CN102689999A - Resourceful treatment method for silica gel waste water - Google Patents
Resourceful treatment method for silica gel waste water Download PDFInfo
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- CN102689999A CN102689999A CN2012101228340A CN201210122834A CN102689999A CN 102689999 A CN102689999 A CN 102689999A CN 2012101228340 A CN2012101228340 A CN 2012101228340A CN 201210122834 A CN201210122834 A CN 201210122834A CN 102689999 A CN102689999 A CN 102689999A
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Abstract
The invention belongs to the technical field of water treatment, and in particular relates to a resourceful treatment method for silica gel waste water. The treatment method mainly comprises the following steps: (1) water quality regulation; (2) silica removal by coagulation; (3) ceramic membrane filtration; and (4) nanofiltration membrane filtration. In the step of silica removal by coagulation, calcium chloride, magnesium chloride, ferric chloride and polyacrylamide are added in the form of an aqueous solution into waste water, wherein the addition amount of calcium chloride, magnesium chloride, ferric chloride and polyacrylamide are respectively 200-400 mg/L, 50-100mg/L, 100-200 mg/L, and 1-5 mg/L in per liter of the waste water. A nanofiltration penetrating liquid of the invention can be reused in production to replace partial fresh water, thereby avoiding pollution and saving abundant fresh water resources at the same time; and a concentrated liquid of the invention can be used in the production of high-quality sodium sulfate, therefore the treatment method of the invention has significant environmental benefits, social benefits, and economic benefits.
Description
Technical field
The invention belongs to water-treatment technology field, particularly a kind of silica gel waste water comprehensive resources treatment method.
Background technology
The main raw material of producing silica gel is water glass (being commonly called as water glass, bubble flower alkali), and it is to be got by the silica chemical process.Be quartzy breeze and the soda ash melts that roasting generates under 1100～1350 ℃ high temperature, obtain water white thick liquid with water extraction.The working method of silica gel has: (1) sulfuric acid process, with the reaction of water glass and sulfuric acid (also available other acids) and get; (2) double decomposition is with water glass and water soluble salt effect and get; (3) precipitator method are separated out silica gel and are got by means of various organic cpds from alkali metal silicate salt solution; (4) electrolytic process, water glass electrolysis and getting.Sulfuric acid process is a method commonly used at present.
Silica gel waste water is mainly derived from silica gel pickling link, and waste water acidity is very high, and the pH value wherein contains a large amount of vitriol and silicate about 2, and sodium sulphate content can reach 4%, also contains small amounts of chlorine ion, calcium ion and mg ion in addition.Silica gel waste water has the acidity height, and saltiness is high, siliceous height, unmanageable characteristics.For the processing of silica gel waste water, the domestic example that does not also have recycling.Application number is that 200810227913.1 Chinese invention patent provides a kind of silicon-containing wastewater treatment method, and this invention is in order to solve SiO in the silicon-containing wastewater
2Be prone to the gel problem; In silicon-containing wastewater, add the nucleation coagulant aids; And silicon-containing wastewater and nucleation coagulant aids are mixed; Said nucleation coagulant aids is meant as the growth core minitype particle material aggregation of the difficult cohesion that suspends in the water is grown up and settled insoluble solid, with the pH regulator of silicon-containing wastewater to 3.5-9.Though this method can be avoided SiO
2Be prone to the gel problem, but unsatisfactory to the treatment effect of activated silica, and can not recycle the useful matter in the waste water.
