CN115646457A - Heavy metal removing additive, heavy metal removing carbon rod and preparation method - Google Patents
Heavy metal removing additive, heavy metal removing carbon rod and preparation method Download PDFInfo
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- CN115646457A CN115646457A CN202211292630.1A CN202211292630A CN115646457A CN 115646457 A CN115646457 A CN 115646457A CN 202211292630 A CN202211292630 A CN 202211292630A CN 115646457 A CN115646457 A CN 115646457A
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- heavy metal
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- activated carbon
- metal removing
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- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 130
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 239000000654 additive Substances 0.000 title claims abstract description 63
- 230000000996 additive effect Effects 0.000 title claims abstract description 60
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000000034 method Methods 0.000 claims abstract description 23
- 239000006185 dispersion Substances 0.000 claims description 42
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 28
- 239000007788 liquid Substances 0.000 claims description 26
- 238000002156 mixing Methods 0.000 claims description 25
- 239000002245 particle Substances 0.000 claims description 24
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 claims description 20
- 239000012071 phase Substances 0.000 claims description 20
- 239000008346 aqueous phase Substances 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 18
- 235000013162 Cocos nucifera Nutrition 0.000 claims description 16
- 244000060011 Cocos nucifera Species 0.000 claims description 16
- 239000000839 emulsion Substances 0.000 claims description 16
- 239000004408 titanium dioxide Substances 0.000 claims description 14
- 239000000853 adhesive Substances 0.000 claims description 12
- 230000001070 adhesive effect Effects 0.000 claims description 12
- 239000004699 Ultra-high molecular weight polyethylene Substances 0.000 claims description 11
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 11
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 11
- 229920000785 ultra high molecular weight polyethylene Polymers 0.000 claims description 11
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 10
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 10
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 10
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 10
- 238000005520 cutting process Methods 0.000 claims description 9
- 229940075507 glyceryl monostearate Drugs 0.000 claims description 9
- 239000001788 mono and diglycerides of fatty acids Substances 0.000 claims description 9
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical group C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 8
- 239000000835 fiber Substances 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- 239000003999 initiator Substances 0.000 claims description 8
- 239000007764 o/w emulsion Substances 0.000 claims description 8
- 239000004094 surface-active agent Substances 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 230000010355 oscillation Effects 0.000 claims description 7
- 238000007873 sieving Methods 0.000 claims description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 6
- 238000004108 freeze drying Methods 0.000 claims description 5
- 238000006116 polymerization reaction Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 229920002678 cellulose Polymers 0.000 claims description 4
- 239000001913 cellulose Substances 0.000 claims description 4
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 3
- 229910021536 Zeolite Inorganic materials 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 3
- 239000002808 molecular sieve Substances 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 3
- 239000010457 zeolite Substances 0.000 claims description 3
- 239000011787 zinc oxide Substances 0.000 claims description 3
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 2
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 2
- 239000002033 PVDF binder Substances 0.000 claims description 2
- 244000082204 Phyllostachys viridis Species 0.000 claims description 2
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 2
- 239000011425 bamboo Substances 0.000 claims description 2
- 239000003245 coal Substances 0.000 claims description 2
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 2
- 239000000194 fatty acid Substances 0.000 claims description 2
- 229930195729 fatty acid Natural products 0.000 claims description 2
- 150000004665 fatty acids Chemical class 0.000 claims description 2
- 229920001903 high density polyethylene Polymers 0.000 claims description 2
- 239000004700 high-density polyethylene Substances 0.000 claims description 2
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims description 2
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims description 2
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims description 2
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims description 2
- 229920000092 linear low density polyethylene Polymers 0.000 claims description 2
- 239000004707 linear low-density polyethylene Substances 0.000 claims description 2
- 229920001684 low density polyethylene Polymers 0.000 claims description 2
- 239000004702 low-density polyethylene Substances 0.000 claims description 2
