CN105251439A - Inorganic silicon nanometer adsorbent and preparing method thereof - Google Patents
Inorganic silicon nanometer adsorbent and preparing method thereof Download PDFInfo
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Abstract
The invention relates to an inorganic silicon nanometer adsorbent for adsorbing toxic and harmful gas (formaldehyde, ammonia, benzene, TVOC and the like), peculiar smells and moisture in air and a preparing method thereof. The adsorbent is prepared from, by mass, 0.020% to 0.024% of Fe2O3, 0.11% to 0.15% of Al2O3, 0.022% to 0.026% of CaO, 95.10% to 95.30% of SiO2 and the balance loss on ignition. The specific area of the adsorbent is 200 m<2>/g to 2,000 m<2>/g, the average pore size is 0.5 nm to 20 nm, and the total pore volume is 0.1 ml/g to 10 ml/g. The adsorbent has the advantages of being stable in chemical property, high in adsorption performance, good in heat stability and high in mechanical strength.
Description
Technical field
The present invention relates to pernicious gas sorbing material, the toxic and harmful (formaldehyde, ammonia, benzene, TVOC etc.) specifically in a kind of absorbed air, inorganic silicon nano adsorber of peculiar smell, moisture content and preparation method thereof.
Background technology
At present, having the means such as chemisorbed and physical absorption to the process of pernicious gas, the activated alumina material of chemisorbed more commonly potassium permanganate load, take aluminium oxide as carrier, take potassium permanganate as active material, but potassium permanganate itself has corrosivity, irritant to organizing, easily pollute skin blackening look, the black dye of oral mucous membrane, gastrorrhagia, hepatorenal damage etc., potassium permanganate lethal dose is about 10 grams.Physical absorption with active carbon and derived product thereof for main representative, but active carbon is inflammable, belongs to dangerous material, and carries a large amount of black dust, can pollute indoor, environment inside car, bring potential safety hazard.
Existing air purifier, main employing ozone purification technology, anion dedusting technology and high voltage electrostatic technique, ozone technology has sterilization, deodorization, but low to the removal efficiency of organic pollution; In addition, ozone itself is to human body and bad environmental.Anion and high voltage electrostatic technique are a kind of physical actions, can remove the flue dust in air, but cannot remove purification to the pollution that chemistry, biology, microorganism etc. are caused.In air purifier product configurations, inner active carbon of filling bears the major function of formaldehyde adsorption, but because active carbon itself exists absorption saturation value, and it is unchanged before and after absorption, user cannot be made correctly distinguish, electronic component is inconvenient dismounting and change again, and in the course of time, product can become an ornament given a long price for.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of inorganic silicon nano adsorber containing a large amount of nano micropore structure capable and preparation method thereof is provided, mainly solve indoor, in relative closure environment, toxic and harmful (formaldehyde, ammonia, benzene, TVOC etc.), peculiar smell and moisture, to the harm in human lives, have stable chemical nature, absorption property is high, Heat stability is good, mechanical strength are higher feature in car etc.
For achieving the above object, the present invention adopts following technical scheme:
A kind of inorganic silicon nano adsorber, chemical composition and the mass percent thereof of described adsorbent are: Fe O: 0.020-0.024%, Al O: 0.11-0.15%, CaO:0.022-0.026%, SiO: 95.10-95.30%, and surplus is loss on ignition; The specific area of described adsorbent is 200 ㎡/g-2000 ㎡/g, and average pore size is 0.5nm-20nm, and total pore volume is 0.1ml/g-10ml/g.
Preferably, chemical composition and the mass percent thereof of described adsorbent are: Fe O: 0.022%, Al O: 0.13%, CaO:0.024%, SiO: 95.18%, loss on ignition: 4.644%; The specific area of described adsorbent is 750-900 ㎡/g, and average pore size is 1.0-2.5nm, and total pore volume is 0.35-0.5ml/g.
Above-mentioned inorganic silicon nano adsorber is nontoxic, tasteless, colourless or white, solid spherical, hemispherical, bulk, irregular bulk, powdery, non-combustible, water insoluble, non-volatile.
