CN106590727A - Alkaline ceramic grease deacidification agent preparation method - Google Patents
Alkaline ceramic grease deacidification agent preparation method Download PDFInfo
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- CN106590727A CN106590727A CN201611135265.8A CN201611135265A CN106590727A CN 106590727 A CN106590727 A CN 106590727A CN 201611135265 A CN201611135265 A CN 201611135265A CN 106590727 A CN106590727 A CN 106590727A
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- diatomite
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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
- C10G19/00—Refining hydrocarbon oils in the absence of hydrogen, by alkaline treatment
- C10G19/073—Refining hydrocarbon oils in the absence of hydrogen, by alkaline treatment with solid alkaline material
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- Oil, Petroleum & Natural Gas (AREA)
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Abstract
The invention relates to an alkaline ceramic grease deacidification agent preparation method and belongs to the technical field of grease deacidification agents. The preparation method includes taking diatomite as aggregate, coating the polyurethane surface with diatomite slurry, and roasting to form so as to obtain diatomite ceramics; modifying through a three-dimensional netted structure, and enabling nanometer silicon particles to grow on the surface of the three-dimensional netted structure evenly so as to obtain diatomite-based porous ceramics of a multi-stage porous structure; using the diatomite-based porous ceramics as a supporter to support alkaline liquor so as to obtain an alkaline ceramic grease deacidification agent. The alkaline ceramic grease deacidification agent is easy to recover and free of environmental pollution, is capable of increasing the effective contact area between alkali and free fatty acids by taking the advantages of intrinsic porosity, large specific surface area and high adsorption capacity, and enables a reaction rate to be increased under the combined action of physical adsorption and chemical adsorption, so that the free fatty acids are removed effectively.
Description
Technical field
The present invention relates to a kind of preparation method of alkaline ceramic lipin deacidifying agent, belongs to lipin deacidifying agent technical field.
Background technology
Depickling is the important step of oil and fat refining, and current acid stripping method has molecular clock depickling, alkali-refining deacidification, physical refining
Depickling, organic solvent extraction depickling and supercritical fluid extraction depickling etc., current most of grease factories adopt alkali-refining deacidification, i.e.,
The free fatty in oil is neutralized using alkali lye, the soap of generation is soluble in water and be insoluble in oil, most dissociate at last fat
Fat acid is removed, so as to reach the purpose of depickling.The method deacidification effect is good, but subsequently need to repeatedly wash and remove soap,
Then vacuum removal moisture, the shortcomings of there is complex process, high energy consumption, pollution environment；The shortcoming of molecularly distilled is pretreatment
Have high demands and high equipment cost；The shortcoming of physical refining deacidification is not to be suitable for thermal sensitivity grease；The shortcoming of extraction is cost
Comparison is high.
Adsorption deacidification refers to utilize that there is adsorbing solid material to remove the free-fat in deoiling to free fatty
Acid, the method low cost, it is easy to operate, without waste water, do not affect environment.Effective adsorption deacidification is used in being critical that for adsorption deacidification
Agent.Mainly there are rice husk and atlapulgite etc. currently used for the material for preparing adsorption deacidification agent, the shortcoming of these materials is not eat
Product additive limits its application in edible oil using in standard.Therefore, for the research of lipin deacidifying agent seems particularly heavy
Will.
The content of the invention
The technical problem to be solved：For traditional acid stripping method high energy consumption, complex process, asking for environment is polluted
Topic, the invention provides a kind of preparation method of alkaline ceramic lipin deacidifying agent, of the invention with diatomite as aggregate, by poly-
The hanging of urethane surface, then Jing calcining shapings, are obtained diatomite ceramics, recycle its tridimensional network to be retrofited, in its table
Face homoepitaxial goes out silicon nanoparticle, is prepared for the Diatomite-based Porous Ceramics with multi-stage artery structure, finally as
Carrier loaded alkali lye, is obtained alkaline ceramic lipin deacidifying agent.Alkaline ceramic lipin deacidifying agent prepared by the present invention is more using itself
The advantages of hole, big specific surface area, high adsorption capacity, the effective contact area of alkali and free fatty is improve, inhaled by physics
Echo the comprehensive function of chemisorbed so that reaction rate is improved, effectively remove free fatty, and easily reclaim, do not pollute ring
Border.