Summary of the invention
But the object of the present invention is to provide that a kind of sewage treatment process is reasonable, treatment effect is preferable and handle after the silica gel waste water reclaiming treatment process of direct reuse, to solve the big technical problem of present silica gel wastewater treatment difficulty.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of silica gel waste water reclaiming treatment process, this method comprises the steps:
(1) water quality regulation: in silica gel waste water, add lime, pH is transferred in the 7-8 scope;
(2) coagulation silica removal: in the waste water that step (1) obtains, add calcium chloride and magnesium chloride successively; Mixing is to remove dissolves silicon in the waste water; In waste water, add iron(ic)chloride again, form alumen ustum, add SEPIGEL 305 at last; The alumen ustum of formation is increased and the acceleration sedimentation, separate obtaining limpider supernatant through pulp water; Coagulation silica removal process is accomplished in coagulative precipitation tank, and the hydraulic detention time of waste water in coagulative precipitation tank was greater than 40 minutes;
Wherein, said calcium chloride, magnesium chloride, iron(ic)chloride, SEPIGEL 305 all add with aqueous solution form, in every liter of waste water; The dosage of calcium chloride, magnesium chloride, iron(ic)chloride, SEPIGEL 305 is respectively 200-400mg/L; 50-100 mg/L, 100-200 mg/L, 1-5 mg/L;
(3) ceramic membrane filter: the ceramic membrane filter processing is carried out in the water outlet of coagulative precipitation tank again, and said ceramic membrane aperture is 0.2 μ m, and working pressure is 0.15-0.2MPa; Ceramic membrane filter is used for removing the residual suspended substance of waste water, colloidal impurity;
(4) nf membrane is filtered: the liquid that sees through of ceramic membrane carries out the nf membrane filtration in the step (3), and described nf membrane is that molecular weight cut-off is FM, polymeric amide or the composite nanometer filtering film of 150-300; The filtering working pressure of nf membrane is 2-2.5MPa, and service temperature is 20-40 ℃.
As preferably; Ceramic membrane can be reused through cleaning step in the step (3); The ceramic membrane cleaning step is: with behind the flushing with clean water 10min, earlier with 2% NaOH solution washing 10min, use flushing with clean water 10min again under the room temperature; Use 2% HCl solution pickling 10min then, get final product with flushing with clean water 10min at last.
As preferably, said nf membrane cleaning step is: deionized water is circulated in the nf membrane device with discharge remain in the remaining feed liquid in the nf membrane device earlier, then with the 0.1%NaOH and 1% Na that prepare
2-EDTA solution does not have pressure reduction or low pressure and mass flow flushing 30min, is the pure water flux that nf membrane is measured in neutral back with deionized water rinsing nf membrane device to water outlet pH value; 0.2%HCl solution with pH2 carries out low pressure and mass flow flushing 30min to this nf membrane again, is neutral with deionized water rinse-system to water outlet pH value.
As preferably, the pore size filter that nf membrane is filtered the security personnel's strainer that adopts in the step (4) is respectively 10 μ m and 2 μ m.
As preferably, above-mentioned silica gel waste water reclaiming treatment process also comprises: (5) resource reusing: the nf membrane that step (4) obtains sees through liquid and obtains the sodium sulfate solid through evaporation drying.The nf membrane that obtains after present method is handled sees through liquid can reuse, and should see through liquid be liquid concentrator, contained better quality fractional sodium sulfate, therefore can obtain high-quality sodium sulfate solid through evaporation drying.The sodium sulfate that recovery obtains can be produced Sodium sulfate anhydrous.min(99), is used for glass, enamel, paper pulp, refrigeration mixture, washing composition, siccative, dye-dilution agent, analytical chemistry reagent, pharmaceuticals etc.
As preferably, the dosage of described calcium chloride, magnesium chloride, iron(ic)chloride, SEPIGEL 305 is respectively 280-320mg/L, 80-100 mg/L, 140-160 mg/L, 2-4 mg/L.
Nearly 250,000 tons/year of the production of China's silica gel, 1 ton of silica gel of every production will consume 40-50 ton clear water, produces more than 30 ton of sewage simultaneously.Nanofiltration of the present invention sees through liquid and can be back in the production, substitutes part fresh water, when avoiding polluting, practices thrift a large amount of Freshwater resources, has significant environmental benefit and social benefit; Liquid concentrator can be produced high-quality sodium sulfate, has remarkable economic efficiency.The present invention provides thinking for the energy-saving and emission-reduction of silica gel industry, for the industrial applications of silica gel wastewater treatment provides an effective way, has significant environmental benefit, economic benefit and social benefit.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Pass through specific embodiment below, and combine accompanying drawing, technical scheme of the present invention is further specified.
