CN105396550A - Preparation method of gasoline discoloring agent namely nano SiO2 loaded attapulgite - Google Patents
Preparation method of gasoline discoloring agent namely nano SiO2 loaded attapulgite Download PDFInfo
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- CN105396550A CN105396550A CN201510987586.XA CN201510987586A CN105396550A CN 105396550 A CN105396550 A CN 105396550A CN 201510987586 A CN201510987586 A CN 201510987586A CN 105396550 A CN105396550 A CN 105396550A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G25/00—Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents
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- Oil, Petroleum & Natural Gas (AREA)
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- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention discloses a preparation method of a gasoline discoloring agent namely nano SiO2 loaded attapulgite, and belongs to the field of discoloring agents. The preparation method comprises the following steps: pre-processing attapulgite, then synthesizing nano silica, mixing attapulgite powder and nano silica, adding a surfactant to carry out surface modification, after modification, carrying out acidification, washing, and grinding, and finally burning the mixture in a muffle furnace at different temperatures so as to obtain the gasoline discoloring agent. Nano SiO2 is firmly loaded on the surface of attapulgite, the dispersibility of nano SiO2 is improved, and the specific surface area and surface chemical activity are both increased, so the discoloring performance is prominently improved. The produced discoloring agent has a good discoloring effect, the discoloring rate can reach 97.9 to 99.2%, moreover, the technology is simple, and the cost is low.
Description
Technical field
The invention discloses a kind of loaded with nano SiO
2the preparation method of attapulgite gasoline decolorizer, belongs to decolorizer field.
Background technology
During gasoline products is formed at home, catalytic cracking (FCC) gasoline accounts for about 70%.Be after the FCC gasoline of raw material stores several days with heavy oil, its colour changed into yellow, deepen, even on bottle wall, deposit one deck glued membrane.FCC gasoline belongs to drippolene, therefore can containing a large amount of unsaturated hydrocarbons, particularly alkadienes.When storing and use, due to the existence of sulfide, under the aerial oxygen effect of these unsaturated hydrocarbons, easily oxidation forms colloid substance, and blocking gasoline piping, carburetor jet and intake valve, interrupt fuel feeding and force engine stop work; And these colloidal substances have very strong colorability, only the colloid of 0.002% mass fraction just can make colourless gasoline become olive drab(O.D), therefore decolours to gasoline very necessary.
Attapulgite (Attapulgite) has another name called Palygorskite, bleaching earth, recessed soil.Due to the crystal habit of attapulgite, crystal habit, the many factors such as depositional mode and internal gutter and give its very high specific area, the surface charge energy imbalance that the attapulgite intrinsic atomic structure in surface and activation process produce defines adsorption site, the combination of the two makes attapulgite have good absorption property, has decolouring, water suction, deodorizing, catalysis, ion-exchange, dispersion, the effect such as thermally-stabilised.
Summary of the invention
The technical problem that the present invention mainly solves: after storing several days for the current heavy oil catalytically cracked gasoline that is raw material, its colour changed into yellow, deepen, even on bottle wall, deposit one deck glued membrane, these colloidal substances have the problem of very strong colorability, provide the preparation method of a kind of copper-carbon back transparent conductive film, the present invention first carries out pretreatment to attapulgite, synthesis of nano silica again, surface modification is carried out by adding surfactant after attapulgite powder and nano silicon mixing, modified acidifying again, washing, pulverize, finally put into Muffle furnace roasting at different temperatures, , the present invention adopts attapulgite to make Nano-meter SiO_2
2load is on its surface securely, thus improves its dispersiveness, increases its specific area and chemical mobility of the surface, and then significantly improving its decoloration performance, obtained decolorizer has good decolorizing effect, and percent of decolourization can reach 97.9 ~ 99.2%, and technique is simple, cost is low.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:
(1) 300 ~ 500g attapulgite is got, added pulverizing in pulverizer, sieved to obtain 150 ~ 170 order powder, in powder, deionized water is added by solid-to-liquid ratio 1:4, carry out ultrasonic disperse 10 ~ 15min after being uniformly mixed, form uniform attapulgite suspension, mass fraction 20% glycine solution is added drop-wise in suspension, until adjust ph is 5.5 ~ 6.0, filter after still aging 2 ~ 3h, by filter residue deionized water cyclic washing 1 ~ 3 time, put into 50 ~ 60 DEG C of constant temperature ovens completely dry;