The preparation method of above-mentioned inorganic silicon nano adsorber, carries out in the steps below:
(1) raw material preparation: prepare sulfuric acid solution with special process, wherein sulfuric acid quality is 5-40% than concentration, prepares sodium silicate solution with special process, and wherein sodium metasilicate quality is 5-50% than concentration.Under the environment of 5 DEG C-80 DEG C, spray under the pressure of 1-15MPa, in atmosphere granulation, be atomized;
(2) be atomized: be ejected to by proportioning solution in normal temperature air environment, solution coagulates is atomized, and is sprinkled into receiver, and in receiver, water is 10 containing the quality of acid than concentration
-8.5%-10
-3%;
(3) alternating temperature leaves standstill: the time of repose of inorganic silicon nano adsorber is 4.5min-15h, and dwell temperature is 5-85 DEG C, heats gradually stage by stage standing, coordinates activation to complete product technology requirement better to make product;
(4) activate:
A. acid activation: use exchanged acid to carry out acid bubble, temperature 10-90 DEG C, sour bubble time 1-12h are steeped in acid, and the quality of exchanged acid is 0.02%-10% than concentration, the height that the most high liquid level (HLL) of exchanged acid exceeds the highest of gel is 5-60cm;
B. water activation: adopt pure water to soak, and air-blowing makes inorganic silicon fully contact with water, temperature is 20-90 DEG C;
C. acid soak: water is 10 containing the quality of acid than concentration
-8%-0.001%;
D. high-temperature activation: be 50-200 DEG C of high-temperature activation in temperature, the humidity 0.1%-99% of environment in heating loss process.
(5) strengthen: repeat step (4) A, (4) B, strengthen index and Data Control precision in preparation link, make inorganic silicon nano adsorber specific area be 200 ㎡/g-2000 ㎡/g, average pore size is 0.5nm-20nm, and total pore volume is 0.1ml/g-10ml/g.
Preferably, step (1) mesosilicic acid sodium modulus is 3.25-3.45.
Preferably, in step (2), the mass concentration ratio of acid content is 10
-5%-10
-8.5%.
Preferably, in described step (4) A, the quality of exchanged acid is 0.8%-6% than concentration, and acid bubble temperature is 40-50 DEG C, sour bubble time 2-8h.
Preferably, in described step (4) A, exchanged acid is one or more in hydrochloric acid, sulfuric acid, nitric acid, oxalic acid or citric acid, and the quality of acid is 0.02%-6% than concentration.
Preferably, in described step (4) B, the temperature of a reaming is 40-60 DEG C.
Preferably, in described step (4) C, the quality of acid is 10 than concentration
-7%-10
-5%.
Preferably, in described step (4) D, bake out temperature is 70-140 DEG C, and humidity is 0.5%-80%.
Adopt the present invention of technique scheme, compared with prior art, its beneficial effect is:
Activated silica nano adsorber of the present invention, nontoxic, colorless and odorless, inside has a large amount of hole, can the toxic and harmful such as formaldehyde, toluene, benzene, ammonia, TOVC, peculiar smell, moisture in absorbed air, can be used for every field and the industries such as industry, agricultural, car industry, real estate.By national indoor cart environment and environment-friendly products Quality Supervision and Inspection Center dependence test, in 24 hours, PARA FORMALDEHYDE PRILLS(91,95) removal rate reaches 93%, ammonia clearance reaches 91%, benzene removal rate reaches 70%, TVOC removal rate reaches 80%, meet food and drug safety standard, wherein dioxide-containing silica reaches 99.5%.
The provable activated silica nano adsorber absorption purifying effect of the present invention of following test.
Test one, be in the test chamber of 1.5m3 at two identical airtight volumes and carry out, one is sample chamber, and another is blank cabin, is placed in sample chamber by some samples; Two cabins are put in identical Form aldehyde release source (uninterrupted slow releasing) respectively, and source of release is mixed with air in cabin, tends to balance, in sample detecting cabin, air formaldehyde concentration is initial concentration value; Air formaldehyde concentration value in difference sampling determination two cabin after 24h.
Removal effect computing formula: y=(Ca-Cb)/Ca*100%
In formula: y=removal rate; Ca=24h blank cabin pollutant levels value; Cb=sample chamber pollutant levels value.