- 239000004533 oil dispersion Substances 0.000 claims description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000000344 soap Substances 0.000 claims description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 2
- 235000019333 sodium laurylsulphate Nutrition 0.000 claims description 2
- 235000013399 edible fruits Nutrition 0.000 claims 1
- 238000001125 extrusion Methods 0.000 abstract description 22
- 229910052785 arsenic Inorganic materials 0.000 abstract description 10
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 abstract description 10
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 abstract description 10
- 229910052753 mercury Inorganic materials 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 7
- 238000000746 purification Methods 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 8
- 239000004005 microsphere Substances 0.000 description 7
- 230000000379 polymerizing effect Effects 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 3
- 239000010419 fine particle Substances 0.000 description 3
- 238000007710 freezing Methods 0.000 description 3
- 230000008014 freezing Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000007720 emulsion polymerization reaction Methods 0.000 description 1
- 238000009292 forward osmosis Methods 0.000 description 1
- YQEMORVAKMFKLG-UHFFFAOYSA-N glycerine monostearate Natural products CCCCCCCCCCCCCCCCCC(=O)OC(CO)CO YQEMORVAKMFKLG-UHFFFAOYSA-N 0.000 description 1
- SVUQHVRAGMNPLW-UHFFFAOYSA-N glycerol monostearate Natural products CCCCCCCCCCCCCCCCC(=O)OCC(O)CO SVUQHVRAGMNPLW-UHFFFAOYSA-N 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000013048 microbiological method Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 238000001223 reverse osmosis Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
Abstract
The invention provides a heavy metal removal additive, a heavy metal removal carbon rod and a preparation method thereof. The heavy metal removal additive also has good strength, and can be used in an extrusion carbon rod forming process to prepare a heavy metal removal carbon rod with good strength and high flow rate. The heavy metal removing carbon rod can be used in the field of household water purification to remove heavy metals such as lead, mercury, arsenic and the like in water, and has a good removing effect.
Description
Technical Field
The invention relates to the technical field of filter elements of water purifiers, in particular to a heavy metal removing additive, a heavy metal removing carbon rod and a preparation method thereof.
Background
Heavy metal elements precipitated from the water supply body due to the corrosion of the water pipeline can cause heavy metal pollution in the water body. Among them, the heavy metals most seriously affecting the human body are mainly lead, mercury, cadmium and arsenic. Heavy metal elements in water are mainly removed by a membrane separation method, an ion exchange method, a microbiological method, an adsorption method and the like, and the heavy metal elements in the water are mainly removed by an RO machine by utilizing a reverse osmosis principle in the field of household water purification. However, the RO machine has the defects of high water consumption, electricity insertion, high noise of a booster pump, generation of overnight water due to shutdown and forward osmosis, poor adsorption effect on small molecular organic matters and the like.
The activated carbon rod has low cost compared with the RO membrane, and has extremely high specific surface area and high adsorption efficiency to organic matters. However, the effect of removing heavy metals is not as good as that of RO membrane, so that the functional carbon rods on the market at present are all added with heavy metal removing additives. Most of the existing common heavy metal removal additives have the defects of fine particle size, unmatched mesh number with activated carbon, poor strength and frangibility, so that the heavy metal removal additives can only be applied to the field of sintered carbon rods with higher cost. If the heavy metal removing additive with adjustable particle size and good strength can be developed, the additive can be suitable for extruding the heavy metal removing carbon rod, and has important significance for reducing the production cost and improving the quality of the extruded heavy metal removing carbon rod.
Disclosure of Invention
The invention aims to provide a heavy metal removing additive which has higher specific surface area and better strength and can be used in an extrusion molding process to prepare a heavy metal removing carbon rod.
The invention also aims to provide a preparation method of the heavy metal removal additive, which adopts an emulsion template method, and can regulate and control the size of emulsion microspheres by regulating and controlling the water-oil volume ratio of emulsion, so that the heavy metal removal additive with high specific surface area, better strength and controllable microsphere particle size can be prepared.
The third purpose of the invention is to provide a heavy metal removing carbon rod which can be used for removing heavy metals such as lead, mercury, arsenic and the like in water and has good removing effect and high flow.
The fourth purpose of the invention is to provide a preparation method of the heavy metal removing carbon rod, the heavy metal removing carbon rod can be prepared by using the heavy metal removing additive in the carbon rod extrusion forming process, and the method is simple, easy to form, controllable in parameters and suitable for industrial large-scale production.
