating, obtains the liquid containing hydrops ammonium acetate and furfural, respectively evaporation concentration, obtain Ammoniom-Acetate concentrated solution and hair aldehyde, process obtains by product sulphur ammonium and product furfural further, but the method consumption is large, processing cost is high, operation and difficult management; Last double-effect evaporation method is by sewage Wingdale or neutralization with lime pH value to 7 ~ 8, enter into decompression double-effect evaporation system afterwards, by dilute solution ebuillition of heated, wherein moisture is made to vaporize and reach the object of concentrated solution, but the method shortcoming produces a large amount of calcium salts as calcium sulphate solid waste processing waste water while, produces secondary pollution.
Summary of the invention
The technical problem that the present invention mainly solves: there is highly acidity for current furfural waste-water, high density, the features such as corrodibility is strong, biodegradability is poor, and though waste water content can be made to decrease during traditional disposal methods, but it is lower still to there is clearance, operation cost is higher and produce the problem of secondary pollution, provide a kind of method utilizing furfural dregs to prepare furfural waste-water treatment agent, first the method utilizes in sodium hydroxide solution and furfural dregs, and remove the materials such as partial lignin, make its space flourishing, add methacryloxypropyl trimethoxy silane again, the materials such as diacetone alcohol carry out modification to furfural dregs, make it have resistance to peracidity simultaneously, carbonize again, the methods such as fermentation prepare furfural waste-water treatment agent.This furfural waste-water treatment agent is starting material with furfuraldehyde waste slag, not only achieves comprehensive utilization of waste materials, and saved running cost, operation is simple and reliable, and can not cause secondary pollution, finally makes furfural waste-water clearance reach more than 90%.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:
(1) get furfural dregs and put into container, add sodium hydroxide solution immersion furfural dregs 10 ~ 15min that massfraction is 10 ~ 20% wherein, be warming up to 55 ~ 60 DEG C again, filter after stirring 1 ~ 2h, the furfural dregs of gained is put into baking oven 20 ~ 30min, temperature is set as 65 ~ 70 DEG C, then takes out and is cooled to room temperature;
(2) furfural dregs of above-mentioned gained is put into container, add methacryloxypropyl trimethoxy silane wherein and soak furfural dregs, add 60 ~ 70 order cerium oxide of furfural dregs quality 2 ~ 4% more respectively, 80 ~ 90 order titanium dioxide of furfural dregs quality 1 ~ 2%, the polyamide wax of furfural dregs quality 0.2 ~ 0.6% and the diacetone alcohol of methacryloxypropyl trimethoxy silane volume 20 ~ 30%, at temperature is 70 ~ 80 DEG C, stir 20 ~ 30min, then filter after leaving standstill 1 ~ 2h, obtain filtrate;
(3) filtrate of above-mentioned gained is put into extrusion machine and be squeezed into block, put it in charring furnace, first temperature is set as 200 ~ 280 DEG C, insulation 20 ~ 30min, again temperature is risen to 320 ~ 420 DEG C, insulation 40 ~ 45min, then rises to 800 ~ 850 DEG C by temperature, keep temperature 2 ~ 3h, then taken out and be cooled to room temperature;
(4) the above-mentioned charing block being cooled to room temperature is put into pulverizer and be ground into 70 ~ 80 order particles, put it into again in encloses container, re-using temperature is that the superheated vapour carrying 100 ~ 110 order calcium carbonate of charing block quality 10 ~ 15% of 900 ~ 1000 DEG C pours in container, when container inner pressure rises to 0.5 ~ 0.6MPa, stop being filled with superheated vapour, stir 30 ~ 35min, speed setting is 1500 ~ 2000r/min, then pressure release is to standard atmospheric pressure, is taken out by charing particle and is cooled to room temperature;
(5) the above-mentioned charing particle being cooled to room temperature is put into fermentation vat, add the river sludge containing furfural waste-water wherein, add-on is 80 ~ 90% of charing granular mass, add 10 ~ 20% extractum carniss of charing granular mass and 15 ~ 35% peptones of charing granular mass more respectively, then adding massfraction is wherein that 20% sodium chloride solution floods mixture 0.5 ~ 1cm, fermentation 10 ~ 15 days is stirred in sealing, and temperature remains 30 ~ 35 DEG C, and speed setting is 150 ~ 200r/min;
(6) after above-mentioned fermentation ends, remove fermented liquid, rinse fermented product 2 ~ 3 times with water, then natural air drying, puts into pulverizer and is ground into 70 ~ 80 order particulate matter, can obtain furfural waste-water treatment agent.
