CN106590727B - A kind of preparation method of alkaline ceramic lipin deacidifying agent - Google Patents
A kind of preparation method of alkaline ceramic lipin deacidifying agent Download PDFInfo
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- CN106590727B CN106590727B CN201611135265.8A CN201611135265A CN106590727B CN 106590727 B CN106590727 B CN 106590727B CN 201611135265 A CN201611135265 A CN 201611135265A CN 106590727 B CN106590727 B CN 106590727B
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- diatomite
- deacidifying agent
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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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Abstract
The present invention relates to a kind of preparation method of alkaline ceramic lipin deacidifying agent, belong to lipin deacidifying agent technical field.The present invention is using diatomite as aggregate, by in polyurethane surface hanging, it is molded again through calcining, diatomite ceramics are made, recycle its tridimensional network to be retrofited, go out silicon nanoparticle in its surface homoepitaxial, be prepared for the Diatomite-based Porous Ceramics with multi-stage artery structure, finally as carrier loaded alkali lye, alkaline ceramic lipin deacidifying agent is made.The advantages that alkaline ceramic lipin deacidifying agent prepared by the present invention utilizes itself porous, specific surface area is big, adsorption capacity is strong, improve effective contact area of alkali and free fatty, pass through physical absorption and the comprehensive function of chemisorbed, so that reaction rate improves, effectively removing free fatty, and easily recovery, it is free from environmental pollution.
Description
Technical field
The present invention relates to a kind of preparation method of alkaline ceramic lipin deacidifying agent, belong to lipin deacidifying agent technical field.
Background technology
Depickling is the important step of oil and fat refining, and acid stripping method has molecular distillation depickling, alkali-refining deacidification, physical refining at present
Depickling, organic solvent extraction depickling and supercritical fluid extraction depickling etc., current most of grease factories use alkali-refining deacidification, i.e.,
The free fatty in oil is neutralized using alkali lye, the soap of generation is soluble in water and is insoluble in oil, and most dissociate fat at last
Fat acid removes, so as to reach the purpose of depickling.This method deacidification effect is good, but subsequently need to repeatedly wash and remove soap,
Then vacuum removal moisture, the shortcomings of complex process, high energy consumption, pollution environment be present；The shortcomings that molecularly distilled is pretreatment
It is required that high and high equipment cost；The shortcomings that physical refining deacidification is not to be suitable for thermal sensitivity grease；The shortcomings that extraction is cost
Compare high.
Adsorption deacidification refers to remove the free-fat in deoiling using the solid material for having free fatty suction-operated
Acid, the method cost is low, it is easy to operate, without waste water, do not influence environment.Adsorption deacidification is critical that with effective adsorption deacidification
Agent.Material currently used for preparing adsorption deacidification agent mainly has rice husk and atlapulgite etc., is not eat the shortcomings that these materials
Product additive is used in standard, limits its application in edible oil.Therefore, the research for lipin deacidifying agent seems particularly heavy
Will.