The technical problem to be solved by the invention is realized by adopting the following technical scheme.
The invention provides a preparation method of a heavy metal removing additive, which comprises the following steps:
s1, mixing heavy metal removing active particles and deionized water, adding hydrophilic fibers and a surfactant, and stirring to obtain an aqueous phase dispersion, wherein the heavy metal removing active particles are selected from two of titanium dioxide, activated alumina, a zeolite molecular sieve, nano zinc oxide, nano iron, ferric oxide and ferric chloride;
s2, dissolving an initiator in a styrene monomer to obtain an oil phase dispersion liquid;
s3, mixing the aqueous phase dispersion liquid and the oil phase dispersion liquid, and then carrying out ultrasonic oscillation for 25-35 min to obtain an oil-in-water type emulsion;
and S4, carrying out polymerization reaction on the oil-in-water emulsion under a water bath condition, and then carrying out freeze drying, grinding and sieving to obtain the heavy metal removal additive.
The invention provides a heavy metal removal additive which is prepared according to the preparation method.
The invention also provides a heavy metal removing carbon rod which comprises, by weight, 50-70 parts of activated carbon powder, 25-30 parts of adhesive and 5-20 parts of heavy metal removing additive.
The invention also provides a preparation method of the heavy metal removing carbon rod, which comprises the following steps:
respectively weighing the activated carbon powder, the adhesive and the heavy metal removal additive according to the weight parts of the heavy metal removal carbon rod, then premixing the activated carbon powder and the heavy metal removal additive, then adding the adhesive for mixing, extruding, molding and cutting to obtain the heavy metal removal carbon rod.
The heavy metal removing additive, the heavy metal removing carbon rod and the preparation method have the beneficial effects that:
the invention takes the mixed solution of the heavy metal removal active particles, the hydrophilic fibers and the surfactant as the water phase dispersing agent, takes the styrene monomer for dissolving the initiator as the oil phase dispersion liquid, adopts the emulsion template method and regulates and controls the volume ratio of the water to the oil of the emulsion so as to regulate and control the size of the emulsion microspheres, and obtains the heavy metal removal additive with high specific surface area and controllable microsphere particle size. The heavy metal removing additive also has better strength, and can be used in the extrusion carbon rod forming process to prepare the heavy metal removing carbon rod with good strength and high flow rate. The heavy metal removing carbon rod can be used in the field of household water purification to remove heavy metals such as lead, mercury, arsenic and the like in water, and has a good removing effect.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The additive for removing heavy metals and the carbon rod for removing heavy metals and the preparation method of the carbon rod for removing heavy metals according to the embodiment of the invention are specifically described below.
The preparation method of the heavy metal removing additive provided by the embodiment of the invention comprises the following steps:
s1, mixing heavy metal removing active particles and deionized water, adding hydrophilic fibers and a surfactant, and stirring to obtain an aqueous phase dispersion, wherein the heavy metal removing active particles are selected from two of titanium dioxide, activated alumina, a zeolite molecular sieve, nano zinc oxide, nano iron, ferric oxide and ferric chloride.
Further, in a preferred embodiment of the present invention, the hydrophilic fiber is selected from one or more of carboxymethyl cellulose, polyanionic cellulose, cellulose nanowhisker, and hydroxypropyl methyl cellulose.
Further, in a preferred embodiment of the present invention, the surfactant is one or more selected from glycerol monostearate, sodium lauryl sulfate, fatty acid soap and sodium dodecylbenzene sulfonate.
Further, in a preferred embodiment of the present invention, the aqueous dispersion comprises 30 to 85 parts by weight of the heavy metal-removing active particles, 10 to 20 parts by weight of the hydrophilic fibers, and 5 to 15 parts by weight of the surfactant.
And S2, dissolving an initiator in a styrene monomer to obtain an oil phase dispersion liquid.
And S3, mixing the aqueous phase dispersion liquid and the oil phase dispersion liquid, and performing ultrasonic oscillation for 25-35 min to obtain the oil-in-water type emulsion.
Further, in a preferred embodiment of the present invention, the volume ratio of the aqueous dispersion to the oil dispersion is 2 to 5:1.