In the present invention, if not refer in particular to, all part, per-cents are weight unit, and all equipment and raw material etc. all can be buied from market or the industry is commonly used.
Following examples of the present invention describe the inventive method with certain silica gel factory waste water, and this waste water quality index is as shown in table 1.
The main water-quality guideline of certain silica gel factory waste water of table 1
| Project | Index/content | Project | Index/content |
| pH | 2.03 | Calcium ion (Ca 2+）/mg/L | 56.3 |
| Specific conductivity/μ s/cm | 17530 | Mg ion (Mg 2+)/mg/L | 50.2 |
| Cl ions (Cl -）/mg/L | 103.5 | Potassium ion (K +）/mg/L | 163.4 |
| Sulfate radical (SO 4 2-）/mg/L | 20282.3 | Total silicon (SiO 2）/mg/L | 306.2 |
| Sodium ion (Na +）/mg/L | 8481.7 | Activated silica/mg/L | 286.1 |
Embodiment 1:
Silica gel waste water reclaiming treatment process as shown in Figure 1, this method comprises the steps:
1. water quality regulation
In the water quality regulation pond, in silica gel waste water, add lime, pH is transferred in the 7-8 scope.
2. coagulation silica removal
The waste water of regulating the pH value flows into coagulative precipitation tank, in waste water, adds 300mg/L calcium chloride and 100 mg/L magnesium chlorides, mixing; Purpose is to remove dissolves silicon in the waste water, in waste water, adds 150 mg/L ferric chloride Solution(38s again, and thorough mixing is to form alumen ustum; Add 2 mg/L SEPIGEL 305s at last, alumen ustum is increased, quicken sedimentation; The hydraulic retention of waste water in coagulative precipitation tank 45 minutes obtains limpider supernatant through the pulp water separation.
Above-mentioned calcium chloride, magnesium chloride, iron(ic)chloride, SEPIGEL 305 all add with aqueous solution form, and dosage is in every liter of waste water.
3. ceramic membrane filter
The water outlet of coagulative precipitation tank is carried out ceramic membrane filter again and is handled.Selecting the aperture for use is 0.2 μ m ceramic membrane, and working pressure is 0.15Mpa, and this step is used for removing residual suspended substance of waste water and colloidal impurity.
Ceramic membrane can be reused through cleaning step; The ceramic membrane cleaning step is: with behind the flushing with clean water 10min, earlier with 2% NaOH solution washing 10min, use flushing with clean water 10min again under the room temperature; Use 2% HCl solution pickling 10min then, get final product with flushing with clean water 10min at last.
4. nf membrane is filtered
The last ceramic membrane that obtains of step is seen through liquid carry out nf membrane and filter, selecting molecular weight cut-off for use is 170 polymeric amide composite nanometer filtering film, nanofiltration system working pressure 2MPa, and service temperature is 25 ℃.The pore size filter that nf membrane is filtered the security personnel's strainer that adopts is respectively 10 μ m and 2 μ m, and the dense water cycles of concentration that obtains is 3.5 times, and wherein sodium sulphate content is 9.92%, after evaporation drying, obtains high-quality sodium sulfate solid; The filtering effluent quality of nf membrane is seen table 2, and water outlet can be back to use in the production.
The filtering effluent quality of table 2 nf membrane
| Project | Index/content | Project | Index/content |
| pH | 7.6 | Calcium ion (Ca 2+）/mg/L | 0.31 |
| Specific conductivity/μ s/cm | 169 | Mg ion (Mg 2+)/mg/L | 0.28 |
| Cl ions (Cl -）/mg/L | 6.2 | Potassium ion (K +）/mg/L | 5.2 |
| Sulfate radical (SO 4 2-）/mg/L | 98.2 | Total silicon (SiO 2）/mg/L | 0.10 |
| Sodium ion (Na +）/mg/L | 43.6 | ? | ? |
Embodiment 2:
Concrete grammar is with embodiment 1, and difference is: in every liter of waste water, the dosage of calcium chloride, magnesium chloride, iron(ic)chloride, SEPIGEL 305 is respectively 200mg/L, 50 mg/L, 100 mg/L, 1mg/L; The hydraulic retention of waste water in coagulative precipitation tank 60 minutes; In the ceramic membrane filter, selecting the aperture for use is 0.2 μ m ceramic membrane, and working pressure is 0.2Mpa; Nf membrane is that molecular weight cut-off is 150 cellulose acetate nano filter-membrane; The filtering working pressure of nf membrane is 2.5MPa, and service temperature is 40 ℃.