Application method of the present invention is: the furfural waste-water treatment agent obtained by the present invention is put into pending furfural waste-water, wherein every 1 ~ 2t furfural waste-water adds 80 ~ 100mg furfural waste-water treatment agent, after stirring afterwards, leave standstill 30 ~ 45min, detect with detector, the COD recording furfural waste-water has been reduced to 500 ~ 800mg/L from 10000 ~ 20000mg/L, and clearance reaches more than 95%, BOD has been reduced to 20 ~ 40mg/L from 2500 ~ 3000mg/L, and clearance reaches more than 98.7%.
The invention has the beneficial effects as follows:
(1) this furfural waste-water treatment agent is starting material with furfuraldehyde waste slag, not only achieves comprehensive utilization of waste materials, and has saved running cost;
(2) not only operation is simple and reliable, and can not cause secondary pollution, finally makes furfural waste-water clearance reach more than 90%.
Embodiment
First get furfural dregs and put into container, add sodium hydroxide solution immersion furfural dregs 10 ~ 15min that massfraction is 10 ~ 20% wherein, be warming up to 55 ~ 60 DEG C again, filter after stirring 1 ~ 2h, the furfural dregs of gained is put into baking oven 20 ~ 30min, temperature is set as 65 ~ 70 DEG C, then takes out and is cooled to room temperature; Then the furfural dregs of above-mentioned gained is put into container, add methacryloxypropyl trimethoxy silane wherein and soak furfural dregs, add 60 ~ 70 order cerium oxide of furfural dregs quality 2 ~ 4% more respectively, 80 ~ 90 order titanium dioxide of furfural dregs quality 1 ~ 2%, the polyamide wax of furfural dregs quality 0.2 ~ 0.6% and the diacetone alcohol of methacryloxypropyl trimethoxy silane volume 20 ~ 30%, at temperature is 70 ~ 80 DEG C, stir 20 ~ 30min, then filter after leaving standstill 1 ~ 2h, obtain filtrate; Subsequently the filtrate of above-mentioned gained is put into extrusion machine and be squeezed into block, put it in charring furnace, first temperature is set as 200 ~ 280 DEG C, insulation 20 ~ 30min, again temperature is risen to 320 ~ 420 DEG C, insulation 40 ~ 45min, then rises to 800 ~ 850 DEG C by temperature, keep temperature 2 ~ 3h, then taken out and be cooled to room temperature; Afterwards the above-mentioned charing block being cooled to room temperature is put into pulverizer and be ground into 70 ~ 80 order particles, put it into again in encloses container, re-using temperature is that the superheated vapour carrying 100 ~ 110 order calcium carbonate of charing block quality 10 ~ 15% of 900 ~ 1000 DEG C pours in container, when container inner pressure rises to 0.5 ~ 0.6MPa, stop being filled with superheated vapour, stir 30 ~ 35min, speed setting is 1500 ~ 2000r/min, then pressure release is to standard atmospheric pressure, is taken out by charing particle and is cooled to room temperature; Next the above-mentioned charing particle being cooled to room temperature is put into fermentation vat, add the river sludge containing furfural waste-water wherein, add-on is 80 ~ 90% of charing granular mass, add 10 ~ 20% extractum carniss of charing granular mass and 15 ~ 35% peptones of charing granular mass more respectively, then adding massfraction is wherein that 20% sodium chloride solution floods mixture 0.5 ~ 1cm, fermentation 10 ~ 15 days is stirred in sealing, temperature remains 30 ~ 35 DEG C, and speed setting is 150 ~ 200r/min; Finally after above-mentioned fermentation ends, remove fermented liquid, rinse fermented product 2 ~ 3 times with water, then natural air drying, puts into pulverizer and is ground into 70 ~ 80 order particulate matter, can obtain furfural waste-water treatment agent.