And S4, carrying out polymerization reaction on the oil-in-water emulsion under the water bath condition, and then carrying out freeze drying, grinding and sieving to obtain the heavy metal removal additive. After the oil-in-water emulsion polymerization reaction, a freeze dryer is used for freeze drying to remove residual solvent, and coarse and fine particles are removed by grinding through 200-mesh and 400-mesh screens respectively, so that the heavy metal removal additive can be obtained.
Further, in the preferred embodiment of the present invention, the temperature of the polymerization reaction is 60 to 80 ℃, and the reaction time is 10 to 15 hours.
The invention uses an emulsion template method, and regulates and controls the size of emulsion microspheres by regulating and controlling the water-oil volume ratio of the emulsion to obtain the heavy metal removal additive with high specific surface area and controllable microsphere particle size. In addition, the heavy metal additive also has better strength, is suitable for being used in the extrusion carbon rod forming process to prepare the heavy metal removing carbon rod, can reduce the production cost and can also improve the quality of the heavy metal removing extrusion carbon rod.
The invention also provides a heavy metal removal additive which is prepared according to the preparation method.
The invention also provides a heavy metal removing carbon rod which comprises, by weight, 50-70 parts of activated carbon powder, 25-30 parts of adhesive and 5-20 parts of the heavy metal removing additive.
Further, in a preferred embodiment of the present invention, the activated carbon powder is selected from one or more of coconut shell activated carbon powder, wooden activated carbon powder, coal activated carbon powder and bamboo activated carbon powder.
Further, in a preferred embodiment of the present invention, the particle size of the activated carbon powder is selected from one or more of 60-140 mesh, 80-200 mesh, 80-325 mesh and 80-400 mesh.
Further, in a preferred embodiment of the present invention, the adhesive is selected from at least one of ultra-high molecular weight polyethylene, high density polyethylene, low density polyethylene, linear low density polyethylene and polyvinylidene fluoride.
Further, in the preferred embodiment of the invention, the height of the heavy metal removing carbon rod is 110-263 mm, the inner diameter is 10-30 mm, the outer diameter is 25-60 mm, and the gram weight is 60-350 g/PCS.
The invention also provides a preparation method of the heavy metal removing carbon rod, which comprises the following steps:
and premixing the activated carbon powder and the heavy metal removal additive, then adding an adhesive for mixing, extruding, molding and cutting to obtain the heavy metal removal carbon rod. The heavy metal removing additive is easy to mix into the activated carbon powder and the adhesive, and the carbon rod with different effects of removing heavy metals such as lead, mercury, arsenic and the like can be obtained after extrusion molding. In addition, the heavy metal removing additive has good strength, so that the heavy metal removing additive cannot generate broken particles when being extruded by a screw, and the heavy metal removing carbon rod added with the heavy metal removing additive also has high flow rate and can be used in the field of household water purification.
Further, in the preferred embodiment of the invention, a conical stirring device is adopted for premixing, the rotating speed of the conical stirring device is 150-200 r/min, and the premixing time is 30-90 min. After the adhesive is added, the rotating speed of the conical stirring device is 100-150 r/min, and the mixing time is 10-30 min.
Further, in a preferred embodiment of the present invention, during the extrusion molding process, the extrusion includes three stages of temperatures, wherein the first stage temperature is 120 to 150 ℃, the second stage temperature is 180 to 220 ℃, and the third stage temperature is 170 to 185 ℃.
Further, in the preferred embodiment of the present invention, the rotation speed of the screw is 200 to 400r/min during the extrusion molding process.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The carbon rod for removing heavy metals provided by the embodiment is prepared according to the following method:
(1) Preparation of heavy metal removal additive:
(11) Mixing titanium dioxide, ferric oxide and deionized water, adding carboxymethyl cellulose and glyceryl monostearate, and stirring to obtain aqueous dispersion. Wherein, according to the weight portion, the heavy metal removing additive comprises: 60 parts of titanium dioxide, 10 parts of ferric oxide, 20 parts of carboxymethyl cellulose and 10 parts of glyceryl monostearate.
(12) The initiator is dissolved in the styrene monomer to obtain an oil phase dispersion.
