CN105833844B - A kind of preparation method of lotus leaf deacidification agent - Google Patents
A kind of preparation method of lotus leaf deacidification agent Download PDFInfo
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- CN105833844B CN105833844B CN201610173076.3A CN201610173076A CN105833844B CN 105833844 B CN105833844 B CN 105833844B CN 201610173076 A CN201610173076 A CN 201610173076A CN 105833844 B CN105833844 B CN 105833844B
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/10—Refining fats or fatty oils by adsorption
-
- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/44—Materials comprising a mixture of organic materials
-
- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
-
- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
-
- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/485—Plants or land vegetals, e.g. cereals, wheat, corn, rice, sphagnum, peat moss
Abstract
The present invention relates to a kind of preparation method of lotus leaf deacidification agent, belong to deacidification agent preparing technical field.For current adsorption deacidification agent single effect and limitation it is larger, it can not meet effective removing to oleic acid, labile problem in adsorption process, milled by the way that new new lotus leaf is dried, extract Nuciferine under ultrasonication, then by the way that dry lotus leaf is milled activation, prepare micropore depickling agent carrier, by the way that Nuciferine and micropore depickling agent carrier is for composite, Nuciferine is loaded on activation lotus leaf depickling agent carrier, vegetable oil acid is effectively removed.Deacidification agent oil consumption loss rate prepared by the present invention is relatively low, is only 0.1%, its adsorption efficiency improves 25~30% compared with other deacidification agents, and preparation process is simple, environmentally protective, environmentally safe.
Description
Technical field
The present invention relates to a kind of preparation method of lotus leaf deacidification agent, belong to deacidification agent preparing technical field.
Background technology
Oil and fat refining is that the oil to be refined of certain mass is processed into the product oil to conform to quality requirements, the reality of this process
Matter is to remove the non-neutral oil composition in oil to be refined, so that more pure product oil is obtained, that is, neutral oil purification
Process.In general, oil and fat refining mainly includes the processes such as grease filtrating, degumming, depickling, decoloration, deodorization, winterization, dewaxing.
The oil Jing Guo filtering, degumming, depickling wherein is become half to refine oil, and the oil by decoloration, deodorization, winterization, dewaxing is known as refining
Oil.Generally without in the crude oil of refining, containing a certain number of free fatties, free fatty in grease is removed
Process is known as depickling.Traditional lipin deacidifying method includes chemical deacidification, physical deacidification and miscella depickling.Traditional depickling side
Method due to the limitation of itself, there are some it is inevitable the shortcomings that.It is the shortcomings that to overcome traditional acid stripping method, many new
Acid stripping method is studied personnel and is invented, and such as chemical resterification depickling, solvent extract deacidification, supercritical extract depickling, molecule steam
Evaporate depickling, enzyme process depickling.
During existing biology depickling, the reaction time is longer, enzyme price is only applicable to high acid value crude oil costly, at present, and changes
When learning esterification deacidification, cost is higher, and solvent consumption, precipitation are of high cost, and absorption method is in deacidification, by some to fat
Acid has in the material absorption grease of selective absorption effect and other impurities, realizes the separation with neutral oil, but existing
Adsorption deacidification agent single effect and limitation it is larger, can not meet effective removing to oleic acid, easily be decomposed in adsorption process, institute
To need the higher deacidification agent of a kind of adsorption efficiency and deacidification efficiency necessary.
The content of the invention
The technical problems to be solved by the invention：For current adsorption deacidification agent single effect and limitation it is larger, can not
Meet to remove the effective of oleic acid, labile problem in adsorption process, there is provided one kind is by the way that new new lotus leaf is dried
Mill, extract Nuciferine under ultrasonication, then by the way that dry lotus leaf is milled activation, prepare micropore depickling agent carrier, pass through
Nuciferine and micropore depickling agent carrier is for composite, Nuciferine is loaded on activation lotus leaf depickling agent carrier, to vegetable oil
Acid is effectively removed.
