CN110339826A - A kind of mesoporous filtrate of lightweight and preparation method thereof - Google Patents

A kind of mesoporous filtrate of lightweight and preparation method thereof Download PDF

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Publication number
CN110339826A
CN110339826A CN201910624378.1A CN201910624378A CN110339826A CN 110339826 A CN110339826 A CN 110339826A CN 201910624378 A CN201910624378 A CN 201910624378A CN 110339826 A CN110339826 A CN 110339826A
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mesoporous
filtrate
lightweight
cotton stalk
present
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刘建恒
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D17/00Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/02Separation of non-miscible liquids
    • B01D17/0202Separation of non-miscible liquids by ab- or adsorption
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D39/00Filtering material for liquid or gaseous fluids
    • B01D39/14Other self-supporting filtering material ; Other filtering material
    • B01D39/20Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
    • B01D39/2068Other inorganic materials, e.g. ceramics
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D39/00Filtering material for liquid or gaseous fluids
    • B01D39/14Other self-supporting filtering material ; Other filtering material
    • B01D39/20Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
    • B01D39/2068Other inorganic materials, e.g. ceramics
    • B01D39/2072Other inorganic materials, e.g. ceramics the material being particulate or granular
    • B01D39/2075Other inorganic materials, e.g. ceramics the material being particulate or granular sintered or bonded by inorganic agents
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28078Pore diameter
    • B01J20/28083Pore diameter being in the range 2-50 nm, i.e. mesopores
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/32Hydrocarbons, e.g. oil
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/10Nature of the water, waste water, sewage or sludge to be treated from quarries or from mining activities

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Geology (AREA)
  • Nanotechnology (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Water Treatment By Sorption (AREA)

Abstract

The invention belongs to filtering material fields more particularly to a kind of mesoporous filtrate of lightweight and preparation method thereof.The mesoporous filtrate of lightweight of the present invention is made of cotton stalk, diaspore, clay, crystalline flake graphite, potassium bichromate, polypropylene fiber, potassium dihydrogen phosphate, isomery undecyl alcohol block polyether, phenolic resin and polyacrylate dispersion.After tested, the mesoporous filtrate of lightweight of the present invention has ideal absorption, filtering, separating effect, can obtain it is higher be separated by filtration efficiency, and the present invention is widely applicable, can be widely used for all kinds of sewage treatments, is especially suitable for carrying out isolation of purified to the grease in oil field.Furthermore, the mesoporous filtrate of lightweight of the present invention also has many advantages, such as clean and environmental protection, using safe, corrosivity is low, degradability is good, low in cost, the popularization and application of the mesoporous filtrate of lightweight of the present invention not only contribute to expand the suitable application area of mesoporous material, also better solution can be provided for the water-oil separating purified treatment in oil field, therefore be very suitable to current industry requirement.