(13) And mixing the aqueous phase dispersion liquid and the oil phase dispersion liquid, and performing ultrasonic oscillation for 25-35 min to obtain the oil-in-water type emulsion. Wherein the volume ratio of the aqueous phase dispersion liquid to the oil phase dispersion liquid is 3:1.
(14) Polymerizing the oil-in-water emulsion for 10 hours under the water bath condition of 60 ℃, and freeze-drying, grinding and sieving to obtain the heavy metal removal additive.
(2) Preparing a heavy metal removing carbon rod:
(21) Respectively weighing coconut shell activated carbon powder, a heavy metal removal additive and ultrahigh molecular weight polyethylene. Wherein, the coconut shell activated carbon powder comprises 60 parts by weight of coconut shell activated carbon powder, 15 parts by weight of heavy metal removal additive and 20 parts by weight of ultrahigh molecular weight polyethylene; the particle size of the coconut shell activated carbon powder is 80-325 meshes.
(22) Pre-mixing the coconut shell activated carbon powder and the heavy metal removal additive in a conical stirring device, wherein the stirring speed is 200r/min, and the pre-mixing time is 60min; then adding ultra-high molecular weight polyethylene, stirring at the rotation speed of 150r/min, and mixing for 30min. And then carrying out extrusion molding and cutting to obtain the heavy metal removing carbon rod. Wherein, in the extrusion molding process, the extrusion comprises three sections of temperatures, wherein the first section of temperature is 130 ℃, the second section of temperature is 190 ℃, and the third section of temperature is 170 ℃; the rotation speed of the screw is 300r/min. When cutting, the materials are cut into 192mm long carbon rods according to the specified size, and the gram weight is 110g.
Example 2
The embodiment provides a heavy metal removing carbon rod, which is different from the embodiment 1 in that:
(1) Preparation of heavy metal removal additive:
(11) Mixing titanium dioxide, ferric oxide and deionized water, adding carboxymethyl cellulose and glyceryl monostearate, and stirring to obtain aqueous phase dispersion. Wherein, the heavy metal removing additive comprises the following components in parts by weight: 50 parts of titanium dioxide, 20 parts of ferric oxide, 20 parts of carboxymethyl cellulose and 10 parts of glyceryl monostearate.
(12) The initiator was dissolved in the styrene monomer to obtain an oil phase dispersion.
(13) And mixing the aqueous phase dispersion liquid and the oil phase dispersion liquid, and performing ultrasonic oscillation for 25-35 min to obtain the oil-in-water type emulsion. Wherein the volume ratio of the aqueous phase dispersion liquid to the oil phase dispersion liquid is 3:1.
(14) Polymerizing the oil-in-water emulsion for 10 hours under the water bath condition of 60 ℃, freezing, drying, grinding and sieving to obtain the heavy metal removal additive.
Example 3
The embodiment provides a heavy metal removing carbon rod, which is different from the embodiment 1 in that:
(1) Preparation of heavy metal removal additive:
(11) Mixing titanium dioxide, ferric oxide and deionized water, adding carboxymethyl cellulose and glyceryl monostearate, and stirring to obtain aqueous phase dispersion. Wherein, the heavy metal removing additive comprises the following components in parts by weight: 45 parts of titanium dioxide, 25 parts of ferric oxide, 20 parts of carboxymethyl cellulose and 10 parts of glyceryl monostearate.
(12) The initiator is dissolved in the styrene monomer to obtain an oil phase dispersion.
(13) And mixing the aqueous phase dispersion liquid and the oil phase dispersion liquid, and performing ultrasonic oscillation for 25-35 min to obtain the oil-in-water type emulsion. Wherein the volume ratio of the aqueous phase dispersion liquid to the oil phase dispersion liquid is 3:1.
(14) Polymerizing the oil-in-water emulsion for 10 hours under the water bath condition of 60 ℃, freezing, drying, grinding and sieving to obtain the heavy metal removal additive.
Example 4
The embodiment provides a heavy metal removing carbon rod, which is different from the embodiment 1 in that:
(1) Preparation of heavy metal removal additive:
(11) Mixing titanium dioxide, ferric oxide and deionized water, adding carboxymethyl cellulose and glyceryl monostearate, and stirring to obtain aqueous phase dispersion. Wherein, the heavy metal removing additive comprises the following components in parts by weight: 45 parts of titanium dioxide, 25 parts of ferric oxide, 20 parts of carboxymethyl cellulose and 10 parts of glyceryl monostearate.
