CN106824130A - A kind of decolorising agent of the addition modified active illite/smectite mixed layer clay refined for vegetable oil - Google Patents
A kind of decolorising agent of the addition modified active illite/smectite mixed layer clay refined for vegetable oil Download PDFInfo
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- CN106824130A CN106824130A CN201710095656.XA CN201710095656A CN106824130A CN 106824130 A CN106824130 A CN 106824130A CN 201710095656 A CN201710095656 A CN 201710095656A CN 106824130 A CN106824130 A CN 106824130A
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- illite
- mixed layer
- layer clay
- smectite mixed
- vegetable oil
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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
- B01J20/26—Synthetic macromolecular compounds
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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
- B01J20/12—Naturally occurring clays or bleaching earth
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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
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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- 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
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- Analytical Chemistry (AREA)
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- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
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- Geochemistry & Mineralogy (AREA)
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- Silicates, Zeolites, And Molecular Sieves (AREA)
- Fats And Perfumes (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a kind of decolorising agent of the addition modified active illite/smectite mixed layer clay refined for vegetable oil, it is characterised in that be made up of the raw material of following weight portion：Illite/smectite mixed layer clay raw ore 100 110, hydrochloric acid 30 33, cetyl trimethylammonium bromide 25 27, appropriate deionized water, macroporous absorbent resin 34 37, shitosan 10 11.5, concentration are acetic acid 100 110, graphene oxide 10 12, appropriate ethylene glycol, sodium acetate 62 65, the Iron(III) chloride hexahydrate 16 18 of 2wt%.The decolorising agent that the present invention is made is used for the refined of vegetable oil, can not only remove the pigment in vegetable oil, additionally it is possible to adsorb the materials such as metal ion, toxin, the residual colloid of residual in vegetable oil, and production technology is easy to control, and decolorizing effect is excellent.
Description
Technical field
The present invention relates to grease-decolor technical field, more particularly to a kind of addition modified active refined for vegetable oil she
Cover the decolorising agent of mixed-layer clay.
Background technology
Grease-decolor is a highly important step process in oil and fat refining process, can improve the outward appearance of oil product, industrial normal
Decolourized with absorption method.Adsorption decoloring method is the difference using molecular attraction between adsorbent and coloring matter and product, is made
Pigment molecular is combined so as to be separated with grease with adsorbent, is played except the method for pigment effect in degreasing.Particularly vegetable oil
Decolorization can not merely remove pigment, improve grease color, also to remove bring into vegetable oil in oil refining process micro
Metal ion, residual colloid and part stink substance, and then cause that vegetable oil reaches different grades.
Atlapulgite is with clay mineral（Typically bentonite）It is raw material, there is network of micropores through acid activation treatment is obtained
Network structure, specific surface area are larger, adsorptivity and a kind of stronger adsorbent of decoloring ability, can be used for the refining of oil, lubricating oil
The purification of decolouring and insulating oil with vegetable and animals oils.The bentonitic acid activation process of tradition is divided into wet method, dry method and semidry method
Three classes.Wet processing acid consumption is big, produces substantial amounts of spent acid waste water, and energy consumption for drying is high；It is uneven to there is acid activation in dry process
It is even, product quality shortcoming not high.
《Iraq/Mongolia mixed-layer clay semidry method hydrochloric acid activation prepares atlapulgite》Semidry method hydrochloric acid activation technique is used in one text
Activation modification is carried out to Iraq/Mongolia mixed-layer clay, process optimization has been carried out to hydrochloric acid consumption, concentration of hydrochloric acid, curing temperature respectively, obtained
To concentration of hydrochloric acid be 6%, hydrochloric acid consumption be clay quality 30%, hydrochloric acid spray charging, curing temperature be 40 DEG C, curing when
Between under conditions of 24 h, Product Activity degree highest when commercially available common carclazyte is mixed, further increases the decolouring of product
Rate, while reducing production cost.But the present invention is cured 24 hours during incubator is put into after being activated using semidry method, raw
Produce efficiency low, and energy consumption is big, it is necessary to be modified to processing mode；Simultaneously because the absorption that obtained product is used for liquid takes off
Color, it is necessary to further improve atlapulgite suspension in a liquid, to meet the demand of application.