Description

A kind of mesoporous filtrate of lightweight and preparation method thereof
Technical field
The invention belongs to filtering material fields more particularly to a kind of mesoporous filtrate of lightweight and preparation method thereof.
Background technique
Mesoporous (or mesoporous) material is that a kind of aperture has huge specific surface area and three between micropore and macropore Tie up the new material of cellular structure.Mesoporous material is with excellent characteristics not available for many other porous materials: as having height Spend orderly cellular structure;Aperture size can the variation in wider range (2-50nm);Mesoporous various shapes, hole wall composition and property Matter is controllable;High heat stability and chemical stability etc..Therefore, mesoporous material is in catalysis, absorption, separation and light, electricity, magnetic etc. Numerous areas has very big application value and good development prospect.
Deep-bed filtration is that a kind of permission suspended matter enters filter type inside filtering layer, and the molecule of every kind of impurity is straight in liquid Diameter is different, and also there were significant differences for freedom of motion, and when mesoporous material is used for deep-bed filtration, different apertures (2-50nm) is logical Road is also different the affinity and adsorption capacity of different impurities, and therefore, the sized molecules impurity in liquid can be different It sieves, retain and adsorbs in the duct in aperture.
Blowdown with Environmental and the pay attention to day by day of water quality ecological, to petrochemical enterprise and sewage treatment industry More stringent requirements are proposed for standard, and it is continuous that the proposition of new standard promotes sewage treatment enterprise to carry out its water purification technology and equipment Upgrading.However, major part sewage plant still uses the mainstreams such as continuous Microfiltration equipment (mocromembrane), ultrafiltration apparatus dirty at present Water terminal process equipment, not only operation mode is single, and operation expense is high, and its filter efficiency does not make us full yet Meaning.At the same time, grease process field of the mesoporous material of indefinite form in sewage treatment especially oil field does not obtain adequately yet Research and application.
Summary of the invention
To develop the new application of mesoporous material and expanding its suitable application area, while being mentioned for the water-oil separating purified treatment in oil field For better solution, our company technical staff passes through continuous recipe determination, technique on the basis of many years production practices Grope and contrast test, final develop obtain a kind of mesoporous filtrate of novel light.The mesoporous filtrate of lightweight of the present invention can fit extensively For all kinds of sewage treatments, it is especially suitable for carrying out isolation of purified to the grease in oil field.After tested, the mesoporous filter of lightweight of the present invention is utilized Material can obtain it is higher be separated by filtration efficiency, and this mesoporous filtrate clean and environmental protection, it is widely applicable, using safe, corrosivity is low, Degradability is good and low in cost.
The present invention provides a kind of mesoporous filtrates of lightweight, it is made of the raw material of following weight parts:
Cotton stalk 130-150;
Diaspore 25-30;
Clay 15-20;
Crystalline flake graphite 80-110;
Potassium bichromate 10-20;
Polypropylene fiber 25-30;
15% potassium dihydrogen phosphate 25-45;
Isomery undecyl alcohol block polyether 7-10;
Phenolic resin 55-70;
Polyacrylate dispersion 30-50.
The parts by weight of above-mentioned raw materials are preferred:
Cotton stalk 130;
Diaspore 25;
Clay 15;
Crystalline flake graphite 80;
Potassium bichromate 10;
Polypropylene fiber 25;
15% potassium dihydrogen phosphate 25;
Isomery undecyl alcohol block polyether 7;
Phenolic resin 55;
Polyacrylate dispersion 30.
The parts by weight of above-mentioned raw materials are further preferably:
Cotton stalk 140;
Diaspore 28;
Clay 17;
Crystalline flake graphite 100;
Potassium bichromate 15;
Polypropylene fiber 27;
15% potassium dihydrogen phosphate 30;
Isomery undecyl alcohol block polyether 9;
Phenolic resin 65;
Polyacrylate dispersion 35.
The parts by weight of above-mentioned raw materials are further preferably:
Cotton stalk 150;
Diaspore 30;
Clay 20;
Crystalline flake graphite 110;
Potassium bichromate 20;
Polypropylene fiber 30;
15% potassium dihydrogen phosphate 45;
Isomery undecyl alcohol block polyether 10;
Phenolic resin 70;
Polyacrylate dispersion 50.
Further, the mesoporous filtrate of lightweight of the present invention is made through following step:
(1) cotton stalk is pyrolyzed the cotton stalk powder being carbonized after crushing, it is mixed with diaspore powder, clay It closes uniformly, is put into baker, 700 DEG C of bakings obtain mixture 1 in 4 hours;
(2) after mixing crystalline flake graphite, potassium bichromate and 15% potassium dihydrogen phosphate, 90 DEG C are heated 0.5 hour, filtering It is mixed after drying with polypropylene fiber, isomery undecyl alcohol block polyether, obtains mixture 2 within hot-pressing processing 1 hour;
(3) phenol-formaldehyde resin powder is heated 6 hours at 160 DEG C, is then rinsed with the dilute hydrochloric acid of 0.1mol/L, is obtained after dry Modified phenolic resin cosmetics;
(4) said mixture 1, mixture 2, modified phenolic resin cosmetics are uniformly mixed, polyacrylate is added thereto Lotion is put into die for molding after being stirred well to substantially uniformity, after hot-pressing processing 2 hours under the conditions of 1000-1600 DEG C into Row sintering processes to get arrive the mesoporous filtrate finished product of lightweight.
Further, the condition of hot-pressing processing described in above-mentioned (2) step is 450 DEG C, 2.5Mpa.
Further, the condition of hot-pressing processing described in above-mentioned (4) step is 300 DEG C, 5Mpa.
Moreover, it relates to application of the above-mentioned mesoporous filtrate of lightweight in preparation water-oil separating filter material.
The invention further relates to application of the mesoporous filtrate of above-mentioned lightweight in sewage treatment.
After tested, the mesoporous filtrate of lightweight of the present invention has ideal absorption, filtering, separating effect, can obtain higher It is separated by filtration efficiency, and the present invention is widely applicable, can be widely used for all kinds of sewage treatments, is especially suitable for carrying out the grease in oil field Isolation of purified.In addition, the mesoporous filtrate of lightweight of the present invention also have clean and environmental protection, using safe, corrosivity is low, degradability is good, at The advantages that this is cheap, the popularization and application of the mesoporous filtrate of lightweight of the present invention not only contribute to expand the suitable application area of mesoporous material, also Better solution can be provided for the water-oil separating purified treatment in oil field, therefore be very suitable to current industry requirement.
Specific embodiment
Illustrate embodiments of the present invention below by way of specific specific example, those skilled in the art can be by this specification Other advantages and efficacy of the present invention can be easily understood for disclosed content.The present invention can also pass through in addition different specific realities The mode of applying is embodied or practiced, the various details in this specification can also based on different viewpoints and application, without departing from Various modifications or alterations are carried out under spirit of the invention.
Before further describing the specific embodiments of the present invention, it should be appreciated that protection scope of the present invention is not limited to down State specific specific embodiment;It is also understood that term used in the embodiment of the present invention is specific specific in order to describe Embodiment, rather than limiting the scope of protection of the present invention.
Unless otherwise defined, all technical and scientific terms and those skilled in the art of the present technique used in the present invention are usual The meaning of understanding is identical.In addition to specific method, equipment, material used in the embodiment, according to those skilled in the art Grasp and record of the invention to the prior art, can also use and method described in the embodiment of the present invention, equipment, material Any method, equipment and the material of the similar or equivalent prior art realizes the present invention.
Embodiment 1
A kind of mesoporous filtrate of lightweight, is made of the raw material of following weight parts:
Cotton stalk 130;
Diaspore 25;
Clay 15;
Crystalline flake graphite 80;
Potassium bichromate 10;
Polypropylene fiber 25;
15% potassium dihydrogen phosphate 25;
Isomery undecyl alcohol block polyether 7;
Phenolic resin 55;
Polyacrylate dispersion 30.
The preparation method is as follows:
(1) cotton stalk is pyrolyzed the cotton stalk powder being carbonized after crushing, it is mixed with diaspore powder, clay It closes uniformly, is put into baker, 700 DEG C of bakings obtain mixture 1 in 4 hours;
(2) after mixing crystalline flake graphite, potassium bichromate and 15% potassium dihydrogen phosphate, 90 DEG C are heated 0.5 hour, filtering It is mixed after drying with polypropylene fiber, isomery undecyl alcohol block polyether, 450 DEG C, mixed within hot-pressing processing 1 hour under the conditions of 2.5Mpa Close object 2;