(12) The initiator is dissolved in the styrene monomer to obtain an oil phase dispersion.
(13) And mixing the aqueous phase dispersion liquid and the oil phase dispersion liquid, and performing ultrasonic oscillation for 25-35 min to obtain the oil-in-water type emulsion. Wherein the volume ratio of the aqueous phase dispersion liquid to the oil phase dispersion liquid is 4:1.
(14) Polymerizing the oil-in-water emulsion for 10 hours under the water bath condition of 60 ℃, freezing, drying, grinding and sieving to obtain the heavy metal removing additive.
Comparative example 1
This comparative example provides a carbon rod prepared according to the following steps:
(1) Respectively weighing coconut shell activated carbon powder and ultra-high molecular weight polyethylene. Wherein, the coconut shell activated carbon powder comprises 75 parts by weight of coconut shell activated carbon powder and 25 parts by weight of ultrahigh molecular weight polyethylene; the particle size of the coconut shell activated carbon powder is 80-325 meshes.
(2) Placing the coconut shell activated carbon powder and the ultra-high molecular weight polyethylene into a stirring device for mixing, wherein the stirring speed is 150r/min, and the mixing time is 30min. And then carrying out extrusion molding and cutting to obtain the carbon rod. Wherein, in the extrusion molding process, the extrusion comprises three sections of temperatures, wherein the first section of temperature is 130 ℃, the second section of temperature is 190 ℃, and the third section of temperature is 170 ℃; the rotation speed of the screw is 300r/min. When cutting, the materials are cut into 192mm long carbon rods according to the specified size, and the gram weight is 110g.
Comparative example 2
The present comparative example provides a carbon rod prepared according to the following steps:
(1) Respectively weighing coconut shell activated carbon powder, ultrahigh molecular weight polyethylene and titanium dioxide heavy metal removal powder. Wherein, the powder comprises 60 parts of coconut shell activated carbon powder, 25 parts of ultra-high molecular weight polyethylene and 15 parts of titanium dioxide heavy metal removal powder by weight; the particle size of the coconut shell activated carbon powder is 80-325 meshes.
(2) Pre-mixing coconut shell activated carbon powder and titanium dioxide heavy metal removal powder in a conical stirring device at the stirring speed of 200r/min for 60min; then adding ultra-high molecular weight polyethylene, stirring at the rotation speed of 150r/min, and mixing for 30min. And then carrying out extrusion molding and cutting to obtain the carbon rod. Wherein, in the extrusion molding process, the extrusion comprises three sections of temperatures, wherein the first section of temperature is 130 ℃, the second section of temperature is 190 ℃, and the third section of temperature is 170 ℃; the rotation speed of the screw is 300r/min. When cutting, the materials are cut into 192mm long carbon rods according to the specified size, and the gram weight is 110g.
Test example 1
The test example respectively detects the removal rates of three heavy metals of lead, mercury and arsenic of the heavy metal removal carbon rods of examples 1 to 4 and the carbon rods of comparative examples 1 to 2, and comprises the following steps:
under the condition of pH6.5, lead standard concentration is 0.15mg/L, mercury standard concentration is 6 mug/L, and pentavalent arsenic standard concentration is 0.3mg/L. The flow rate of water is 2L/min, and the removal rate of heavy metals after 2T standard solution feeding and the flow rate at 30Psi are shown in Table 1.