In order to solve the above technical problems, the present invention is using technical solution as described below：
（1）New new lotus leaf is collected, dry 6~8h is placed at 85~90 DEG C, then it is milled and is sieved, is prepared into
50~60 mesh Lotus Leafs, then in mass ratio 1:10, Lotus Leaf is mixed with absolute ethyl alcohol and stirring, is placed on 65~80
10~15min of heating water bath at DEG C；
（2）After the completion of to be heated, apply 300~400W to it and be ultrasonically treated 10~15min, Lotus Leaf matter is then added dropwise
The hydrochloric acid solution of the 0.2mol/L of amount 50%, it is 10~15min to control time for adding, after being added dropwise to complete, 2~3h of Heat preservation；
（3）After the completion for the treatment of Heat preservation, it is filtered and collects filtrate, with mass concentration for 2% ammonia spirit adjust pH to
8.5, it is stirred to its completely precipitation, it is filtered and collects filtrate, by volume 1:5, filtrate and absolute ethyl alcohol are stirred
Mixing is mixed, then with 0.50 μm of membrane filtration and filtrate is collected, is placed on rotary evaporated to dryness at 75~80 DEG C, you can preparation
Obtain Nuciferine；
（4）By step（1）Obtained Lotus Leaf is placed in Muffle furnace, at 100~110 DEG C thermal activation treatment 3~
5min, then mills and sieves to it, is prepared into 60~70 mesh activation Lotus Leaf, then counts in parts by weight, weighs 45 respectively
~55 parts of deionized waters, 10~15 parts of Nuciferines and 35~40 parts of activation Lotus Leafs are placed in four-hole boiling flask, are stirred 10
~15min；
（5）After the completion of mixing to be mixed, it is placed on heating water bath at 85~90 DEG C and is stirred 45~60min, treat
After the completion of being stirred, stop heating and standing being cooled to 25 DEG C, then it is filtered and collects filter residue, is placed on 80~85
Dry 6~8h at DEG C, you can be prepared into a kind of lotus leaf deacidification agent.
The present invention application process be：The degumming rapeseed oil of certain mass is weighed in flask, covers lid, is loaded parallel
Reaction station, opens heating, and after oil temperature reaches preset temperature, the deacidification agent of vegetable seed oil quality 10% is added into oil, adjusts stirring
Speed is to 150~200r/min, after 30~45min of reaction to be adsorbed, by the deacidification agent degumming oil mixture in flask be transferred to from
Depickling oil is centrifugally separating to obtain in heart pipe.
Compared with other methods, advantageous effects are the present invention：
（1）Deacidification agent oil consumption loss rate prepared by the present invention is relatively low, is only 0.1%, its adsorption efficiency is improved compared with other deacidification agents
25~30%；
（2）Preparation process of the present invention is simple, environmentally protective, environmentally safe.
Embodiment
New new lotus leaf is collected first, is placed at 85~90 DEG C dry 6~8h, then it is milled and is sieved, prepare
50~60 mesh Lotus Leafs, then in mass ratio 1:10, Lotus Leaf is mixed with absolute ethyl alcohol and stirring, it is placed on 65~
10~15min of heating water bath at 80 DEG C；After the completion of to be heated, apply 300~400W to it and be ultrasonically treated 10~15min, then
The hydrochloric acid solution of the 0.2mol/L of Lotus Leaf quality 50% is added dropwise, it is 10~15min to control time for adding, after being added dropwise to complete,
2~3h of Heat preservation；After the completion for the treatment of Heat preservation, it is filtered and collects filtrate, adjusted with mass concentration for 2% ammonia spirit
PH to 8.5, is stirred to its completely precipitation, it is filtered and collects filtrate, and by volume 1:5, by filtrate and anhydrous second
Alcohol is stirred, and then with 0.50 μm of membrane filtration and is collected filtrate, is placed on rotary evaporated to dryness at 75~80 DEG C, you can
It is prepared into Nuciferine；Lotus Leaf is placed in Muffle furnace, 3~5min of thermal activation treatment at 100~110 DEG C, then to it
Mill and sieve, be prepared into 60~70 mesh activation Lotus Leaf, then count in parts by weight, weigh 45~55 parts of deionizations respectively
Water, 10~15 parts of Nuciferines and 35~40 parts of activation Lotus Leafs are placed in four-hole boiling flask, are stirred 10~15min；Wait to stir
After the completion of mixing mixing, it is placed on heating water bath at 85~90 DEG C and is stirred 45~60min, after the completion of mixing to be mixed,
Stop heating and standing being cooled to 25 DEG C, then it filtered and collects filter residue, be placed at 80~85 DEG C dry 6~8h,
A kind of lotus leaf deacidification agent can be prepared into.