Result of the test sees the following form:
Test two, be in the test chamber of 1.5m3 at two identical airtight volumes and carry out, one is sample chamber, and another is blank cabin, is placed in sample chamber by some samples; Identical ammonia source of release (uninterrupted slow releasing) is put into two cabins respectively, and source of release is mixed with air in cabin, tends to balance, in sample detecting cabin, ammonia concentration in air is initial concentration value; Ammonia concentration in air value in difference sampling determination two cabin after 24h.
Removal effect computing formula: y=(Ca-Cb)/Ca*100%
In formula: y=removal rate; Ca=24h blank cabin pollutant levels value; Cb=sample chamber pollutant levels value.
Result of the test sees the following form:
Test three, be in the test chamber of 1.5m3 at two identical airtight volumes and carry out, one is sample chamber, and another is blank cabin, is placed in sample chamber by some samples; Identical benzene source of release (uninterrupted slow releasing) is put into two cabins respectively, and source of release is mixed with air in cabin, tends to balance, in sample detecting cabin, benzene in air concentration is initial concentration value; Benzene in air concentration value in difference sampling determination two cabin after 24h.
Removal effect computing formula: y=(Ca-Cb)/Ca*100%
In formula: y=removal rate; Ca=24h blank cabin pollutant levels value; Cb=sample chamber pollutant levels value.
Result of the test sees the following form:
Test four, be in the test chamber of 1.5m3 at two identical airtight volumes and carry out, one is sample chamber, and another is blank cabin, is placed in sample chamber by some samples; Identical TVOC source of release (uninterrupted slow releasing) is put into two cabins respectively, and source of release is mixed with air in cabin, tends to balance, in sample detecting cabin, in air, TVOC concentration is initial concentration value; Respectively TVOC concentration value in air in sampling determination two cabin after 24h.
Removal effect computing formula: y=(Ca-Cb)/Ca*100%
In formula: y=removal rate; Ca=24h blank cabin pollutant levels value; Cb=sample chamber pollutant levels value.
Result of the test sees the following form:
Detailed description of the invention
By the following examples in detail the present invention is described in detail, object is only to understand content of the present invention better, the cited case protection domain described in unrestricted technical solution of the present invention.
Embodiment 1, sprays reaction solution under a certain pressure, and the raw material participating in reaction has H SO, Na CO, H O etc., granulation of condensing in atmosphere respectively, and obtaining spherical, hemispherical, its particle size range of oval particle is 0.1mm-10mm.
(1) raw material preparation:
Under the environment of 30 DEG C, utilize sodium silicate solution and sulfuric acid solution reaction, described sodium silicate solution mesosilicic acid sodium quality is 18.25% than concentration, and in sulfuric acid solution, the quality of sulfuric acid is 22% than concentration.
(2) be atomized:
Be ejected to by proportioning solution in normal temperature air environment, solution coagulates is atomized, and is sprinkled into receiver, and in receiver, water is 10 containing the quality of acid than concentration
-6.5%.
(3) alternating temperature leaves standstill:
The time of repose of inorganic silicon is 1h, and dwell temperature is 30 DEG C, 31 DEG C, 33 DEG C, 36 DEG C, 40 DEG C, 45 DEG C, 50 DEG C.
(4) activate:
A. acid activation: use exchanged acid to carry out acid bubble, temperature 30 DEG C is steeped in acid, sour bubble time 2h, and the quality of described exchanged acid is 4.5% than concentration, the height that the most high liquid level (HLL) of exchanged acid exceeds the highest of gel is 40cm.
B. water activation: adopt pure water to soak, and air-blowing makes inorganic silicon fully contact with water, temperature is 30 DEG C.
C. acid soak: water is 0.0001% containing the quality of acid than concentration.
D. high-temperature activation: high-temperature activation under temperature is 120 DEG C of conditions, the humidity 7% of environment in heating loss process.