(2) 100 ~ 120g ethyl orthosilicate is got in the there-necked flask of 500mL, in bottle, the ethanolic solution of mass fraction 95% is added by solid-to-liquid ratio 1:1.3, put it in water-bath and stir simultaneously, raise bath temperature to 55 ~ 65 DEG C, the ammoniacal liquor slowly dripping mass fraction 15% after stirring 10 ~ 20min regulates mixed liquor pH value to be 9.0 ~ 9.5, stirring reaction 1 ~ 2h is continued after regulating, room temperature is cooled to after reaction terminates, filter, the solid obtained is used distilled water respectively, washes of absolute alcohol 1 ~ 3 time, centrifugation is carried out after cleaning, obtain sediment, the baking oven putting into 75 ~ 90 DEG C is completely dry,
(3) 50 ~ 70g step (1) pretreated attapulgite powder and 20 ~ 25g step (2) dried nano grade silica particles is got respectively, add the deionized water of 300mL wherein, carry out ultrasonic disperse 15 ~ 20min, gross mass 3 ~ 5% polyvinylpyrrolidone and gross mass 3 ~ 5% lauryl sodium sulfate is added in suspension after dispersion, ultrasonic cell disruptor dispersion 5 ~ 8min is put into after being uniformly mixed 10 ~ 15min, after having disperseed, mixture proceeds in colorimetric cylinder respectively, vertically be placed on rack for test tube, it is allowed to carry out natural subsidence 5 ~ 6h, filter, collect filter residue,
(4) the above-mentioned filter residue that obtains is put into beaker, adding concentration wherein by solid-to-liquid ratio 1:3 is 12mol/L hydrochloric acid solution, after being uniformly mixed 10 ~ 15min, put into the water-bath acidifying 2 ~ 3h of 50 ~ 55 DEG C, filter after acidifying, by filter residue distilled water flushing to filtrate pH value 6.5 ~ 7.0, then filter residue is put into constant temperature oven and at 100 ~ 110 DEG C, carry out drying completely, solid after drying is pulverized and sieved to obtain 170 ~ 180 order powder, powder is loaded in crucible, move into elder generation roasting 20 ~ 25min at 200 ~ 250 DEG C in Muffle furnace again, roasting 15 ~ 20min is carried out at being warming up to 500 ~ 550 DEG C again, take out after being cooled to room temperature, .
Application process of the present invention: the catalytically cracked gasoline getting 100 ~ 200mL loads in the funnel of 250mL, the decolorizer finished product that 8 ~ 15g the present invention prepares in adsorption column, carry out normal temperature and pressure to catalytically cracked gasoline and carry out decolouring 20 ~ 30min, it is 97.9 ~ 99.2% that the absorbance of the rear visible spectrophotometer diesel oil after 528nm place measures decolouring that decolours calculates percent of decolourization.
The invention has the beneficial effects as follows:
(1) the present invention adopts attapulgite to make Nano-meter SiO_2
2load is on its surface securely, thus improves its dispersiveness, increases its specific area and chemical mobility of the surface, and then significantly improves its decoloration performance;
(2) decolorizer that the present invention obtains has good decolorizing effect and technique is simple, and cost is low.
Detailed description of the invention
First 300 ~ 500g attapulgite is got, added pulverizing in pulverizer, sieved to obtain 150 ~ 170 order powder, in powder, deionized water is added by solid-to-liquid ratio 1:4, carry out ultrasonic disperse 10 ~ 15min after being uniformly mixed, form uniform attapulgite suspension, mass fraction 20% glycine solution is added drop-wise in suspension, until adjust ph is 5.5 ~ 6.0, filter after still aging 2 ~ 3h, by filter residue deionized water cyclic washing 1 ~ 3 time, put into 50 ~ 60 DEG C of constant temperature ovens completely dry, get 100 ~ 120g ethyl orthosilicate in the there-necked flask of 500mL, in bottle, the ethanolic solution of mass fraction 95% is added by solid-to-liquid ratio 1:1.3, put it in water-bath and stir simultaneously, raise bath temperature to 55 ~ 65 DEG C, the ammoniacal liquor slowly dripping mass fraction 15% after stirring 10 ~ 20min regulates mixed liquor pH value to be 9.0 ~ 9.5, stirring reaction 1 ~ 2h is continued after regulating, room temperature is cooled to after reaction terminates, filter, the solid obtained is used distilled water respectively, washes of absolute alcohol 1 ~ 3 time, centrifugation is carried out after cleaning, obtain sediment, the baking oven putting into 75 ~ 90 DEG C is completely dry, get 50 ~ 70g pretreated attapulgite powder and the dried nano grade silica particles of 20 ~ 25g respectively, add the deionized water of 300mL wherein, carry out ultrasonic disperse 15 ~ 20min, gross mass 3 ~ 5% polyvinylpyrrolidone and gross mass 3 ~ 5% lauryl sodium sulfate is added in suspension after dispersion, ultrasonic cell disruptor dispersion 5 ~ 8min is put into after being uniformly mixed 10 ~ 15min, after having disperseed, mixture proceeds in colorimetric cylinder respectively, vertically be placed on rack for test tube, it is allowed to carry out natural subsidence 5 ~ 6h, filter, collect filter residue, filter residue will be obtained and put into beaker, adding concentration wherein by solid-to-liquid ratio 1:3 is 12mol/L hydrochloric acid solution, after being uniformly mixed 10 ~ 15min, put into the water-bath acidifying 2 ~ 3h of 50 ~ 55 DEG C, filter after acidifying, by filter residue distilled water flushing to filtrate pH value 6.5 ~ 7.0, then filter residue is put into constant temperature oven and at 100 ~ 110 DEG C, carry out drying completely, solid after drying is pulverized and sieved to obtain 170 ~ 180 order powder, powder is loaded in crucible, move into elder generation roasting 20 ~ 25min at 200 ~ 250 DEG C in Muffle furnace again, roasting 15 ~ 20min is carried out at being warming up to 500 ~ 550 DEG C again, take out after being cooled to room temperature, .