The content of the invention
The technical problems to be solved by the invention：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, the present invention is using diatomite as aggregate, by poly-
The hanging of urethane surface, then be molded through calcining, diatomite ceramics are made, recycle its tridimensional network to be modified, 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, alkaline ceramic lipin deacidifying agent is made.Alkaline ceramic lipin deacidifying agent prepared by the present invention is more using itself
Hole, the advantages that specific surface area is big, adsorption capacity is strong, effective contact area of alkali and free fatty is improved, is inhaled by physics
Echo the comprehensive function of chemisorbed so that reaction rate improves, and effectively removes free fatty, and easily recovery, does not pollute ring
Border.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
（1）One piece of 1cm × 1cm × 1cm of clip flexible polyurethane foams, being immersed in 100~150mL mass fractions is
In 10% sodium hydroxide solution, 2~3h is soaked under 60~65 DEG C of waters bath with thermostatic control, takes out flexible polyurethane foams, and use deionization
After water washing 2~3 times, then it is in 1% carboxymethylcellulose sodium solution, in 60~65 DEG C of thermostatted waters to be immersed in mass fraction
Bath 1~2h of lower immersion, then takes out flexible polyurethane foams, natural air drying obtains surface preparation flexible polyurethane foams, standby
With；
（2）Weigh 1.2~1.5g sodium chloride, 2~5g sodium metasilicate, add in 60~65mL deionized waters, with 300~
400r/min stirs 10~15min, adds 25~30g diatomite, 7~8mL mass fractions are 10% phthalic acid diethyl two
Alcohol diacrylate ester solution, 10~12h is stirred with 800~1000r/min, obtains diatomite slurry；
（3）By step（1）The surface preparation flexible polyurethane foams of preparation immerse 3~5min in above-mentioned diatomite slurry
Afterwards, take out polyurethane foam and remove additional size with roll squeezer pressure, then be placed on woven wire filter plate, with above-mentioned diatomite
Slurry carries out drenching slurry processing to foams, and removes additional size with roll squeezer pressure, repeats above-mentioned leaching slurry and operates 3~4 times, then turns
Enter in drying box, 1~2h is dried at 70~80 DEG C, then be placed in Muffle furnace, be heated to 600~800 DEG C, keep temperature
Degree 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 using 1~3mL/min
In ammonium hydroxide aqueous solution, 10~12h is stirred with 300~400r/min, above-mentioned diatomite ceramics are added, in 90~95 DEG C of perseverances
60~70h is reacted under tepidarium, then filtering, after filter residue 3~5 times is washed with deionized, filter residue is placed in drying box,
1~2h to be dried at 70~80 DEG C, then is placed in Muffle furnace, is heated to 550~600 DEG C, keeping temperature calcines 3~5h, from
Room temperature so is cooled to, obtains multi-stage artery structure Diatomite-based Porous Ceramics；
（5）The above-mentioned multi-stage artery structure Diatomite-based Porous Ceramics of 10~20g are weighed, add 50~100mL mass fractions
In 25% sodium hydroxide solution, to be heated to 60~70 DEG C, and 40~50min is stirred with 300~500r/min, then filtered, will
Filter cake is placed in drying box, is dried at 105~110 DEG C to constant weight, is obtained 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 into 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, processing time is short, and technique is simple；
（2）Prepared by alkaline ceramic lipin deacidifying agent prepared by the present invention convenient, the recyclable reuse of carrier, does not pollute ring
Border.
Embodiment
One piece of 1cm × 1cm × 1cm of clip flexible polyurethane foams, it is 10% hydrogen to be immersed in 100~150mL mass fractions
In sodium hydroxide solution, 2~3h is soaked under 60~65 DEG C of waters bath with thermostatic control, takes 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 is soaked, flexible polyurethane foams is then taken out, natural air drying, obtains surface preparation flexible polyurethane foams；Weigh 1.2
~1.5g sodium chloride, 2~5g sodium metasilicate, add in 60~65mL deionized waters, 10~15min stirred with 300~400r/min,
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 to drench slurry processing, and additional size is removed with roll squeezer pressure, repeat above-mentioned leaching slurry
Operation 3~4 times, is then continued in drying box, and 1~2h is dried 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, 25~30mL mass fractions are instilled as in the 20% TPAOH aqueous solution using 1~3mL/min, with 300~400r/
Min stirs 10~12h, adds above-mentioned diatomite ceramics, 60~70h is reacted under 90~95 DEG C of waters bath with thermostatic control, then filtering,
After filter residue 3~5 times is washed with deionized, 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, add 50~100mL mass
Fraction is in 25% sodium hydroxide solution, is heated to 60~70 DEG C, and stirs 40~50min with 300~500r/min, is then taken out
Filter, filter cake is placed in drying box, is dried at 105~110 DEG C to constant weight, is obtained alkaline ceramic lipin deacidifying agent.