Example 1
New new lotus leaf is collected first, is placed at 85 DEG C dry 6h, then it is milled and is sieved, is prepared into 50 mesh lotuses
Leaf powder, then in mass ratio 1:10, Lotus Leaf is mixed with absolute ethyl alcohol and stirring, is placed on heating water bath at 65 DEG C
10min；After the completion of to be heated, apply 300W to it and be ultrasonically treated 10min, the 0.2mol/ of Lotus Leaf quality 50% is then added dropwise
The hydrochloric acid solution of L, it is 10min to control time for adding, after being added dropwise to complete, Heat preservation 2h；After the completion for the treatment of Heat preservation, to it
Filter and collect filtrate, adjust pH to 8.5 for 2% ammonia spirit with mass concentration, be stirred to its completely precipitation, to it
Filter and collect filtrate, by volume 1:5, filtrate is mixed with absolute ethyl alcohol and stirring, then with 0.50 μm of membrane filtration and is received
Collect filtrate, be placed on rotary evaporated to dryness at 75 DEG C, you can be prepared into Nuciferine；Lotus Leaf is placed in Muffle furnace, in
Thermal activation treatment 3min at 110 DEG C, then mills and sieves to it, is prepared into 60 mesh activation Lotus Leaf, then in parts by weight
Meter, weighs 45 parts of deionized waters, 15 parts of Nuciferines and 40 parts of activation Lotus Leafs and is placed in four-hole boiling flask, be stirred respectively
10min；After the completion of mixing to be mixed, it is placed on heating water bath at 85 DEG C and is stirred 45min, mixing to be mixed is completed
Afterwards, stop heating and standing being cooled to 25 DEG C, then it filtered and collects filter residue, be placed at 80 DEG C dry 6h, you can
It is prepared into a kind of lotus leaf deacidification agent.
The degumming rapeseed oil of certain mass is weighed in flask, covers lid, loads parallel reaction station, heating is opened, treats
After oil temperature reaches preset temperature, the deacidification agent of vegetable seed oil quality 10% is added into oil, mixing speed is adjusted to 150r/min, treats
After adsorption reaction 30min, the deacidification agent degumming oil mixture in flask is transferred in centrifuge tube and is centrifugally separating to obtain depickling oil.