(5) strengthen:
A. repeat (4)-A processing step, the quality of secondary exchanged acid acid is 1.0% than concentration; Acid bubble 3h;
B. repeat (4)-B processing step, second reaming adopts pure water to soak, and temperature is 35 DEG C;
C. repeat (4)-A processing step, the quality of three exchanged acid acid is 1.5% than concentration; Acid bubble 3.5h;
D. repeat (4)-B processing step, three reamings adopt pure water to soak, and temperature is 40 DEG C.
According to the inorganic silicon nano adsorber that above-mentioned technique is obtained, its chemical composition and mass percent thereof are: Fe O: 0.022%, Al O: 0.13%, CaO:0.024%, SiO: 95.18%; Its average pore size is 1.0-2.5nm, and specific area is 750-900 ㎡/g, and total pore volume is 0.35-0.5ml/g.
Embodiment 2, imports reaction solution in container, and the raw material participating in reaction has H SO, Na CO, H O etc. respectively, and condense into irregular bulk after solution mixing, particle size range is 0.1mm-10mm.
(1) raw material preparation:
Under the environment of 30 DEG C, utilize sodium silicate solution and sulfuric acid solution reaction, described sodium silicate solution mesosilicic acid sodium quality is 16.1% than concentration, and in sulfuric acid solution, the quality of sulfuric acid is 21.1% than concentration.
(2) be atomized:
Be ejected to by proportioning solution in normal temperature air environment, solution coagulates is atomized, and is sprinkled into receiver, and in receiver, water is 10 containing the quality of acid than concentration
-6.5%.
(3) alternating temperature leaves standstill:
The time of repose of inorganic silicon nano adsorber is 3h, and dwell temperature is 40 DEG C, 42 DEG C, 45 DEG C, 50 DEG C, 60 DEG C.
(4) activate:
A. acid activation: use exchanged acid to carry out acid bubble, temperature 45 C is steeped in acid, sour bubble time 4h, and the quality of described exchanged acid is 4.8% than concentration, the height that the most high liquid level (HLL) of exchanged acid exceeds the highest of gel is 50cm.
B. water activation: adopt pure water to soak, and air-blowing makes inorganic silicon fully contact with water, temperature is 45 DEG C.
C. acid soak: water is 0.00015% containing the quality of acid than concentration.
D. high-temperature activation: high-temperature activation under temperature is 110 DEG C of conditions, the humidity 5% of environment in heating loss process.
(5) strengthen:
A. repeat (4)-A processing step, the quality of secondary exchanged acid acid is 1.5% than concentration; Acid bubble 4h;
B. repeat (4)-B processing step, second reaming adopts pure water to soak, and temperature is 40 DEG C;
C. repeat (4)-A processing step, the quality of three exchanged acid acid is 2% than concentration; Acid bubble 4.5h;
D. repeat (4)-B processing step, three reamings adopt pure water to soak, and temperature is 45 DEG C.
According to the inorganic silicon nano adsorber that above-mentioned technique is obtained, its chemical composition and mass percent thereof are: Fe O: 0.02%, Al O: 0.15%, CaO:0.022%, SiO: 95.3%; Its average pore size is 2.5-5nm, and specific area is 500-700 ㎡/g, and total pore volume is 0.45-0.7ml/g.
Embodiment 3: spray reaction solution under a certain pressure, the raw material participating in reaction has H SO, Na CO, H O etc., granulation of condensing in atmosphere respectively, and obtaining spherical, hemispherical, its particle size range of oval particle is 0.1mm-10mm.
(1) raw material preparation:
Under the environment of 35 DEG C, utilize sodium silicate solution and sulfuric acid solution reaction, described sodium silicate solution mesosilicic acid sodium quality is 17.11% than concentration, and in sulfuric acid solution, the quality of sulfuric acid is 20.37% than concentration.
(2) be atomized:
Be ejected to by proportioning solution in normal temperature air environment, solution coagulates is atomized, and is sprinkled into receiver, and in receiver, water is 10 containing the quality of acid than concentration
-6.5%.
(3) alternating temperature leaves standstill:
The time of repose of inorganic silicon is 5h, and dwell temperature is 30 DEG C, 40 DEG C, 50 DEG C, 55 DEG C, 57 DEG C, 60 DEG C.
(4) activate:
A. acid activation: use exchanged acid to carry out acid bubble, temperature 21 DEG C is steeped in acid, sour bubble time 2h, and the quality of described exchanged acid is 4.2% than concentration, the height that the most high liquid level (HLL) of exchanged acid exceeds the highest of gel is 50cm.