Example 1
First 300g attapulgite is got, added pulverizing in pulverizer, sieved to obtain 150 order powder, in powder, deionized water is added by solid-to-liquid ratio 1:4, carry out ultrasonic disperse 10min after being uniformly mixed, form uniform attapulgite suspension, mass fraction 20% glycine solution is added drop-wise in suspension, until adjust ph is 5.5, filter after still aging 2h, by filter residue deionized water cyclic washing 1 time, put into 50 DEG C of constant temperature ovens completely dry; Get 100g ethyl orthosilicate in the there-necked flask of 500mL, in bottle, the ethanolic solution of mass fraction 95% is added by solid-to-liquid ratio 1:1.3, put it in water-bath and stir simultaneously, raise bath temperature to 55 DEG C, the ammoniacal liquor slowly dripping mass fraction 15% after stirring 10min regulates mixed liquor pH value to be 9.0, stirring reaction 1h is continued after regulating, room temperature is cooled to after reaction terminates, filter, the solid obtained is used respectively distilled water, washes of absolute alcohol 1 time, carry out centrifugation after cleaning, obtain sediment, the baking oven putting into 75 DEG C is completely dry; Get 50g pretreated attapulgite powder and the dried nano grade silica particles of 20g respectively, add the deionized water of 300mL wherein, carry out ultrasonic disperse 15min, gross mass 3% polyvinylpyrrolidone and gross mass 3% lauryl sodium sulfate is added in suspension after dispersion, put into ultrasonic cell disruptor after being uniformly mixed 10min and disperse 5min, after having disperseed, mixture proceeds in colorimetric cylinder respectively, vertically be placed on rack for test tube, it is allowed to carry out natural subsidence 5h, filter, collect filter residue; Filter residue will be obtained and put into beaker, adding concentration wherein by solid-to-liquid ratio 1:3 is 12mol/L hydrochloric acid solution, after being uniformly mixed 10min, put into the water-bath acidifying 2h of 50 DEG C, filter after acidifying, by filter residue distilled water flushing to filtrate pH value 6.5, then filter residue is put into constant temperature oven and at 100 DEG C, carry out drying completely, solid after drying is pulverized and sieved to obtain 170 order powder, powder is loaded in crucible, then moves into elder generation roasting 20min at 200 DEG C in Muffle furnace, then carry out roasting 15min at being warming up to 500 DEG C, take out after being cooled to room temperature.
The catalytically cracked gasoline getting 100mL loads in the funnel of 250mL, the decolorizer finished product that 8g the present invention prepares in adsorption column, carry out normal temperature and pressure to catalytically cracked gasoline and carry out decolouring 20min, it is 97.9% that the absorbance of the rear visible spectrophotometer diesel oil after 528nm place measures decolouring that decolours calculates percent of decolourization.