To solve above-mentioned technical problem, the technical solution used in the present invention is：
（1）The flexible polyurethane foams of one piece of 1cm × 1cm × 1cm of clip, are immersed in 100～150mL mass fractions for 10% hydrogen
In sodium hydroxide solution, 2～3h is soaked under 60～65 DEG C of waters bath with thermostatic control, take out flexible polyurethane foams, and be washed with deionized water
After washing 2～3 times, then it is in 1% carboxymethylcellulose sodium solution, under 60～65 DEG C of waters bath with thermostatic control to be immersed in mass fraction
1～2h of immersion, subsequently takes out flexible polyurethane foams, and natural air drying obtains surface preparation flexible polyurethane foams, standby；
（2）Weigh 1.2～1.5g sodium chloride, 2～5g sodium metasilicate, in adding 60～65mL deionized waters, with 300～400r/min
10～15min of stirring, adds 25～30g diatomite, and 7～8mL mass fractions are 10% O-phthalic acid diethylene glycol dipropyl alkene
Acid esters solution, with 800～1000r/min 10～12h is stirred, and obtains diatomite slurry；
（3）By step（1）The surface preparation flexible polyurethane foams of preparation are immersed in above-mentioned diatomite slurry after 3～5min,
Take out polyurethane foam and remove additional size with roll squeezer pressure, then be placed on woven wire filter plate, starched with above-mentioned diatomite
Material carries out drenching slurry process to foams, and goes additional size, repetition above-mentioned pouring slurry operation 3～4 times to then continue at roll squeezer pressure
In drying box, 1～2h is dried at 70～80 DEG C, then is placed in Muffle furnace, be heated to 600～800 DEG C, keeping temperature
3～5h of calcining, naturally cools to room temperature, obtains diatomite ceramics；
（4）10～12mL tetraethyl orthosilicates are measured, 25～30mL mass fractions are instilled as 20% tetrapropyl hydrogen-oxygen with 1～3mL/min
In changing aqueous ammonium, 10～12h is stirred with 300～400r/min, above-mentioned diatomite ceramics are added, in 90～95 DEG C of thermostatted waters
Bath 60～70h of lower reaction, subsequently filters, and after being washed with deionized filter residue 3～5 times, filter residue is placed in drying box, 70～
1～2h is dried at 80 DEG C, then is placed in Muffle furnace, be heated to 550～600 DEG C, keeping temperature calcines 3～5h, naturally cold
But to room temperature, multi-stage artery structure Diatomite-based Porous Ceramics are obtained；
（5）The above-mentioned multi-stage artery structure Diatomite-based Porous Ceramics of 10～20g are weighed, adds 50～100mL mass fractions to be 25%
In sodium hydroxide solution, 60～70 DEG C are heated to, and 40～50min, subsequent suction filtration, by filter cake are stirred with 300～500r/min
In being placed in drying box, it is dried to constant weight at 105～110 DEG C, obtains alkaline ceramic lipin deacidifying agent.
The present invention application process be：It is 1～2% by addition, alkaline ceramic prepared by the present invention is added in rapeseed oil
Lipin deacidifying agent, 25～30min of depickling at 50～60 DEG C, acid number is down to 0.85～0.92mg/g in rapeseed oil, reaches squeezing
One-level oil standard.
The method have the benefit that：
（1）Alkaline ceramic lipin deacidifying agent prepared by the present invention, deacidification effect is good, and process time is short, and process is simple；
（2）Prepared by alkaline ceramic lipin deacidifying agent prepared by the present invention convenient, and the recyclable reuse of carrier is free from environmental pollution.