B. water activation: adopt pure water to soak, and air-blowing makes inorganic silicon fully contact with water, temperature is 50 DEG C.
C. acid soak: water is 0.0002% containing the quality of acid than concentration.
D. high-temperature activation: high-temperature activation under temperature is 100 DEG C of conditions, the humidity 9% of environment in heating loss process.
(5) strengthen:
A. repeat (4)-A processing step, the quality of secondary exchanged acid acid is 1.2% than concentration; Acid bubble 5h;
B. repeat (4)-B processing step, second reaming adopts pure water to soak, and temperature is 42 DEG C;
C. repeat (4)-A processing step, the quality of three exchanged acid acid is 1.7% than concentration; Acid bubble 2.5h;
D. repeat (4)-B processing step, three reamings adopt pure water to soak, and temperature is 47 DEG C.
According to the inorganic silicon nano adsorber that above-mentioned technique is obtained, its chemical composition and mass percent thereof are: Fe O: 0.024%, Al O: 0.11%, CaO:0.026%, SiO: 95.1%; Its average pore size is 1-3nm, and specific area is 1000-1200 ㎡/g, and total pore volume is 0.55-0.75ml/g.
The inorganic silicon nano adsorber that above-described embodiment is worth, can be used as pernicious gas, deodorizing, peculiar smell adsorption agent, drier, moisture regulator etc. in the family; Industry is used as petroleum hydrocarbon decolorizer, catalyst carrier, pressure-variable adsorption agent etc.; Fine chemistry industry separating-purifying agent, Beer stabilizer, coating thickener, toothpaste abrasives, delustering agent, coating for wall surface, environmental-protection decorative ancient piece of jade, round, flat and with a hole in its centre material etc.
The foregoing is only the better feasible embodiment of the present invention, not thereby limit to interest field of the present invention, the equivalence change that all utilizations description of the present invention is done, be all contained within interest field of the present invention.
Claims (10)
1. an inorganic silicon nano adsorber, is characterized in that, chemical composition and the mass percent thereof of described adsorbent are: Fe O: 0.020-0.024%, Al O: 0.11-0.15%, CaO:0.022-0.026%, SiO: 95.10-95.30%, surplus is loss on ignition; The specific area of described adsorbent is 200 ㎡/g-2000 ㎡/g, and average pore size is 0.5nm-20nm, and total pore volume is 0.1ml/g-10ml/g.
2. inorganic silicon nano adsorber according to claim 1, is characterized in that, chemical composition and the mass percent thereof of described adsorbent are: Fe O: 0.022%, Al O: 0.13%, CaO:0.024%, SiO: 95.18%, loss on ignition: 4.644%; The specific area of described adsorbent is 750-900 ㎡/g, and average pore size is 1.0-2.5nm, and total pore volume is 0.35-0.5ml/g.
3. a preparation method for inorganic silicon nano adsorber as claimed in claim 1, is characterized in that, carry out in the steps below:
(1) raw material preparation: prepare sulfuric acid solution with special process, wherein sulfuric acid quality is 5-40% than concentration, prepares sodium silicate solution with special process, and wherein sodium metasilicate quality is 5-50% than concentration;
Under the environment of 5 DEG C-80 DEG C, spray under the pressure of 1-15MPa, in atmosphere granulation, be atomized;
(2) be atomized: be ejected to by proportioning solution in normal temperature air environment, solution coagulates is atomized, and is sprinkled into receiver, and in receiver, water is 10 containing the quality of acid than concentration
-8.5%-10
-3%;
(3) alternating temperature leaves standstill: the time of repose of inorganic silicon nano adsorber is 4.5min-15h, and dwell temperature is 5-85 DEG C, heats gradually stage by stage standing, coordinates activation to complete product technology requirement better to make product;
(4) activate:
Acid activation: use exchanged acid to carry out acid bubble, temperature 10-90 DEG C, sour bubble time 1-12h are steeped in acid, and the quality of exchanged acid is 0.02%-10% than concentration, the height that the most high liquid level (HLL) of exchanged acid exceeds the highest of gel is 5-60cm;
Water activates: adopt pure water to soak, and air-blowing makes inorganic silicon fully contact with water, temperature is 20-90 DEG C;
Acid soak: water is 10 containing the quality of acid than concentration
-8%-0.001%;
High-temperature activation: be 50-200 DEG C of high-temperature activation in temperature, the humidity 0.1%-99% of environment in heating loss process;
(5) strengthen: repeat step (4) A, (4) B, strengthen index and Data Control precision in preparation link, make inorganic silicon nano adsorber specific area be 200 ㎡/g-2000 ㎡/g, average pore size is 0.5nm-20nm, and total pore volume is 0.1ml/g-10ml/g.