Example 2
First 400g attapulgite is got, added pulverizing in pulverizer, sieved to obtain 160 order powder, in powder, deionized water is added by solid-to-liquid ratio 1:4, carry out ultrasonic disperse 13min after being uniformly mixed, form uniform attapulgite suspension, mass fraction 20% glycine solution is added drop-wise in suspension, until adjust ph is 5.8, filter after still aging 2.5h, by filter residue deionized water cyclic washing 2 times, put into 55 DEG C of constant temperature ovens completely dry; Get 110g ethyl orthosilicate in the there-necked flask of 500mL, in bottle, the ethanolic solution of mass fraction 95% is added by solid-to-liquid ratio 1:1.3, put it in water-bath and stir simultaneously, raise bath temperature to 60 DEG C, the ammoniacal liquor slowly dripping mass fraction 15% after stirring 15min regulates mixed liquor pH value to be 9.3, stirring reaction 1.5h is continued after regulating, room temperature is cooled to after reaction terminates, filter, the solid obtained is used respectively distilled water, washes of absolute alcohol 2 times, carry out centrifugation after cleaning, obtain sediment, the baking oven putting into 85 DEG C is completely dry; Get 60g pretreated attapulgite powder and the dried nano grade silica particles of 23g respectively, add the deionized water of 300mL wherein, carry out ultrasonic disperse 17min, gross mass 4% polyvinylpyrrolidone and gross mass 4% lauryl sodium sulfate is added in suspension after dispersion, put into ultrasonic cell disruptor after being uniformly mixed 13min and disperse 6min, after having disperseed, mixture proceeds in colorimetric cylinder respectively, vertically be placed on rack for test tube, it is allowed to carry out natural subsidence 5.5h, filter, collect filter residue; Filter residue will be obtained and put into beaker, adding concentration wherein by solid-to-liquid ratio 1:3 is 12mol/L hydrochloric acid solution, after being uniformly mixed 13min, put into the water-bath acidifying 2.5h of 53 DEG C, filter after acidifying, by filter residue distilled water flushing to filtrate pH value 6.8, then filter residue is put into constant temperature oven and at 105 DEG C, carry out drying completely, solid after drying is pulverized and sieved to obtain 175 order powder, powder is loaded in crucible, then moves into elder generation roasting 23min at 225 DEG C in Muffle furnace, then carry out roasting 17min at being warming up to 525 DEG C, take out after being cooled to room temperature.
The catalytically cracked gasoline getting 150mL loads in the funnel of 200mL, the decolorizer finished product that 12g the present invention prepares in adsorption column, carry out normal temperature and pressure to catalytically cracked gasoline and carry out decolouring 25min, it is 98.5% that the absorbance of the rear visible spectrophotometer diesel oil after 528nm place measures decolouring that decolours calculates percent of decolourization.
Example 3
First 500g attapulgite is got, added pulverizing in pulverizer, sieved to obtain 170 order powder, in powder, deionized water is added by solid-to-liquid ratio 1:4, carry out ultrasonic disperse 15min after being uniformly mixed, form uniform attapulgite suspension, mass fraction 20% glycine solution is added drop-wise in suspension, until adjust ph is 6.0, filter after still aging 3h, by filter residue deionized water cyclic washing 3 times, put into 60 DEG C of constant temperature ovens completely dry; Get 120g ethyl orthosilicate in the there-necked flask of 500mL, in bottle, the ethanolic solution of mass fraction 95% is added by solid-to-liquid ratio 1:1.3, put it in water-bath and stir simultaneously, raise bath temperature to 65 DEG C, the ammoniacal liquor slowly dripping mass fraction 15% after stirring 20min regulates mixed liquor pH value to be 9.5, stirring reaction 2h is continued after regulating, room temperature is cooled to after reaction terminates, filter, the solid obtained is used respectively distilled water, washes of absolute alcohol 3 times, carry out centrifugation after cleaning, obtain sediment, the baking oven putting into 90 DEG C is completely dry; Get 70g pretreated attapulgite powder and the dried nano grade silica particles of 25g respectively, add the deionized water of 300mL wherein, carry out ultrasonic disperse 20min, gross mass 5% polyvinylpyrrolidone and gross mass 5% lauryl sodium sulfate is added in suspension after dispersion, put into ultrasonic cell disruptor after being uniformly mixed 15min and disperse 8min, after having disperseed, mixture proceeds in colorimetric cylinder respectively, vertically be placed on rack for test tube, it is allowed to carry out natural subsidence 6h, filter, collect filter residue; Filter residue will be obtained and put into beaker, adding concentration wherein by solid-to-liquid ratio 1:3 is 12mol/L hydrochloric acid solution, after being uniformly mixed 15min, put into the water-bath acidifying 3h of 55 DEG C, filter after acidifying, by filter residue distilled water flushing to filtrate pH value 7, then filter residue is put into constant temperature oven and at 110 DEG C, carry out drying completely, solid after drying is pulverized and sieved to obtain 180 order powder, powder is loaded in crucible, then moves into elder generation roasting 25min at 250 DEG C in Muffle furnace, then carry out roasting 20min at being warming up to 550 DEG C, take out after being cooled to room temperature.