Specific embodiment
The flexible polyurethane foams of one piece of 1cm × 1cm × 1cm of clip, are immersed in 100～150mL mass fractions for 10% hydrogen
In sodium hydroxide solution, 2～3h is soaked under 60～65 DEG C of waters bath with thermostatic control, take out flexible polyurethane foams, and be washed with deionized water
After washing 2～3 times, then it is in 1% carboxymethylcellulose sodium solution, under 60～65 DEG C of waters bath with thermostatic control to be immersed in mass fraction
1～2h of immersion, subsequently takes out flexible polyurethane foams, and natural air drying obtains surface preparation flexible polyurethane foams；Weigh 1.2
～1.5g sodium chloride, 2～5g sodium metasilicate in adding 60～65mL deionized waters, with 300～400r/min 10～15min is stirred,
25～30g diatomite is added, 7～8mL mass fractions are 10% PDDA solution, with 800
～1000r/min stirs 10～12h, obtains diatomite slurry；Above-mentioned surface preparation flexible polyurethane foams are immersed into above-mentioned silicon
In diatomaceous earth slurry after 3～5min, take out polyurethane foam and remove additional size with roll squeezer pressure, then be placed on woven wire filter
On plate, foams are carried out with above-mentioned diatomite slurry drench slurry process, and additional size, the above-mentioned pouring slurry of repetition are removed with roll squeezer pressure
Operation 3～4 times, in then continuing at drying box, is dried 1～2h at 70～80 DEG C, then is placed in Muffle furnace, is heated to
600～800 DEG C, keeping temperature calcines 3～5h, naturally cools to room temperature, obtains diatomite ceramics；Measure the positive silicic acid of 10～12mL
Ethyl ester, in instilling 25～30mL mass fractions as the 20% TPAOH aqueous solution with 1～3mL/min, with 300～400r/
Min stirs 10～12h, adds above-mentioned diatomite ceramics, and 60～70h is reacted under 90～95 DEG C of waters bath with thermostatic control, subsequently filters,
After being washed with deionized filter residue 3～5 times, filter residue is placed in drying box, 1～2h is dried at 70～80 DEG C, then put
In Muffle furnace, 550～600 DEG C are heated to, keeping temperature calcines 3～5h, naturally cools to room temperature, obtains multi-stage artery structure silicon
Diatomaceous earth base porous ceramics；The above-mentioned multi-stage artery structure Diatomite-based Porous Ceramics of 10～20g are weighed, 50～100mL mass is added
Fraction is in 25% sodium hydroxide solution, to be heated to 60～70 DEG C, and stirs 40～50min with 300～500r/min, is subsequently taken out
Filter, filter cake is placed in drying box, is dried to constant weight at 105～110 DEG C, obtains alkaline ceramic lipin deacidifying agent.
Example 1
The flexible polyurethane foams of one piece of 1cm × 1cm × 1cm of clip, it is that 10% NaOH is molten to be immersed in 100mL mass fractions
In liquid, 2h is soaked under 60 DEG C of waters bath with thermostatic control, take out flexible polyurethane foams, and after being washed with deionized 2 times, then soaked
Bubble soaks 1h in mass fraction is 1% carboxymethylcellulose sodium solution under 60 DEG C of waters bath with thermostatic control, subsequently takes out soft poly- ammonia
Ester foam, natural air drying obtains surface preparation flexible polyurethane foams；1.2g sodium chloride is weighed, 2g sodium metasilicate adds 60mL to go
In ionized water, 10min is stirred with 300r/min, add 25g diatomite, 7mL mass fractions are 10% phthalic acid diethyl two
Alcohol diacrylate ester solution, with 800r/min 10h is stirred, and obtains diatomite slurry；By above-mentioned surface preparation flexibel polyurethane bubble
Foam is immersed in above-mentioned diatomite slurry after 3min, is taken out polyurethane foam and is removed additional size with roll squeezer pressure, then is placed on
On woven wire filter plate, foams are carried out with above-mentioned diatomite slurry drench slurry process, and additional size is removed with roll squeezer pressure, weight
Multiple above-mentioned pouring slurry operation 3 times, in then continuing at drying box, is dried 1h at 70 DEG C, then is placed in Muffle furnace, is heated to
600 DEG C, keeping temperature calcining 3h naturally cools to room temperature, obtains diatomite ceramics；10mL tetraethyl orthosilicates are measured, with 1mL/
It is in the 20% TPAOH aqueous solution, with 300r/min 10h to be stirred that min instills 25mL mass fractions, adds above-mentioned silicon
Diatomaceous earth ceramics, under 90 DEG C of waters bath with thermostatic control 60h is reacted, and is subsequently filtered, and after being washed with deionized filter residue 3 times, filter residue is placed in
In drying box, 1h is dried at 70 DEG C, then is placed in Muffle furnace, be heated to 550 DEG C, keeping temperature calcining 3h is naturally cold
But to room temperature, multi-stage artery structure Diatomite-based Porous Ceramics are obtained；Weigh the above-mentioned multi-stage artery structure Diatomite-based Porous potteries of 10g
Porcelain, adds 50mL mass fractions to be in 25% sodium hydroxide solution, to be heated to 60 DEG C, and stirs 40min with 300r/min, subsequently
Suction filtration, filter cake is placed in drying box, is dried to constant weight at 105 DEG C, obtains alkaline ceramic lipin deacidifying agent.