4. the preparation method of inorganic silicon nano adsorber according to claim 3, is characterized in that, step (1) mesosilicic acid sodium modulus is 3.25-3.45.
5. the preparation method of inorganic silicon nano adsorber according to claim 3, is characterized in that, in step (2), the mass concentration ratio of acid content is 10
-5%-10
-8.5%.
6. the preparation method of inorganic silicon nano adsorber according to claim 3, is characterized in that, in described step (4), the quality of exchanged acid is 0.8%-6% than concentration, and acid bubble temperature is 40-50 DEG C, sour bubble time 2-8h.
7. the preparation method of inorganic silicon nano adsorber according to claim 3, is characterized in that, in described step (4), exchanged acid is one or more in hydrochloric acid, sulfuric acid, nitric acid, oxalic acid or citric acid, and the quality of acid is 0.02%-6% than concentration.
8. the preparation method of inorganic silicon nano adsorber according to claim 3, is characterized in that, in described step (4) A, the temperature of a reaming is 40-60 DEG C.
9. the preparation method of inorganic silicon nano adsorber according to claim 3, is characterized in that, in described step (4) C, the quality of acid is 10 than concentration
-7%-10
-5%.
10. the preparation method of inorganic silicon nano adsorber according to claim 3, is characterized in that, in described step (4) D, bake out temperature is 70-140 DEG C, and humidity is 0.5%-80%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105664664A (en) * | 2016-04-08 | 2016-06-15 | 安徽宝昱电子科技有限公司 | Toxic gas adsorbing device for sewer |
| CN110918048A (en) * | 2019-12-19 | 2020-03-27 | 乳山市大洋硅胶厂 | Preparation method of hydrogen-absorbing pressure swing adsorption silica gel |
| CN111252772A (en) * | 2018-11-30 | 2020-06-09 | 中国科学院大连化学物理研究所 | Method for adjusting aperture of silicon dioxide |
| CN114315519A (en) * | 2020-09-27 | 2022-04-12 | 太仓沪试试剂有限公司 | Method for purifying high-purity organic solvent methanol |
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| CN1899961A (en) * | 2005-07-22 | 2007-01-24 | 周玉芳 | High dispersion gel-free white carbon black and its preparing method |
| CN104525099A (en) * | 2014-12-19 | 2015-04-22 | 青岛美高集团有限公司 | Silica gel having high adsorbability as well as preparation method and use of silica gel |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1899961A (en) * | 2005-07-22 | 2007-01-24 | 周玉芳 | High dispersion gel-free white carbon black and its preparing method |
| CN104525099A (en) * | 2014-12-19 | 2015-04-22 | 青岛美高集团有限公司 | Silica gel having high adsorbability as well as preparation method and use of silica gel |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105664664A (en) * | 2016-04-08 | 2016-06-15 | 安徽宝昱电子科技有限公司 | Toxic gas adsorbing device for sewer |
| CN111252772A (en) * | 2018-11-30 | 2020-06-09 | 中国科学院大连化学物理研究所 | Method for adjusting aperture of silicon dioxide |
| CN111252772B (en) * | 2018-11-30 | 2022-03-22 | 中国科学院大连化学物理研究所 | Method for adjusting aperture of silicon dioxide |
| CN110918048A (en) * | 2019-12-19 | 2020-03-27 | 乳山市大洋硅胶厂 | Preparation method of hydrogen-absorbing pressure swing adsorption silica gel |
| CN114315519A (en) * | 2020-09-27 | 2022-04-12 | 太仓沪试试剂有限公司 | Method for purifying high-purity organic solvent methanol |
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