Example 2
New new lotus leaf is collected first, is placed at 87 DEG C dry 7h, then it is milled and is sieved, is prepared into 55 mesh lotuses
Leaf powder, then in mass ratio 1:10, Lotus Leaf is mixed with absolute ethyl alcohol and stirring, is placed on heating water bath at 72 DEG C
12min；After the completion of to be heated, apply 350W to it and be ultrasonically treated 12min, the 0.2mol/ of Lotus Leaf quality 50% is then added dropwise
The hydrochloric acid solution of L, it is 12min to control time for adding, after being added dropwise to complete, Heat preservation 2h；After the completion for the treatment of Heat preservation, to it
Filter and collect filtrate, adjust pH to 8.5 for 2% ammonia spirit with mass concentration, be stirred to its completely precipitation, to it
Filter and collect filtrate, by volume 1:5, filtrate is mixed with absolute ethyl alcohol and stirring, then with 0.50 μm of membrane filtration and is received
Collect filtrate, be placed on rotary evaporated to dryness at 77 DEG C, you can be prepared into Nuciferine；Lotus Leaf is placed in Muffle furnace, in
Thermal activation treatment 4min at 105 DEG C, then mills and sieves to it, is prepared into 65 mesh activation Lotus Leaf, then in parts by weight
Meter, weighs 50 parts of deionized waters, 12 parts of Nuciferines and 37 parts of activation Lotus Leafs and is placed in four-hole boiling flask, be stirred respectively
12min；After the completion of mixing to be mixed, it is placed on heating water bath at 87 DEG C and is stirred 52min, mixing to be mixed is completed
Afterwards, stop heating and standing being cooled to 25 DEG C, then it filtered and collects filter residue, be placed at 82 DEG C dry 7h, you can
It is prepared into a kind of lotus leaf deacidification agent.
The degumming rapeseed oil of certain mass is weighed in flask, covers lid, loads parallel reaction station, heating is opened, treats
After oil temperature reaches preset temperature, the deacidification agent of vegetable seed oil quality 10% is added into oil, mixing speed is adjusted to 170r/min, treats
After adsorption reaction 38min, the deacidification agent degumming oil mixture in flask is transferred in centrifuge tube and is centrifugally separating to obtain depickling oil.
Example 3
New new lotus leaf is collected first, is placed at 90 DEG C dry 8h, then it is milled and is sieved, is prepared into 60 mesh lotuses
Leaf powder, then in mass ratio 1:10, Lotus Leaf is mixed with absolute ethyl alcohol and stirring, is placed on heating water bath at 80 DEG C
15min；After the completion of to be heated, apply 400W to it and be ultrasonically treated 15min, the 0.2mol/ of Lotus Leaf quality 50% is then added dropwise
The hydrochloric acid solution of L, it is 15min to control time for adding, after being added dropwise to complete, Heat preservation 3h；After the completion for the treatment of Heat preservation, to it
Filter and collect filtrate, adjust pH to 8.5 for 2% ammonia spirit with mass concentration, be stirred to its completely precipitation, to it
Filter and collect filtrate, by volume 1:5, filtrate is mixed with absolute ethyl alcohol and stirring, then with 0.50 μm of membrane filtration and is received
Collect filtrate, be placed on rotary evaporated to dryness at 80 DEG C, you can be prepared into Nuciferine；Lotus Leaf is placed in Muffle furnace, in
Thermal activation treatment 5min at 110 DEG C, then mills and sieves to it, is prepared into 70 mesh activation Lotus Leaf, then in parts by weight
Meter, weighs 55 parts of deionized waters, 10 parts of Nuciferines and 35 parts of activation Lotus Leafs and is placed in four-hole boiling flask, be stirred respectively
15min；After the completion of mixing to be mixed, it is placed on heating water bath at 90 DEG C and is stirred 60min, mixing to be mixed is completed
Afterwards, stop heating and standing being cooled to 25 DEG C, then it filtered and collects filter residue, be placed at 85 DEG C dry 8h, you can
It is prepared into a kind of lotus leaf deacidification agent.
The degumming rapeseed oil of certain mass is weighed in flask, covers lid, loads parallel reaction station, heating is opened, treats
After oil temperature reaches preset temperature, the deacidification agent of vegetable seed oil quality 10% is added into oil, mixing speed is adjusted to 200r/min, treats
After adsorption reaction 45min, the deacidification agent degumming oil mixture in flask is transferred in centrifuge tube and is centrifugally separating to obtain depickling oil.