The content of the invention
The object of the invention is exactly to make up the defect of prior art, there is provided a kind of to be modified for the addition that vegetable oil is refined
Activate the decolorising agent of illite/smectite mixed layer clay.
The present invention is achieved by the following technical solutions：
A kind of decolorising agent of the addition modified active illite/smectite mixed layer clay refined for vegetable oil, by the raw material system of following weight portion
Prepare into：Illite/smectite mixed layer clay raw ore 100-110, hydrochloric acid 30-33, cetyl trimethylammonium bromide 25-27, deionized water are fitted
Amount, macroporous absorbent resin 34-37, shitosan 10-11.5, concentration are acetic acid 100-110, graphene oxide 10-12, the second of 2wt%
Appropriate glycol, sodium acetate 62-65, Iron(III) chloride hexahydrate 16-18.
The decolorising agent of a kind of organic modified active illite/smectite mixed layer clay of addition refined for vegetable oil, by following tool
Body step is prepared from：
（1）Illite/smectite mixed layer clay raw ore is carried out into preliminary treatment, 200 mesh sieves was crushed stand-by；By cetyl trimethyl bromination
Ammonium is dissolved in the 40-45 times of deionized water measured, and adds the illite/smectite mixed layer clay after above-mentioned crushing, turned with 1000-1200 at room temperature/
Point speed stir 4-5 hour, centrifugation, be put into baking oven with 60-80 DEG C drying, mistake 200 mesh sieves, obtain it is organically-modified she
Cover mixed-layer clay stand-by；Above-mentioned organically-modified illite/smectite mixed layer clay is put into reactor, 0.3-0.35 times is added dropwise while stirring
The hydrochloric acid of amount, until being added dropwise complete, is then put it into micro-wave oven and is taken after 30-40 seconds with the power priming reaction of 450-500W
Go out, be put into baking oven and dried 3-4 hours with 100-110 DEG C, grind to form powdery, obtain organically-modified activation illite/smectite mixed layer clay；
（2）Dissolve the chitosan in the acetic acid that concentration is 2wt%, stir stand-by；Add graphene oxide into 60-70
Again in the ethylene glycol of amount, mixed liquor is formed within ultrasonic disperse 20-30 minutes, be subsequently adding Iron(III) chloride hexahydrate, continue ultrasound 15-
20 minutes, sodium acetate is continuously added, above-mentioned chitosan-acetic acid solution is added after being stirred vigorously 20-30 minutes, mix 30-40
Minute；
（3）By step（2）The mixture for obtaining is put into hydrothermal reaction kettle, is heated to 180-190 DEG C, cold after reacting 5-6 hours
But to room temperature, product is filtered, is put into vacuum drying chamber after being washed with deionized 2-3 times and dries 8- with 50-60 DEG C
10 hours, obtain shitosan magnetic graphene complex；
（4）By step（1）Step（3）The product mixing for obtaining, adds remaining residual components, obtains final product.
A kind of decolorising agent of described addition modified active illite/smectite mixed layer clay refined for vegetable oil, hydrochloric acid is quality
Concentration is 6% hydrochloric acid.
A kind of decolorising agent of described addition modified active illite/smectite mixed layer clay refined for vegetable oil, macroporous absorption tree
Fat includes the one kind in macroporous absorbent resin HP2MGL, macroporous absorbent resin HP20, macroporous absorbent resin SP80.
A kind of preparation of the decolorising agent of described organic modified active illite/smectite mixed layer clay of addition refined for vegetable oil
Method, step（1）Described in illite/smectite mixed layer clay raw ore preliminary treatment include first by illite/smectite mixed layer clay crushing raw ore extremely
Then average grain diameter is dried with 150-250 DEG C of temperature in an oven less than the particle of 20 mesh, then size-reduced machine is ground into 200
Purpose powder.