The present invention application process be：It is 1% by addition, alkaline ceramic oil prepared by the present invention is added in rapeseed oil
Fat deacidification agent, the depickling 25min at 50 DEG C, acid number is down to 0.85mg/g in rapeseed oil, reaches squeezing one-level oil standard.
Example 2
The flexible polyurethane foams of one piece of 1cm × 1cm × 1cm of clip, it is that 10% NaOH is molten to be immersed in 120mL mass fractions
In liquid, soak 2.5h under 62 DEG C of waters bath with thermostatic control, take out flexible polyurethane foams, and after being washed with deionized 2 times, then by its
Mass fraction is immersed in 1% carboxymethylcellulose sodium solution, 1.5h to be soaked under 62 DEG C of waters bath with thermostatic control, subsequently takes out soft
Polyurethane foam, natural air drying obtains surface preparation flexible polyurethane foams；1.3g sodium chloride is weighed, 3g sodium metasilicate is added
In 62mL deionized waters, 12min is stirred with 350r/min, add 28g diatomite, 7.5mL mass fractions are 10% O-phthalic
Acid diethylene glycol diacrylate ester solution, with 900r/min 11h is stirred, and obtains diatomite slurry；Above-mentioned surface preparation is soft
Polyurethane foam is immersed in above-mentioned diatomite slurry after 4min, is taken out polyurethane foam and is removed additional size with roll squeezer pressure, then
It is placed on woven wire filter plate, foams is carried out with above-mentioned diatomite slurry drench slurry process, and is gone with roll squeezer pressure many
Remaining slurry material, repetition above-mentioned pouring slurry operation 3 times, in then continuing at drying box, is dried 1.5h at 75 DEG C, then is placed on Muffle furnace
In, 700 DEG C are heated to, keeping temperature calcining 4h naturally cools to room temperature, obtains diatomite ceramics；Measure the positive silicic acid second of 11mL
Ester, in instilling 28mL mass fractions as the 20% TPAOH aqueous solution with 2mL/min, with 360r/min 11h is stirred, then
Above-mentioned diatomite ceramics are added, under 92 DEG C of waters bath with thermostatic control 65h is reacted, subsequently filtered, after being washed with deionized filter residue 4 times,
Filter residue is placed in drying box, 1.5h is dried at 75 DEG C, then be placed in Muffle furnace, be heated to 580 DEG C, keeping temperature is forged
4h is burnt, room temperature is naturally cooled to, multi-stage artery structure Diatomite-based Porous Ceramics are obtained；Weigh the above-mentioned multi-stage artery structure silicon of 15g
Diatomaceous earth base porous ceramics, adds 80mL mass fractions to be in 25% sodium hydroxide solution, to be heated to 65 DEG C, and is stirred with 400r/min
45min is mixed, subsequent suction filtration is placed in filter cake in drying box, be dried to constant weight at 108 DEG C, obtain alkaline ceramic lipin deacidifying agent.
The present invention application process be：It is 1.5% by addition, alkaline ceramic prepared by the present invention is added in rapeseed oil
Lipin deacidifying agent, the depickling 28min at 55 DEG C, acid number is down to 0.89mg/g in rapeseed oil, reaches squeezing one-level oil standard.