(3) phenol-formaldehyde resin powder is heated 6 hours at 160 DEG C, is then rinsed with the dilute hydrochloric acid of 0.1mol/L, is obtained after dry Modified phenolic resin cosmetics;
(4) said mixture 1, mixture 2, modified phenolic resin cosmetics are uniformly mixed, polyacrylate is added thereto Lotion is stirred well to after substantially uniformity and is put into die for molding, 300 DEG C, under the conditions of 5Mpa after hot-pressing processing 2 hours 1100 It is sintered under the conditions of DEG C to get the mesoporous filtrate finished product of lightweight is arrived.
Embodiment 2
A kind of mesoporous filtrate of lightweight, is made of the raw material of following weight parts:
Cotton stalk 140;
Diaspore 28;
Clay 17;
Crystalline flake graphite 100;
Potassium bichromate 15;
Polypropylene fiber 27;
15% potassium dihydrogen phosphate 30;
Isomery undecyl alcohol block polyether 9;
Phenolic resin 65;
Polyacrylate dispersion 35.
The preparation method is as follows:
(1) cotton stalk is pyrolyzed the cotton stalk powder being carbonized after crushing, it is mixed with diaspore powder, clay It closes uniformly, is put into baker, 700 DEG C of bakings obtain mixture 1 in 4 hours;
(2) after mixing crystalline flake graphite, potassium bichromate and 15% potassium dihydrogen phosphate, 90 DEG C are heated 0.5 hour, filtering It is mixed after drying with polypropylene fiber, isomery undecyl alcohol block polyether, 450 DEG C, mixed within hot-pressing processing 1 hour under the conditions of 2.5Mpa Close object 2;
(3) phenol-formaldehyde resin powder is heated 6 hours at 160 DEG C, is then rinsed with the dilute hydrochloric acid of 0.1mol/L, is obtained after dry Modified phenolic resin cosmetics;
(4) said mixture 1, mixture 2, modified phenolic resin cosmetics are uniformly mixed, polyacrylate is added thereto Lotion is stirred well to after substantially uniformity and is put into die for molding, 300 DEG C, under the conditions of 5Mpa after hot-pressing processing 2 hours 1300 It is sintered under the conditions of DEG C to get the mesoporous filtrate finished product of lightweight is arrived.
Embodiment 3
A kind of mesoporous filtrate of lightweight, is made of the raw material of following weight parts:
Cotton stalk 150;
Diaspore 30;
Clay 20;
Crystalline flake graphite 110;
Potassium bichromate 20;
Polypropylene fiber 30;
15% potassium dihydrogen phosphate 45;
Isomery undecyl alcohol block polyether 10;
Phenolic resin 70;
Polyacrylate dispersion 50.
The preparation method is as follows:
(1) cotton stalk is pyrolyzed the cotton stalk powder being carbonized after crushing, it is mixed with diaspore powder, clay It closes uniformly, is put into baker, 700 DEG C of bakings obtain mixture 1 in 4 hours;
(2) after mixing crystalline flake graphite, potassium bichromate and 15% potassium dihydrogen phosphate, 90 DEG C are heated 0.5 hour, filtering It is mixed after drying with polypropylene fiber, isomery undecyl alcohol block polyether, 450 DEG C, mixed within hot-pressing processing 1 hour under the conditions of 2.5Mpa Close object 2;
(3) phenol-formaldehyde resin powder is heated 6 hours at 160 DEG C, is then rinsed with the dilute hydrochloric acid of 0.1mol/L, is obtained after dry Modified phenolic resin cosmetics;
(4) said mixture 1, mixture 2, modified phenolic resin cosmetics are uniformly mixed, polyacrylate is added thereto Lotion is stirred well to after substantially uniformity and is put into die for molding, 300 DEG C, under the conditions of 5Mpa after hot-pressing processing 2 hours 1500 It is sintered under the conditions of DEG C to get the mesoporous filtrate finished product of lightweight is arrived.
Filter absorption property test
Test object: the mesoporous filtrate sample of lightweight (embodiment 1-3 sample) of the present invention and commercially available porous filter-material.
Test object: underground water, oily wastewater through Air Exposure.
Test index: amount containing Fe, solid suspension, oil removal rate after turbidity, filter after filter.
Test result is as follows shown in table 1:
1 each group sample filtering absorption property test result of table
Sample Turbidity after filter Amount containing Fe after filter Solid suspension Oil removal rate
Embodiment 1 ≤1FTU 0.2mg/L 4mg/L 85%
Embodiment 2 ≤1FTU 0.2mg/L 1mg/L 94%
Embodiment 3 ≤1FTU 0.2mg/L 3mg/L 91%
Commercially available filtrate ≤5FTU 0.4mg/L 9mg/L 56%
The preferred embodiments of the disclosure and embodiment are explained in detail above, but the present invention is not limited to The above-described embodiment and examples can also not depart from the present invention within the knowledge of those skilled in the art Various changes can be made under the premise of design.