Example 1
First get furfural dregs and put into container, add the sodium hydroxide solution immersion furfural dregs 10min that massfraction is 10% wherein, then be warming up to 55 DEG C, filter after stirring 1h, the furfural dregs of gained is put into baking oven 20min, and temperature is set as 65 DEG C, then takes out and is cooled to room temperature; Then the furfural dregs of above-mentioned gained is put into container, add methacryloxypropyl trimethoxy silane wherein and soak furfural dregs, add 60 order cerium oxide of furfural dregs quality 2% more respectively, 80 order titanium dioxide of furfural dregs quality 1%, the polyamide wax of furfural dregs quality 0.2% and the diacetone alcohol of methacryloxypropyl trimethoxy silane volume 20%, at temperature is 70 DEG C, stir 20min, then filter after leaving standstill 1h, obtain filtrate; Subsequently the filtrate of above-mentioned gained is put into extrusion machine and be squeezed into block, put it in charring furnace, first temperature is set as 200 DEG C, insulation 20min, then temperature is risen to 320 DEG C, insulation 40min, then temperature is risen to 800 DEG C, keep temperature 2h, then taken out and be cooled to room temperature; Afterwards the above-mentioned charing block being cooled to room temperature is put into pulverizer and be ground into 70 order particles, put it into again in encloses container, re-using temperature is that the superheated vapour carrying 100 order calcium carbonate of charing block quality 10% of 900 DEG C pours in container, when container inner pressure rises to 0.5MPa, stop being filled with superheated vapour, stir 30min, speed setting is 1500r/min, then pressure release is to standard atmospheric pressure, is taken out by charing particle and is cooled to room temperature; Next the above-mentioned charing particle being cooled to room temperature is put into fermentation vat, add the river sludge containing furfural waste-water wherein, add-on is 80% of charing granular mass, add 10% extractum carnis of charing granular mass and 15% peptone of charing granular mass more respectively, then adding massfraction is wherein that 20% sodium chloride solution floods mixture 0.5cm, fermentation 10 days is stirred in sealing, and temperature remains 30 DEG C, and speed setting is 150r/min; Finally after above-mentioned fermentation ends, remove fermented liquid, rinse fermented product 2 times with water, then natural air drying, puts into pulverizer and is ground into 70 order particulate matter, can obtain furfural waste-water treatment agent.
During this example operation, furfural waste-water treatment agent obtained by the present invention is put into pending furfural waste-water, wherein every 1t furfural waste-water adds 80mg furfural waste-water treatment agent, after stirring afterwards, leave standstill 30min, detect with detector, the COD recording furfural waste-water has been reduced to 500mg/L from 10000mg/L, clearance reaches 95%, BOD and has been reduced to 20mg/L from 2500mg/L, and clearance reaches 98.7%.