Example 3
The flexible polyurethane foams of one piece of 1cm × 1cm × 1cm of clip, it is that 10% NaOH is molten to be immersed in 150mL mass fractions
In liquid, 3h is soaked under 65 DEG C of waters bath with thermostatic control, take out flexible polyurethane foams, and after being washed with deionized 3 times, then soaked
Bubble soaks 2h in mass fraction is 1% carboxymethylcellulose sodium solution under 65 DEG C of waters bath with thermostatic control, subsequently takes out soft poly- ammonia
Ester foam, natural air drying obtains surface preparation flexible polyurethane foams；1.5g sodium chloride is weighed, 5g sodium metasilicate adds 65mL to go
In ionized water, 15min is stirred with 400r/min, add 30g diatomite, 8mL mass fractions are 10% phthalic acid diethyl two
Alcohol diacrylate ester solution, with 1000r/min 12h is stirred, and obtains diatomite slurry；By above-mentioned surface preparation flexibel polyurethane bubble
Foam is immersed in above-mentioned diatomite slurry after 5min, is taken out polyurethane foam and is removed additional size with roll squeezer pressure, then is placed on
On woven wire filter plate, foams are carried out with above-mentioned diatomite slurry drench slurry process, and additional size is removed with roll squeezer pressure, weight
Multiple above-mentioned pouring slurry operation 4 times, in then continuing at drying box, is dried 2h at 80 DEG C, then is placed in Muffle furnace, is heated to
800 DEG C, keeping temperature calcining 5h naturally cools to room temperature, obtains diatomite ceramics；12mL tetraethyl orthosilicates are measured, with 3mL/
It is in the 20% TPAOH aqueous solution, with 400r/min 12h to be stirred that min instills 30mL mass fractions, adds above-mentioned silicon
Diatomaceous earth ceramics, under 95 DEG C of waters bath with thermostatic control 70h is reacted, and is subsequently filtered, and after being washed with deionized filter residue 5 times, filter residue is placed in
In drying box, 2h is dried at 80 DEG C, then is placed in Muffle furnace, be heated to 600 DEG C, keeping temperature calcining 5h is naturally cold
But to room temperature, multi-stage artery structure Diatomite-based Porous Ceramics are obtained；Weigh the above-mentioned multi-stage artery structure Diatomite-based Porous potteries of 20g
Porcelain, adds 100mL mass fractions to be in 25% sodium hydroxide solution, to be heated to 70 DEG C, and stirs 50min with 500r/min, subsequently
Suction filtration, filter cake is placed in drying box, is dried to constant weight at 110 DEG C, obtains alkaline ceramic lipin deacidifying agent.
The present invention application process be：It is 2% by addition, alkaline ceramic oil prepared by the present invention is added in rapeseed oil
Fat deacidification agent, the depickling 30min at 60 DEG C, acid number is down to 0.92mg/g in rapeseed oil, reaches squeezing one-level oil standard.
Claims (1)
1. a kind of preparation method of alkaline ceramic lipin deacidifying agent, it is characterised in that concrete preparation process is：
（1）The flexible polyurethane foams of one piece of 1cm × 1cm × 1cm of clip, are immersed in 100～150mL mass fractions for 10% hydrogen
In sodium hydroxide solution, 2～3h is soaked under 60～65 DEG C of waters bath with thermostatic control, take out flexible polyurethane foams, and be washed with deionized water
After washing 2～3 times, then it is in 1% carboxymethylcellulose sodium solution, under 60～65 DEG C of waters bath with thermostatic control to be immersed in mass fraction
1～2h of immersion, subsequently takes out flexible polyurethane foams, and natural air drying obtains surface preparation flexible polyurethane foams, standby；
（2）Weigh 1.2～1.5g sodium chloride, 2～5g sodium metasilicate, in adding 60～65mL deionized waters, with 300～400r/min
10～15min of stirring, adds 25～30g diatomite, and 7～8mL mass fractions are 10% O-phthalic acid diethylene glycol dipropyl alkene
Acid esters solution, with 800～1000r/min 10～12h is stirred, and obtains diatomite slurry；
（3）By step（1）The surface preparation flexible polyurethane foams of preparation are immersed in above-mentioned diatomite slurry after 3～5min,
Take out polyurethane foam and remove additional size with roll squeezer pressure, then be placed on woven wire filter plate, starched with above-mentioned diatomite