The catalytically cracked gasoline getting 200mL loads in the funnel of 250mL, the decolorizer finished product that 15g the present invention prepares in adsorption column, carry out normal temperature and pressure to catalytically cracked gasoline and carry out decolouring 30min, it is 99.2% that the absorbance of the rear visible spectrophotometer diesel oil after 528nm place measures decolouring that decolours calculates percent of decolourization.
Claims (1)
1. a loaded with nano SiO
2the preparation method of attapulgite gasoline decolorizer, is characterized in that concrete preparation process:
(1) 300 ~ 500g attapulgite is got, added pulverizing in pulverizer, sieved to obtain 150 ~ 170 order powder, in powder, deionized water is added by solid-to-liquid ratio 1:4, carry out ultrasonic disperse 10 ~ 15min after being uniformly mixed, form uniform attapulgite suspension, mass fraction 20% glycine solution is added drop-wise in suspension, until adjust ph is 5.5 ~ 6.0, filter after still aging 2 ~ 3h, by filter residue deionized water cyclic washing 1 ~ 3 time, put into 50 ~ 60 DEG C of constant temperature ovens completely dry;
(2) 100 ~ 120g ethyl orthosilicate is got in the there-necked flask of 500mL, in bottle, the ethanolic solution of mass fraction 95% is added by solid-to-liquid ratio 1:1.3, put it in water-bath and stir simultaneously, raise bath temperature to 55 ~ 65 DEG C, the ammoniacal liquor slowly dripping mass fraction 15% after stirring 10 ~ 20min regulates mixed liquor pH value to be 9.0 ~ 9.5, stirring reaction 1 ~ 2h is continued after regulating, room temperature is cooled to after reaction terminates, filter, the solid obtained is used distilled water respectively, washes of absolute alcohol 1 ~ 3 time, centrifugation is carried out after cleaning, obtain sediment, the baking oven putting into 75 ~ 90 DEG C is completely dry,
(3) 50 ~ 70g step (1) pretreated attapulgite powder and 20 ~ 25g step (2) dried nano grade silica particles is got respectively, add the deionized water of 300mL wherein, carry out ultrasonic disperse 15 ~ 20min, gross mass 3 ~ 5% polyvinylpyrrolidone and gross mass 3 ~ 5% lauryl sodium sulfate is added in suspension after dispersion, ultrasonic cell disruptor dispersion 5 ~ 8min is put into after being uniformly mixed 10 ~ 15min, after having disperseed, mixture proceeds in colorimetric cylinder respectively, vertically be placed on rack for test tube, it is allowed to carry out natural subsidence 5 ~ 6h, filter, collect filter residue,
(4) the above-mentioned filter residue that obtains is put into beaker, adding concentration wherein by solid-to-liquid ratio 1:3 is 12mol/L hydrochloric acid solution, after being uniformly mixed 10 ~ 15min, put into the water-bath acidifying 2 ~ 3h of 50 ~ 55 DEG C, filter after acidifying, by filter residue distilled water flushing to filtrate pH value 6.5 ~ 7, then filter residue is put into constant temperature oven and at 100 ~ 110 DEG C, carry out drying completely, solid after drying is pulverized and sieved to obtain 170 ~ 180 order powder, powder is loaded in crucible, move into elder generation roasting 20 ~ 25min at 200 ~ 250 DEG C in Muffle furnace again, roasting 15 ~ 20min is carried out at being warming up to 500 ~ 550 DEG C again, take out after being cooled to room temperature, .
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106242090A (en) * | 2016-09-08 | 2016-12-21 | 合肥智慧殿投资管理有限公司 | A kind of phosphate-free corrosion inhibition antisludging agent and its preparation method and application |
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CN109126732A (en) * | 2018-09-12 | 2019-01-04 | 苏州涵轩信息科技有限公司 | The recessed loaded mesoporous silica of soil-sodium alginate adsorbent material and preparation method thereof |
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CN106242090A (en) * | 2016-09-08 | 2016-12-21 | 合肥智慧殿投资管理有限公司 | A kind of phosphate-free corrosion inhibition antisludging agent and its preparation method and application |
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CN109126732A (en) * | 2018-09-12 | 2019-01-04 | 苏州涵轩信息科技有限公司 | The recessed loaded mesoporous silica of soil-sodium alginate adsorbent material and preparation method thereof |
CN116631675A (en) * | 2023-06-15 | 2023-08-22 | 安徽远征电缆科技有限公司 | Mobile abrasion-resistant and drag-resistant shielded cable with large cross section and flame resistance |
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