Example 2
First get furfural dregs and put into container, add the sodium hydroxide solution immersion furfural dregs 13min that massfraction is 15% wherein, then be warming up to 58 DEG C, filter after stirring 1.5h, the furfural dregs of gained is put into baking oven 25min, and temperature is set as 68 DEG C, then takes out and is cooled to room temperature; Then the furfural dregs of above-mentioned gained is put into container, add methacryloxypropyl trimethoxy silane wherein and soak furfural dregs, add 65 order cerium oxide of furfural dregs quality 3% more respectively, 85 order titanium dioxide of furfural dregs quality 1.5%, the polyamide wax of furfural dregs quality 0.5% and the diacetone alcohol of methacryloxypropyl trimethoxy silane volume 25%, at temperature is 72 DEG C, stir 25min, then filter after leaving standstill 1.5h, obtain filtrate; Subsequently the filtrate of above-mentioned gained is put into extrusion machine and be squeezed into block, put it in charring furnace, first temperature is set as 250 DEG C, insulation 25min, then temperature is risen to 380 DEG C, insulation 43min, then temperature is risen to 830 DEG C, keep temperature 2.5h, then taken out and be cooled to room temperature; Afterwards the above-mentioned charing block being cooled to room temperature is put into pulverizer and be ground into 75 order particles, put it into again in encloses container, re-using temperature is that the superheated vapour carrying 105 order calcium carbonate of charing block quality 13% of 950 DEG C pours in container, when container inner pressure rises to 0.55MPa, stop being filled with superheated vapour, stir 33min, speed setting is 1800r/min, then pressure release is to standard atmospheric pressure, is taken out by charing particle and is cooled to room temperature; Next the above-mentioned charing particle being cooled to room temperature is put into fermentation vat, add the river sludge containing furfural waste-water wherein, add-on is 85% of charing granular mass, add 15% extractum carnis of charing granular mass and 30% peptone of charing granular mass more respectively, then adding massfraction is wherein that 20% sodium chloride solution floods mixture 0.8cm, fermentation 13 days is stirred in sealing, and temperature remains 33 DEG C, and speed setting is 180r/min; Finally after above-mentioned fermentation ends, remove fermented liquid, rinse fermented product 2.5 times with water, then natural air drying, puts into pulverizer and is ground into 75 order particulate matter, can obtain furfural waste-water treatment agent.
During this example operation, furfural waste-water treatment agent obtained by the present invention is put into pending furfural waste-water, wherein every 1.5t furfural waste-water adds 90mg furfural waste-water treatment agent, after stirring afterwards, leave standstill 40min, detect with detector, the COD recording furfural waste-water has been reduced to 650mg/L from 15000mg/L, clearance reaches 95.7%, BOD and has been reduced to 30mg/L from 2800mg/L, and clearance reaches 98.9%.
Example 3
First get furfural dregs and put into container, add the sodium hydroxide solution immersion furfural dregs 15min that massfraction is 20% wherein, then be warming up to 60 DEG C, filter after stirring 2h, the furfural dregs of gained is put into baking oven 30min, and temperature is set as 70 DEG C, then takes out and is cooled to room temperature; Then the furfural dregs of above-mentioned gained is put into container, add methacryloxypropyl trimethoxy silane wherein and soak furfural dregs, add 70 order cerium oxide of furfural dregs quality 4% more respectively, 90 order titanium dioxide of furfural dregs quality 1%, the polyamide wax of furfural dregs quality 0.6% and the diacetone alcohol of methacryloxypropyl trimethoxy silane volume 30%, at temperature is 80 DEG C, stir 30min, then filter after leaving standstill 2h, obtain filtrate; Subsequently the filtrate of above-mentioned gained is put into extrusion machine and be squeezed into block, put it in charring furnace, first temperature is set as 280 DEG C, insulation 30min, then temperature is risen to 420 DEG C, insulation 45min, then temperature is risen to 850 DEG C, keep temperature 3h, then taken out and be cooled to room temperature; Afterwards the above-mentioned charing block being cooled to room temperature is put into pulverizer and be ground into 80 order particles, put it into again in encloses container, re-using temperature is that the superheated vapour carrying 110 order calcium carbonate of charing block quality 15% of 1000 DEG C pours in container, when container inner pressure rises to 0.6MPa, stop being filled with superheated vapour, stir 35min, speed setting is 2000r/min, then pressure release is to standard atmospheric pressure, is taken out by charing particle and is cooled to room temperature; Next the above-mentioned charing particle being cooled to room temperature is put into fermentation vat, add the river sludge containing furfural waste-water wherein, add-on is 90% of charing granular mass, add 20% extractum carnis of charing granular mass and 35% peptone of charing granular mass more respectively, then adding massfraction is wherein that 20% sodium chloride solution floods mixture 1cm, fermentation 15 days is stirred in sealing, and temperature remains 35 DEG C, and speed setting is 200r/min; Finally after above-mentioned fermentation ends, remove fermented liquid, rinse fermented product 3 times with water, then natural air drying, puts into pulverizer and is ground into 80 order particulate matter, can obtain furfural waste-water treatment agent.