Material carries out drenching slurry process to foams, and goes additional size, repetition above-mentioned pouring slurry operation 3～4 times to then continue at roll squeezer pressure
In drying box, 1～2h is dried at 70～80 DEG C, then is placed in Muffle furnace, be heated to 600～800 DEG C, keeping temperature
3～5h of calcining, naturally cools to room temperature, obtains diatomite ceramics；
（4）10～12mL tetraethyl orthosilicates are measured, 25～30mL mass fractions are instilled as 20% tetrapropyl hydrogen-oxygen with 1～3mL/min
In changing aqueous ammonium, 10～12h is stirred with 300～400r/min, above-mentioned diatomite ceramics are added, in 90～95 DEG C of thermostatted waters
Bath 60～70h of lower reaction, subsequently filters, and after being washed with deionized filter residue 3～5 times, filter residue is placed in drying box, 70～
1～2h is dried at 80 DEG C, then is placed in Muffle furnace, be heated to 550～600 DEG C, keeping temperature calcines 3～5h, naturally cold
But to room temperature, multi-stage artery structure Diatomite-based Porous Ceramics are obtained；
（5）The above-mentioned multi-stage artery structure Diatomite-based Porous Ceramics of 10～20g are weighed, adds 50～100mL mass fractions to be 25%
In sodium hydroxide solution, 60～70 DEG C are heated to, and 40～50min, subsequent suction filtration, by filter cake are stirred with 300～500r/min
In being placed in drying box, it is dried to constant weight at 105～110 DEG C, obtains alkaline ceramic lipin deacidifying agent.
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| CN201611135265.8A CN106590727B (en) | 2016-12-11 | 2016-12-11 | A kind of preparation method of alkaline ceramic lipin deacidifying agent |
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| CN201611135265.8A CN106590727B (en) | 2016-12-11 | 2016-12-11 | A kind of preparation method of alkaline ceramic lipin deacidifying agent |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108531270A (en) * | 2018-03-30 | 2018-09-14 | 王敏 | A kind of vegetable insulating oil and preparation method thereof |
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|---|---|---|---|---|
| US3658695A (en) * | 1970-12-14 | 1972-04-25 | Phillips Petroleum Co | Production of low-metal content gas oil from topped crude oil |
| CN1123825A (en) * | 1995-09-05 | 1996-06-05 | 新疆石油管理局克拉玛依炼油厂 | Deacidifying process for petroleum cut fraction with amino-alcohol |
| CN101220294A (en) * | 2007-12-14 | 2008-07-16 | 武汉科技学院 | Lubricating oil basic oil depickling agent and use method thereof |
| CN101311249A (en) * | 2007-05-25 | 2008-11-26 | 北京化工大学 | Method for preparing lubrication deacidification agent |
| CN104492412A (en) * | 2015-01-07 | 2015-04-08 | 李�杰 | Preparation method of petroleum deacidification catalyst |
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2016
- 2016-12-11 CN CN201611135265.8A patent/CN106590727B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3658695A (en) * | 1970-12-14 | 1972-04-25 | Phillips Petroleum Co | Production of low-metal content gas oil from topped crude oil |
| CN1123825A (en) * | 1995-09-05 | 1996-06-05 | 新疆石油管理局克拉玛依炼油厂 | Deacidifying process for petroleum cut fraction with amino-alcohol |
| CN101311249A (en) * | 2007-05-25 | 2008-11-26 | 北京化工大学 | Method for preparing lubrication deacidification agent |
| CN101220294A (en) * | 2007-12-14 | 2008-07-16 | 武汉科技学院 | Lubricating oil basic oil depickling agent and use method thereof |
| CN104492412A (en) * | 2015-01-07 | 2015-04-08 | 李�杰 | Preparation method of petroleum deacidification catalyst |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108531270A (en) * | 2018-03-30 | 2018-09-14 | 王敏 | A kind of vegetable insulating oil and preparation method thereof |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
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| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Wang Zhirong Inventor after: Liu Yaogang Inventor before: Yan Bowen Inventor before: Zhang Xiao |
|
| TA01 | Transfer of patent application right | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20180123 Address after: 226403 Jiangsu city of Nantong province Rudong County Chahe town traffic road No. 33 Applicant after: Golden sun oil Limited by Share Ltd Address before: North Street, Meihua road Jiangsu city Changzhou province 215489 Zhonglou District No. 105 Applicant before: Yan Bowen |
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| GR01 | Patent grant | ||
| GR01 | Patent grant |