It is an advantage of the invention that：The present invention carries out season first with cetyl trimethylammonium bromide to illite/smectite mixed layer clay
Ammonium salt is organically-modified, is reacted with intercalation so that the zeta current potentials increase of illite/smectite mixed layer clay, improves suspension stability,
Recycle hydrochloric acid carries out semidry method microwave activation to it, substantially reduces activity cycle, improves production efficiency, reduces hydrochloric acid
Usage amount, while activation after illite/smectite mixed layer clay particle in impurity be removed, duct is dredged, specific surface area increase, inhale
Attached performance is improved.
The present invention by sodium acetate and Iron(III) chloride hexahydrate reaction load in graphene oxide, then by hydro-thermal reaction with
Shitosan carries out reaction generation shitosan magnetic graphene complex, further enhancing adsorbing separation effect；The present invention is made
Decolorising agent be used for the refined of vegetable oil, the pigment in vegetable oil can not only be removed, additionally it is possible to adsorb what is remained in vegetable oil
The materials such as metal ion, toxin, residual colloid, and production technology is easy to control, and decolorizing effect is excellent.
Specific embodiment
A kind of decolorising agent of the addition modified active illite/smectite mixed layer clay refined for vegetable oil, by following weight portion（It is public
Jin）Raw material be made：Illite/smectite mixed layer clay raw ore 100, concentration is the hydrochloric acid 30, cetyl trimethylammonium bromide of 6wt%
25th, appropriate deionized water, macroporous absorbent resin HP2MGL34, shitosan 10, concentration are the acetic acid 100, graphene oxide of 2wt%
10th, appropriate ethylene glycol, sodium acetate 62, Iron(III) chloride hexahydrate 16.
The decolorising agent of a kind of organic modified active illite/smectite mixed layer clay of addition refined for vegetable oil, by following tool
Body step is prepared from：
（1）First by the particle that illite/smectite mixed layer clay crushing raw ore to average grain diameter is 15 mesh, then in an oven with 200 DEG C
Temperature dry, then size-reduced machine be ground into 200 mesh powder it is stand-by；By cetyl trimethylammonium bromide be dissolved in 40 times amount
In deionized water, the illite/smectite mixed layer clay after above-mentioned crushing is added, stirred 4 hours with 1000 revs/min of speed at room temperature, centrifugation
Separate, be put into baking oven with 65 DEG C of drying, cross 200 mesh sieves, obtain organically-modified illite/smectite mixed layer clay stand-by；Organic change above-mentioned
Property illite/smectite mixed layer clay be put into reactor, while stirring be added dropwise 0.3 times amount concentration for 6wt% hydrochloric acid, until dripping
Entirely, then put it into micro-wave oven and taken out after 30 seconds with the power priming reaction of 480W, be put into baking oven with 100 DEG C of dryings 3
Hour, powdery is ground to form, obtain organically-modified activation illite/smectite mixed layer clay；
（2）Dissolve the chitosan in the acetic acid that concentration is 2wt%, stir stand-by；Add graphene oxide into 60 times of amounts
Ethylene glycol in, ultrasonic disperse 20 minutes forms mixed liquor, is subsequently adding Iron(III) chloride hexahydrate, continues ultrasound 15 minutes, after
It is continuous to add sodium acetate, above-mentioned chitosan-acetic acid solution is added after being stirred vigorously 20 minutes, mix 30 minutes；
（3）By step（2）The mixture for obtaining is put into hydrothermal reaction kettle, is heated to 180 DEG C, and reaction is cooled to room after 5 hours
Temperature, product is filtered, and is put into after being washed with deionized 2 times in vacuum drying chamber with 50 DEG C of dryings 8 hours, is obtained shell and is gathered
Sugared magnetic graphene compound；
（4）By step（1）Step（3）The product mixing for obtaining, adds remaining residual components, obtains final product.