During this example operation, furfural waste-water treatment agent obtained by the present invention is put into pending furfural waste-water, wherein every 2t furfural waste-water adds 100mg furfural waste-water treatment agent, after stirring afterwards, leave standstill 45min, detect with detector, the COD recording furfural waste-water has been reduced to 800mg/L from 20000mg/L, clearance reaches 96%, BOD and has been reduced to 40mg/L from 3000mg/L, and clearance reaches 99.2%.
Claims (1)
1. utilize furfural dregs to prepare a method for furfural waste-water treatment agent, it is characterized in that concrete preparation process is:
(1) get furfural dregs and put into container, add sodium hydroxide solution immersion furfural dregs 10 ~ 15min that massfraction is 10 ~ 20% wherein, be warming up to 55 ~ 60 DEG C again, filter after stirring 1 ~ 2h, the furfural dregs of gained is put into baking oven 20 ~ 30min, temperature is set as 65 ~ 70 DEG C, then takes out and is cooled to room temperature;
(2) furfural dregs of above-mentioned gained is put into container, add methacryloxypropyl trimethoxy silane wherein and soak furfural dregs, add 60 ~ 70 order cerium oxide of furfural dregs quality 2 ~ 4% more respectively, 80 ~ 90 order titanium dioxide of furfural dregs quality 1 ~ 2%, the polyamide wax of furfural dregs quality 0.2 ~ 0.6% and the diacetone alcohol of methacryloxypropyl trimethoxy silane volume 20 ~ 30%, at temperature is 70 ~ 80 DEG C, stir 20 ~ 30min, then filter after leaving standstill 1 ~ 2h, obtain filtrate;
(3) filtrate of above-mentioned gained is put into extrusion machine and be squeezed into block, put it in charring furnace, first temperature is set as 200 ~ 280 DEG C, insulation 20 ~ 30min, again temperature is risen to 320 ~ 420 DEG C, insulation 40 ~ 45min, then rises to 800 ~ 850 DEG C by temperature, keep temperature 2 ~ 3h, then taken out and be cooled to room temperature;
(4) the above-mentioned charing block being cooled to room temperature is put into pulverizer and be ground into 70 ~ 80 order particles, put it into again in encloses container, re-using temperature is that the superheated vapour carrying 100 ~ 110 order calcium carbonate of charing block quality 10 ~ 15% of 900 ~ 1000 DEG C pours in container, when container inner pressure rises to 0.5 ~ 0.6MPa, stop being filled with superheated vapour, stir 30 ~ 35min, speed setting is 1500 ~ 2000r/min, then pressure release is to standard atmospheric pressure, is taken out by charing particle and is cooled to room temperature;
(5) the above-mentioned charing particle being cooled to room temperature is put into fermentation vat, add the river sludge containing furfural waste-water wherein, add-on is 80 ~ 90% of charing granular mass, add 10 ~ 20% extractum carniss of charing granular mass and 15 ~ 35% peptones of charing granular mass more respectively, then adding massfraction is wherein that 20% sodium chloride solution floods mixture 0.5 ~ 1cm, fermentation 10 ~ 15 days is stirred in sealing, and temperature remains 30 ~ 35 DEG C, and speed setting is 150 ~ 200r/min;
(6) after above-mentioned fermentation ends, remove fermented liquid, rinse fermented product 2 ~ 3 times with water, then natural air drying, puts into pulverizer and is ground into 70 ~ 80 order particulate matter, can obtain furfural waste-water treatment agent.
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