| Item | Lead removal rate% | Mercury removal Rate% | Arsenic removal Rate% | Flow rate (L/min @ 30PSI) |
| Example 1 | 99.3％ | 95.9％ | 72％ | 3.5 |
| Example 2 | 99.1％ | 92.5％ | 81.5％ | 3.5 |
| Example 3 | 97.8％ | 89.3％ | 90.2％ | 3.5 |
| Example 4 | 98.3％ | 94.8％ | 93.5％ | 3.4 |
| Comparative example 1 | 63.5％ | 55.8％ | 50.4％ | 3.8 |
| Comparative example 2 | 98.％ | 86.5％ | 75.3％ | 1.0 |
As can be seen from Table 1, the use of the first heavy metal removal particles alone in the heavy metal removal additive provides good lead and mercury removal, but limited arsenic removal. Along with the increase of the proportion of the second heavy metal removing particles, the removal rate of arsenic is obviously increased, the removal rate of lead and mercury is still kept at a higher level, so that the mass ratio of the two heavy metal removing particles is controlled to be 2: about 1 is a more ideal ratio. With the increase of the proportion of the aqueous phase dispersion, the amount of effective particles in the heavy metal removal additive is increased, the particle size of the microspheres is reduced, and the specific surface area is increased, so that the heavy metal removal effect of the carbon rod for removing heavy metals in the embodiment 4 is better than that in the embodiment 3. In addition, compared with the comparative example 2, the flow rate of the carbon rod extrusion is higher after the carbon rod extrusion, and the main reason is that the strength of the heavy metal removing additive is good, and no broken particles are generated during screw extrusion, so that a carbon rod flow channel is not blocked by fine particles, and the flow rate is high.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (10)
1. The preparation method of the heavy metal removing additive is characterized by comprising the following steps:
s1, mixing heavy metal removing active particles and deionized water, adding hydrophilic fibers and a surfactant, and stirring to obtain an aqueous phase dispersion, wherein the heavy metal removing active particles are two selected from titanium dioxide, activated alumina, a zeolite molecular sieve, nano zinc oxide, nano iron, ferric oxide and ferric chloride;
s2, dissolving an initiator in a styrene monomer to obtain an oil phase dispersion liquid;
s3, mixing the aqueous phase dispersion liquid and the oil phase dispersion liquid, and then carrying out ultrasonic oscillation for 25-35 min to obtain an oil-in-water type emulsion;
and S4, carrying out polymerization reaction on the oil-in-water emulsion under the water bath condition, and then carrying out freeze drying, grinding and sieving to obtain the heavy metal removal additive.
2. The method for preparing the heavy metal removal additive according to claim 1, wherein the hydrophilic fiber is one or more selected from carboxymethyl cellulose, polyanionic cellulose, cellulose nanowhisker and hydroxypropyl methyl cellulose.
3. The method for preparing the heavy metal removal additive according to claim 1, wherein the surfactant is one or more selected from the group consisting of glyceryl monostearate, sodium lauryl sulfate, fatty acid soap and sodium dodecylbenzenesulfonate.
4. The method of claim 1, wherein the aqueous dispersion comprises 30 to 85 parts by weight of the heavy metal removing active particles, 10 to 20 parts by weight of the hydrophilic fiber, and 5 to 15 parts by weight of the surfactant.
5. The method of claim 1, wherein the volume ratio of the aqueous dispersion to the oil dispersion is 2 to 5:1.
6. The method for preparing the heavy metal removing additive according to claim 1, wherein the polymerization temperature is 60-80 ℃ and the reaction time is 10-15 h.
7. A heavy metal removing additive, characterized by being prepared by the preparation method according to any one of claims 1 to 6.
8. The carbon rod for removing heavy metals is characterized by comprising 50-70 parts of activated carbon powder, 25-30 parts of adhesive and 5-20 parts of heavy metal removing additive according to claim 7 in parts by weight.
9. The carbon rod for removing heavy metals according to claim 8, wherein the activated carbon powder is selected from one or more of coconut shell activated carbon powder, fruit shell activated carbon powder, wooden activated carbon powder, coal activated carbon powder and bamboo activated carbon powder; the adhesive is at least one selected from ultrahigh molecular weight polyethylene, high density polyethylene, low density polyethylene, linear low density polyethylene and polyvinylidene fluoride.
10. The preparation method of the heavy metal removing carbon rod is characterized by comprising the following steps:
the method comprises the steps of weighing the activated carbon powder, the adhesive and the heavy metal removal additive according to the parts by weight of the heavy metal removal carbon rod as claimed in any one of claims 8 or 9, premixing the activated carbon powder and the heavy metal removal additive, adding the adhesive, mixing, extruding, molding and cutting to obtain the heavy metal removal carbon rod.
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