Claims (5)
1. it is a kind of for vegetable oil refine addition modified active illite/smectite mixed layer clay decolorising agent, it is characterised in that by following
The raw material of weight portion is made：Illite/smectite mixed layer clay raw ore 100-110, hydrochloric acid 30-33, cetyl trimethylammonium bromide
25-27, appropriate deionized water, macroporous absorbent resin 34-37, shitosan 10-11.5, concentration are acetic acid 100-110, the oxygen of 2wt%
Graphite alkene 10-12, appropriate ethylene glycol, sodium acetate 62-65, Iron(III) chloride hexahydrate 16-18.
2. a kind of decolouring of the organic modified active illite/smectite mixed layer clay of addition refined for vegetable oil according to claim 1
Agent, it is characterised in that be prepared from by step in detail below：
（1）Illite/smectite mixed layer clay raw ore is carried out into preliminary treatment, 200 mesh sieves was crushed stand-by；By cetyl trimethyl bromination
Ammonium is dissolved in the 40-45 times of deionized water measured, and adds the illite/smectite mixed layer clay after above-mentioned crushing, turned with 1000-1200 at room temperature/
Point speed stir 4-5 hour, centrifugation, be put into baking oven with 60-80 DEG C drying, mistake 200 mesh sieves, obtain it is organically-modified she
Cover mixed-layer clay stand-by；Above-mentioned organically-modified illite/smectite mixed layer clay is put into reactor, 0.3-0.35 times is added dropwise while stirring
The hydrochloric acid of amount, until being added dropwise complete, is then put it into micro-wave oven and is taken after 30-40 seconds with the power priming reaction of 450-500W
Go out, be put into baking oven and dried 3-4 hours with 100-110 DEG C, grind to form powdery, obtain organically-modified activation illite/smectite mixed layer clay；
（2）Dissolve the chitosan in the acetic acid that concentration is 2wt%, stir stand-by；Add graphene oxide into 60-70
Again in the ethylene glycol of amount, mixed liquor is formed within ultrasonic disperse 20-30 minutes, be subsequently adding Iron(III) chloride hexahydrate, continue ultrasound 15-
20 minutes, sodium acetate is continuously added, above-mentioned chitosan-acetic acid solution is added after being stirred vigorously 20-30 minutes, mix 30-40
Minute；
（3）By step（2）The mixture for obtaining is put into hydrothermal reaction kettle, is heated to 180-190 DEG C, cold after reacting 5-6 hours
But to room temperature, product is filtered, is put into vacuum drying chamber after being washed with deionized 2-3 times and dries 8- with 50-60 DEG C
10 hours, obtain shitosan magnetic graphene complex；
（4）By step（1）Step（3）The product mixing for obtaining, adds remaining residual components, obtains final product.
3. the decolouring of a kind of addition modified active illite/smectite mixed layer clay refined for vegetable oil according to claim 1
Agent, it is characterised in that described hydrochloric acid is hydrochloric acid that mass concentration is 6%.
4. the decolouring of a kind of addition modified active illite/smectite mixed layer clay refined for vegetable oil according to claim 1
Agent, it is characterised in that described macroporous absorbent resin includes macroporous absorbent resin HP2MGL, macroporous absorbent resin HP20, macropore
One kind in polymeric adsorbent SP80.
5. a kind of organic modified active illite/smectite mixed layer clay of addition refined for vegetable oil according to claim 2
The preparation method of decolorising agent, it is characterised in that step（1）Described in illite/smectite mixed layer clay raw ore preliminary treatment include first will
Particle of the illite/smectite mixed layer clay crushing raw ore to average grain diameter less than 20 mesh, is then dried with 150-250 DEG C of temperature in an oven
Do, then size-reduced machine is ground into the powder of 200 mesh.
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| CN201710095656.XA CN106824130A (en) | 2017-02-22 | 2017-02-22 | A kind of decolorising agent of the addition modified active illite/smectite mixed layer clay refined for vegetable oil |
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| CN201710095656.XA CN106824130A (en) | 2017-02-22 | 2017-02-22 | A kind of decolorising agent of the addition modified active illite/smectite mixed layer clay refined for vegetable oil |
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Application publication date: 20170613 |