Example 1
One piece of 1cm × 1cm × 1cm of clip flexible polyurethane foams, it is 10% hydroxide to be immersed in 100mL mass fractions
In sodium solution, 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 will
It is immersed in mass fraction in 1% carboxymethylcellulose sodium solution, 1h to be soaked under 60 DEG C of waters bath with thermostatic control, is then taken out soft
Polyurethane foam, natural air drying, obtain surface preparation flexible polyurethane foams；1.2g sodium chloride is weighed, 2g sodium metasilicate, is added
In 60mL deionized waters, 10min is stirred with 300r/min, adds 25g diatomite, 7mL mass fractions are 10% phthalic acid
Diethylene glycol diacrylate solution, 10h is stirred with 800r/min, obtains diatomite slurry；Above-mentioned surface preparation is soft poly-
Urethane 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 will
It is placed on woven wire filter plate, and with above-mentioned diatomite slurry foams are carried out drenching slurry with handling, and gone with roll squeezer pressure it is unnecessary
Slurry, repeat above-mentioned leaching slurry and operate 3 times, then continue in drying box, 1h is dried at 70 DEG C, then be placed in Muffle furnace,
600 DEG C are heated to, keeping temperature calcining 3h, room temperature is naturally cooled to, obtains diatomite ceramics；10mL tetraethyl orthosilicates are measured, with
It is in the 20% TPAOH aqueous solution that 1mL/min, which instills 25mL mass fractions, stirs 10h with 300r/min, adds
Diatomite ceramics are stated, react 60h under 90 DEG C of waters bath with thermostatic control, then filtering, after filter residue 3 times is washed with deionized, by filter residue
It is placed in drying box, 1h is dried at 70 DEG C, then be placed in Muffle furnace, is heated to 550 DEG C, keeping temperature calcining 3h, from
Room temperature so is cooled to, obtains multi-stage artery structure Diatomite-based Porous Ceramics；Weigh the above-mentioned multi-stage artery structure diatomite Quito of 10g
Hole ceramics, it is in 25% sodium hydroxide solution to add 50mL mass fractions, is heated to 60 DEG C, and stirs 40min with 300r/min,
Then filter, filter cake is placed in drying box, dried at 105 DEG C to constant weight, obtain 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 into 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
One piece of 1cm × 1cm × 1cm of clip flexible polyurethane foams, it is 10% hydroxide to be immersed in 120mL mass fractions
In sodium solution, 2.5h is soaked under 62 DEG C of waters bath with thermostatic control, take out flexible polyurethane foams, and after being washed with deionized 2 times, then
Mass fraction is immersed in 1% carboxymethylcellulose sodium solution, to soak 1.5h under 62 DEG C of waters bath with thermostatic control, is then taken out
Flexible polyurethane foams, natural air drying, obtain surface preparation flexible polyurethane foams；1.3g sodium chloride is weighed, 3g sodium metasilicate, is added
Enter in 62mL deionized waters, 12min is stirred with 350r/min, adds 28g diatomite, 7.5mL mass fractions are 10% adjacent benzene two
Formic acid diethylene glycol diacrylate solution, 11h is stirred with 900r/min, obtains diatomite slurry；Above-mentioned surface preparation is soft
Matter 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,
It is placed on again on woven wire filter plate, foams is carried out with above-mentioned diatomite slurry to drench slurry processing, and gone with roll squeezer pressure
Additional size, repeat above-mentioned leaching slurry and operate 3 times, then continue in drying box, 1.5h is dried at 75 DEG C, then be placed on Muffle
In stove, 700 DEG C are heated to, keeping temperature calcining 4h, room temperature is naturally cooled to, obtains diatomite ceramics；Measure the positive silicic acid second of 11mL
Ester, 28mL mass fractions are instilled as in the 20% TPAOH aqueous solution using 2mL/min, 11h is stirred with 360r/min, then
Above-mentioned diatomite ceramics are added, react 65h under 92 DEG C of waters bath with thermostatic control, then filtering, after filter residue 4 times is washed with deionized,
Filter residue is placed in drying box, 1.5h is dried at 75 DEG C, then is placed in Muffle furnace, is heated to 580 DEG C, keeping temperature is forged
4h is burnt, room temperature is naturally cooled to, obtains multi-stage artery structure Diatomite-based Porous Ceramics；Weigh the above-mentioned multi-stage artery structure silicon of 15g
Diatomaceous earth base porous ceramics, it is in 25% sodium hydroxide solution to add 80mL mass fractions, is heated to 65 DEG C, and stir with 400r/min