The dense water cycles of concentration that present embodiment obtains is 3.4 times, and wherein sodium sulphate content is 9.68%, after evaporation drying, obtains high-quality sodium sulfate solid; The filtering effluent quality of nf membrane is seen table 3.
The filtering effluent quality of table 3 nf membrane
| Project | Index/content | Project | Index/content |
| pH | 7.6 | Calcium ion (Ca 2+）/mg/L | 0.32 |
| Specific conductivity/μ s/cm | 165 | Mg ion (Mg 2+)/mg/L | 0.25 |
| Cl ions (Cl -）/mg/L | 6.0 | Potassium ion (K +）/mg/L | 5.8 |
| Sulfate radical (SO 4 2-）/mg/L | 98.0 | Total silicon (SiO 2）/mg/L | 0.14 |
| Sodium ion (Na +）/mg/L | 43.8 | ? | ? |
Embodiment 3:
Concrete grammar is with embodiment 1, and difference is: in every liter of waste water, the dosage of calcium chloride, magnesium chloride, iron(ic)chloride, SEPIGEL 305 is respectively 400mg/L, 80 mg/L, 200 mg/L, 5 mg/L; The hydraulic retention of waste water in coagulative precipitation tank 60 minutes; In the ceramic membrane filter, selecting the aperture for use is 0.2 μ m ceramic membrane, and working pressure is 0.2Mpa; Nf membrane is that molecular weight cut-off is 300 composite nanometer filtering film; The filtering working pressure of nf membrane is 2.5MPa, and service temperature is 20 ℃.
The dense water cycles of concentration that obtains is 3.5 times, and wherein sodium sulphate content is 9.98%, after evaporation drying, obtains high-quality sodium sulfate solid; The filtering effluent quality of nf membrane is seen table 4.
The filtering effluent quality of table 4 nf membrane
| Project | Index/content | Project | Index/content |
| pH | 7.2 | Calcium ion (Ca 2+）/mg/L | 0.30 |
| Specific conductivity/μ s/cm | 172 | Mg ion (Mg 2+)/mg/L | 0.26 |
| Cl ions (Cl -）/mg/L | 6.3 | Potassium ion (K +）/mg/L | 5.1 |
| Sulfate radical (SO 4 2-）/mg/L | 98.4 | Total silicon (SiO 2）/mg/L | 0.10 |
| Sodium ion (Na +）/mg/L | 43.0 | ? | ? |
Embodiment 4:
Concrete grammar is with embodiment 1, and difference is: in every liter of waste water, the dosage of calcium chloride, magnesium chloride, iron(ic)chloride, SEPIGEL 305 is respectively 280mg/L, 80 mg/L, 140 mg/L, 2 mg/L; The hydraulic retention of waste water in coagulative precipitation tank 60 minutes; In the ceramic membrane filter, selecting the aperture for use is 0.2 μ m ceramic membrane, and working pressure is 0.2Mpa; Nf membrane is that molecular weight cut-off is 300 polymeric amide composite nanometer filtering film; The filtering working pressure of nf membrane is 2.5MPa, and service temperature is 20 ℃.
The dense water cycles of concentration that obtains is 3.5 times, and wherein sodium sulphate content is 9.72%, after evaporation drying, obtains high-quality sodium sulfate solid; The filtering effluent quality of nf membrane is seen table 5.