Claims (1)
1. a kind of preparation method of lotus leaf deacidification agent, it is characterised in that specifically preparation process is：
（1）New new lotus leaf is collected, dry 6~8h is placed at 85~90 DEG C, then it is milled and is sieved, it is prepared into 50~
60 mesh Lotus Leafs, then in mass ratio 1:10, Lotus Leaf is mixed with absolute ethyl alcohol and stirring, is placed at 65~80 DEG C
10~15min of heating water bath；
（2）After the completion of to be heated, apply 300~400W to it and be ultrasonically treated 10~15min, Lotus Leaf quality is then added dropwise
The hydrochloric acid solution of 50% 0.2mol/L, it is 10~15min to control time for adding, after being added dropwise to complete, 2~3h of Heat preservation；
（3）After the completion for the treatment of Heat preservation, it is filtered and collects filtrate, pH to 8.5 is adjusted for 2% ammonia spirit with mass concentration,
It is stirred to its completely precipitation, it is filtered and collects filtrate, by volume 1:5, filtrate and absolute ethyl alcohol and stirring are mixed
Close, then with 0.50 μm of membrane filtration and collect filtrate, be placed on rotary evaporated to dryness at 75~80 DEG C, you can be prepared into lotus
Leaf alkali；
（4）By step（1）Obtained Lotus Leaf is placed in Muffle furnace, 3~5min of thermal activation treatment at 100~110 DEG C, with
It is milled and is sieved afterwards, is prepared into 60~70 mesh activation Lotus Leaf, then is counted in parts by weight, weighing 45~55 parts respectively goes
Ionized water, 10~15 parts of Nuciferines and 35~40 parts of activation Lotus Leafs are placed in four-hole boiling flask, are stirred 10~15min；
（5）After the completion of mixing to be mixed, it is placed on heating water bath at 85~90 DEG C and is stirred 45~60min, it is to be mixed
After the completion of mixing, stop heating and standing being cooled to 25 DEG C, then it is filtered and collects filter residue, is placed at 80~85 DEG C
Dry 6~8h, you can be prepared into a kind of lotus leaf deacidification agent.
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| CN108504384B (en) * | 2018-03-28 | 2020-09-08 | 福州专志信息技术有限公司 | Preparation method of diesel deacidification agent |
| CN111254005B (en) * | 2020-01-19 | 2023-04-07 | 河南农业大学 | Preparation method of functional edible oil |
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| DE10157067A1 (en) * | 2001-11-21 | 2003-05-28 | Cognis Deutschland Gmbh | Process for deacidifying natural fats and oils |
| CN100463868C (en) * | 2007-01-25 | 2009-02-25 | 河北农业大学 | Ecological, environmental protective composite water treatment agent |
| CN102442949A (en) * | 2010-10-09 | 2012-05-09 | 苏州宝泽堂医药科技有限公司 | Method for extracting nuciferine from lotus leaves |
| CN104607153A (en) * | 2014-12-26 | 2015-05-13 | 安徽省中日农业环保科技有限公司 | Heavy metal ion adsorbent prepared from lotus leaves and preparation method thereof |
| CN105170077B (en) * | 2015-09-30 | 2017-10-27 | 太仓碧奇新材料研发有限公司 | The preparation method of pinkish red chalk powder composite material in a kind of removal dyeing waste water |
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Effective date of registration: 20180227 Address after: The ten Party of Shiyan city in Hubei province 442000 yuan Cun Tan Jia Wan Zhen Yunyang District Applicant after: Hubei Xiang Yu Yu edible oil industry and Trade Co., Ltd. Address before: 213155 room 703, Phoenix famous city, Xinbei District, Changzhou, Jiangsu Applicant before: Dong Xiao |
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Address after: 442000 ten TAN Fang village, Tan Jia Wan Town, Yunyang District, Shiyan, Hubei Patentee after: Hubei Xiang Man Yu Biological Technology Co., Ltd. Address before: 442000 ten TAN Fang village, Tan Jia Wan Town, Yunyang District, Shiyan, Hubei Patentee before: Hubei Xiang Yu Yu edible oil industry and Trade Co., Ltd. |
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