Claims (9)

1. a kind of mesoporous filtrate of lightweight, it is characterised in that it is made of the raw material of following weight parts:
Cotton stalk 130-150;
Diaspore 25-30;
Clay 15-20;
Crystalline flake graphite 80-110;
Potassium bichromate 10-20;
Polypropylene fiber 25-30;
15% potassium dihydrogen phosphate 25-45;
Isomery undecyl alcohol block polyether 7-10;
Phenolic resin 55-70;
Polyacrylate dispersion 30-50.
2. the mesoporous filtrate of lightweight as described in claim 1, wherein the parts by weight of each raw material are:
Cotton stalk 130;
Diaspore 25;
Clay 15;
Crystalline flake graphite 80;
Potassium bichromate 10;
Polypropylene fiber 25;
15% potassium dihydrogen phosphate 25;
Isomery undecyl alcohol block polyether 7;
Phenolic resin 55;
Polyacrylate dispersion 30.
3. the mesoporous filtrate of lightweight as described in claim 1, wherein the parts by weight of each raw material are:
Cotton stalk 140;
Diaspore 28;
Clay 17;
Crystalline flake graphite 100;
Potassium bichromate 15;
Polypropylene fiber 27;
15% potassium dihydrogen phosphate 30;
Isomery undecyl alcohol block polyether 9;
Phenolic resin 65;
Polyacrylate dispersion 35.
4. the mesoporous filtrate of lightweight as described in claim 1, wherein the parts by weight of each raw material are:
Cotton stalk 150;
Diaspore 30;
Clay 20;
Crystalline flake graphite 110;
Potassium bichromate 20;
Polypropylene fiber 30;
15% potassium dihydrogen phosphate 45;
Isomery undecyl alcohol block polyether 10;
Phenolic resin 70;
Polyacrylate dispersion 50.
5. the mesoporous filtrate of lightweight as described in claim 1, it is characterised in that the mesoporous filtrate of lightweight is made through following step:
(1) cotton stalk is pyrolyzed the cotton stalk powder being carbonized after crushing, it is mixed with diaspore powder, clay It is even, it is put into baker, 700 DEG C of bakings obtain mixture 1 in 4 hours;
(2) after mixing crystalline flake graphite, potassium bichromate and 15% potassium dihydrogen phosphate, 90 DEG C are heated 0.5 hour, filtration drying It is mixed afterwards with polypropylene fiber, isomery undecyl alcohol block polyether, obtains mixture 2 within hot-pressing processing 1 hour;
(3) phenol-formaldehyde resin powder is heated 6 hours at 160 DEG C, is then rinsed with the dilute hydrochloric acid of 0.1mol/L, is modified after dry Phenol-formaldehyde resin powder;
(4) said mixture 1, mixture 2, modified phenolic resin cosmetics are uniformly mixed, polyacrylate dispersion are added thereto, It is put into die for molding after being stirred well to substantially uniformity, is sintered under the conditions of 1000-1600 DEG C after hot-pressing processing 2 hours It handles to get the mesoporous filtrate finished product of lightweight is arrived.
6. the mesoporous filtrate of lightweight as claimed in claim 5, wherein the condition of hot-pressing processing described in (2) step be 450 DEG C, 2.5Mpa。
7. the mesoporous filtrate of lightweight as claimed in claim 5, wherein the condition of hot-pressing processing described in (4) step be 300 DEG C, 5Mpa。
8. such as application of the mesoporous filtrate of the described in any item lightweights of claim 1-7 in preparation water-oil separating filter material.
9. such as application of the mesoporous filtrate of the described in any item lightweights of claim 1-7 in sewage treatment.
CN201910624378.1A 2019-07-11 2019-07-11 A kind of mesoporous filtrate of lightweight and preparation method thereof Pending CN110339826A (en)

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Application publication date: 20191018