The filtering effluent quality of table 5 nf membrane
| Project | Index/content | Project | Index/content |
| pH | 7.5 | Calcium ion (Ca 2+）/mg/L | 0.33 |
| Specific conductivity/μ s/cm | 167 | Mg ion (Mg 2+)/mg/L | 0.25 |
| Cl ions (Cl -）/mg/L | 6.1 | Potassium ion (K +）/mg/L | 5.5 |
| Sulfate radical (SO 4 2-）/mg/L | 98.0 | Total silicon (SiO 2）/mg/L | 0.12 |
| Sodium ion (Na +）/mg/L | 43.5 | ? | ? |
Embodiment 5:
Concrete grammar is with embodiment 1, and difference is: in every liter of waste water, the dosage of calcium chloride, magnesium chloride, iron(ic)chloride, SEPIGEL 305 is respectively 320mg/L, 100 mg/L, 160 mg/L, 4 mg/L; The hydraulic retention of waste water in coagulative precipitation tank 60 minutes; In the ceramic membrane filter, selecting the aperture for use is 0.2 μ m ceramic membrane, and working pressure is 0.2Mpa; Nf membrane is that molecular weight cut-off is 300 cellulose acetate nano filter-membrane; The filtering working pressure of nf membrane is 2.5MPa, and service temperature is 20 ℃.
The dense water cycles of concentration that obtains is 4 times, and wherein sodium sulphate content is 11.08%, after evaporation drying, obtains high-quality sodium sulfate solid; The filtering effluent quality of nf membrane is seen table 6.
The filtering effluent quality of table 6 nf membrane
| Project | Index/content | Project | Index/content |
| pH | 7.6 | Calcium ion (Ca 2+）/mg/L | 0.32 |
| Specific conductivity/μ s/cm | 170 | Mg ion (Mg 2+)/mg/L | 0.24 |
| Cl ions (Cl -）/mg/L | 6.0 | Potassium ion (K +）/mg/L | 5.4 |
| Sulfate radical (SO 4 2-）/mg/L | 98.2 | Total silicon (SiO 2）/mg/L | 0.10 |
| Sodium ion (Na +）/mg/L | 43.7 | ? | ? |
The nanofiltration that above embodiment obtains sees through liquid and can be back in the production, substitutes part fresh water, when avoiding polluting, practices thrift a large amount of Freshwater resources, has significant environmental benefit and social benefit; Liquid concentrator can be produced high-quality sodium sulfate, has remarkable economic efficiency.The present invention provides thinking for the energy-saving and emission-reduction of silica gel industry, for the industrial applications of silica gel wastewater treatment provides an effective way, has significant environmental benefit, economic benefit and social benefit.
Above-described embodiment is a kind of preferable scheme of the present invention, is not that the present invention is done any pro forma restriction, under the prerequisite that does not exceed the technical scheme that claim puts down in writing, also has other variant and remodeling.
Claims (9)
1. a silica gel waste water reclaiming treatment process is characterized in that this method comprises the steps:
(1) water quality regulation: in silica gel waste water, add lime, pH is transferred in the 7-8 scope;
(2) coagulation silica removal: in the waste water that step (1) obtains, add calcium chloride and magnesium chloride successively, behind the mixing, in waste water, add iron(ic)chloride again, form alumen ustum, add SEPIGEL 305 at last, separate obtaining limpider supernatant through pulp water; Coagulation silica removal process is accomplished in coagulative precipitation tank, and the hydraulic detention time of waste water in coagulative precipitation tank was greater than 40 minutes;
Wherein, said calcium chloride, magnesium chloride, iron(ic)chloride, SEPIGEL 305 all add with aqueous solution form, in every liter of waste water; The dosage of calcium chloride, magnesium chloride, iron(ic)chloride, SEPIGEL 305 is respectively 200-400mg/L; 50-100 mg/L, 100-200 mg/L, 1-5 mg/L;
(3) ceramic membrane filter: the ceramic membrane filter processing is carried out in the water outlet of coagulative precipitation tank again, and said ceramic membrane aperture is 0.2 μ m, and working pressure is 0.15-0.2MPa;
(4) nf membrane is filtered: the liquid that sees through of ceramic membrane carries out the nf membrane filtration in the step (3), and described nf membrane is that molecular weight cut-off is FM, polymeric amide or the composite nanometer filtering film of 150-300; The filtering working pressure of nf membrane is 2-2.5MPa, and service temperature is 20-40 ℃.