45min is mixed, then filters, filter cake is placed in drying box, is dried at 108 DEG C to constant weight, obtains 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 into 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
One piece of 1cm × 1cm × 1cm of clip flexible polyurethane foams, it is 10% hydroxide to be immersed in 150mL mass fractions
In sodium solution, 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 will
It is immersed in mass fraction in 1% carboxymethylcellulose sodium solution, 2h to be soaked under 65 DEG C of waters bath with thermostatic control, is then taken out soft
Polyurethane foam, natural air drying, obtain surface preparation flexible polyurethane foams；1.5g sodium chloride is weighed, 5g sodium metasilicate, is added
In 65mL deionized waters, 15min is stirred with 400r/min, adds 30g diatomite, 8mL mass fractions are 10% phthalic acid
Diethylene glycol diacrylate solution, 12h is stirred with 1000r/min, obtains diatomite slurry；Above-mentioned surface preparation is soft poly-
Urethane 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 will
It is placed on woven wire filter plate, and with above-mentioned diatomite slurry foams are carried out drenching slurry with handling, and gone with roll squeezer pressure it is unnecessary
Slurry, repeat above-mentioned leaching slurry and operate 4 times, then continue in drying box, 2h is dried at 80 DEG C, then be placed in Muffle furnace,
800 DEG C are heated to, keeping temperature calcining 5h, room temperature is naturally cooled to, obtains diatomite ceramics；12mL tetraethyl orthosilicates are measured, with
It is in the 20% TPAOH aqueous solution that 3mL/min, which instills 30mL mass fractions, stirs 12h with 400r/min, adds
Diatomite ceramics are stated, react 70h under 95 DEG C of waters bath with thermostatic control, then filtering, after filter residue 5 times is washed with deionized, by filter residue
It is placed in drying box, 2h is dried at 80 DEG C, then be placed in Muffle furnace, is heated to 600 DEG C, keeping temperature calcining 5h, from
Room temperature so is cooled to, obtains multi-stage artery structure Diatomite-based Porous Ceramics；Weigh the above-mentioned multi-stage artery structure diatomite Quito of 20g
Hole ceramics, it is in 25% sodium hydroxide solution to add 100mL mass fractions, is heated to 70 DEG C, and stirs 50min with 500r/min,
Then filter, filter cake is placed in drying box, dried at 110 DEG C to constant weight, obtain 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 into 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 specifically preparation process is：
（1）One piece of 1cm × 1cm × 1cm of clip flexible polyurethane foams, it is 10% hydrogen to be immersed in 100~150mL mass fractions
In sodium hydroxide solution, 2~3h is soaked under 60~65 DEG C of waters bath with thermostatic control, takes 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 is soaked, flexible polyurethane foams is then taken out, natural air drying, obtains surface preparation flexible polyurethane foams, it is standby；
（2）1.2~1.5g sodium chloride is weighed, 2~5g sodium metasilicate, is added in 60~65mL deionized waters, with 300~400r/min
10~15min is stirred, adds 25~30g diatomite, 7~8mL mass fractions are 10% O-phthalic acid diethylene glycol dipropyl alkene
Acid esters solution, 10~12h is stirred with 800~1000r/min, 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 processing to foams, and removes additional size with roll squeezer pressure, repeats above-mentioned leaching and starches operation 3~4 times, then continues at
In drying box, 1~2h is dried at 70~80 DEG C, then is placed in Muffle furnace, is heated to 600~800 DEG C, keeping temperature
3~5h is calcined, 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 using 1~3mL/min
Change in 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, then filtering, after filter residue 3~5 times is washed with deionized, filter residue is placed in drying box, 70~
1~2h is dried at 80 DEG C, then is placed in Muffle furnace, is 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, it is 25% to add 50~100mL mass fractions
In sodium hydroxide solution, 60~70 DEG C are heated to, and 40~50min is stirred with 300~500r/min, is then filtered, by filter cake
It is placed in drying box, is dried at 105~110 DEG C to constant weight, obtain alkaline ceramic lipin deacidifying agent.
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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 |
-
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 |
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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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