2. silica gel waste water reclaiming treatment process according to claim 1; It is characterized in that: ceramic membrane is reused through cleaning step in the step (3); The ceramic membrane cleaning step is: with behind the flushing with clean water 10min, with the NaOH solution washing 10min of 2wt%, use flushing with clean water 10min more earlier under the room temperature; Use the HCl solution pickling 10min of 2wt% then, get final product with flushing with clean water 10min at last.
3. silica gel waste water reclaiming treatment process according to claim 1; It is characterized in that: said nf membrane cleaning step is: deionized water is circulated in the nf membrane device with discharge remain in the remaining feed liquid in the nf membrane device earlier, then with the 0.1wt%NaOH and the 1wt% Na that prepare
2-EDTA solution does not have pressure reduction or low pressure and mass flow flushing 30min, is the pure water flux that nf membrane is measured in neutral back with deionized water rinsing nf membrane device to water outlet pH value; 0.2wt%HCl solution with pH2 carries out low pressure and mass flow flushing 30min to this nf membrane again, is neutral with deionized water rinsing to system water outlet pH value.
4. according to claim 1 or 2 or 3 described silica gel waste water reclaiming treatment processs, it is characterized in that: the pore size filter of security personnel's strainer that the nf membrane filtration is adopted in the step (4) is respectively 10 μ m and 2 μ m.
5. according to claim 1 or 2 or 3 described silica gel waste water reclaiming treatment processs, it is characterized in that also comprising: (5) resource reusing: the nf membrane that step (4) obtains sees through liquid and obtains the sodium sulfate solid through evaporation drying.
6. silica gel waste water reclaiming treatment process according to claim 4 is characterized in that also comprising: (5) resource reusing: the nf membrane that step (4) obtains sees through liquid and obtains the sodium sulfate solid through evaporation drying.
7. according to claim 1 or 2 or 3 described silica gel waste water reclaiming treatment processs; It is characterized in that also comprising: the dosage of described calcium chloride, magnesium chloride, iron(ic)chloride, SEPIGEL 305 is respectively 280-320mg/L; 80-100 mg/L, 140-160 mg/L, 2-4 mg/L.
8. silica gel waste water reclaiming treatment process according to claim 4; It is characterized in that also comprising: the dosage of described calcium chloride, magnesium chloride, iron(ic)chloride, SEPIGEL 305 is respectively 280-320mg/L; 80-100 mg/L, 140-160 mg/L, 2-4 mg/L.
9. silica gel waste water reclaiming treatment process according to claim 5; It is characterized in that also comprising: the dosage of described calcium chloride, magnesium chloride, iron(ic)chloride, SEPIGEL 305 is respectively 280-320mg/L; 80-100 mg/L, 140-160 mg/L, 2-4 mg/L.
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| CN110002655A (en) * | 2019-05-13 | 2019-07-12 | 山东金汇膜科技股份有限公司 | A kind of silica gel Wastewater zero-discharge treatment system |
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| CN104030499B (en) * | 2014-05-22 | 2015-10-28 | 浙江工业大学 | A kind of integrated conduct method of extraordinary molecular sieve synthesis mother liquid |
| CN104030499A (en) * | 2014-05-22 | 2014-09-10 | 浙江工业大学 | Comprehensive treatment method of special-type molecular sieve synthesis mother solution |
| CN104973717A (en) * | 2015-07-06 | 2015-10-14 | 江苏德邦工程有限公司 | Saline wastewater deep treatment method |
| CN105036408A (en) * | 2015-07-06 | 2015-11-11 | 江苏德邦工程有限公司 | Treatment method of wastewater containing high-concentration active silicon |
| CN107043191A (en) * | 2016-12-26 | 2017-08-15 | 青岛美高集团有限公司 | A kind of silica gel produces treatment method for high-salinity wastewater |
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Application publication date: 20120926 |