CN106166475A - A kind of biodiesel solid decolorizer and preparation method - Google Patents
A kind of biodiesel solid decolorizer and preparation method Download PDFInfo
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- CN106166475A CN106166475A CN201610597214.0A CN201610597214A CN106166475A CN 106166475 A CN106166475 A CN 106166475A CN 201610597214 A CN201610597214 A CN 201610597214A CN 106166475 A CN106166475 A CN 106166475A
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- attapulgite
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- biodiesel
- decolorizer
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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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
- B01J20/0296—Nitrates of compounds other than those provided for in B01J20/04
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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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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Dispersion Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
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Abstract
The invention discloses a kind of biodiesel solid decolorizer and preparation method, belong to decolorising agent field, belong to biodiesel decolorising agent field in particular, the expanding agent that acidifying attapulgite, mass fraction are 1% ~ 2% and active component that mass fraction is 3% ~ 8% are sufficiently mixed rear wet granulation and dry roasting and obtain.Compared with prior art, the invention has the beneficial effects as follows: with acid attapulgite as carrier, use expanding agent and active component to be modified processing to it, thus improve specific surface area and the pore size of decolorising agent；Uniform solid decolorizer is obtained by the method such as pelletize, roasting, filtration link can be saved, effectively solve the problems such as powdery decolorising agent filtration difficulty, can effectively reduce the decolorising agent entrainment rate to oils and fats simultaneously, reduce the cost of decolorization refining, increase economic efficiency.The decolorising agent that this invention prepares has preferable decolorizing effect to dark oils and fats for the dark biodiesel that raw material prepares, and technique is simple, and cost is relatively low.
Description
Technical field
The invention discloses a kind of biodiesel solid decolorizer and preparation method, belong to decolorising agent field, more specifically
Say and belong to biodiesel decolorising agent field.
Background technology
The decolorising agent being currently used for biodiesel decolouring has chemical decolorization agent and adsorption decolouriser two kinds.And chemical decolorization agent
Pigment is had certain selectivity, and reaction condition is required by course of reaction relatively strict, and some chemical decolorization agent
Itself there is toxicity, during operation, need Special controlling, add equipment and running cost.Active hargil, attapulgite etc. are natural
Adsorbent is the most more to commonly use adsorption decolouriser, but, using these powder decolorising agents to biodiesel
When decolouring, it may appear that filtration difficulty, the problems such as oils and fats entrainment rate is high, thus add the one-tenth of biodiesel decolorization refining
This.
Chinese patent CN200910092293.X discloses a kind of biodiesel discoloration method, uses active hargil and swelling
Earth mixtures adsorption bleaching, is carrying out hydrogen peroxide oxidation, obtains biodiesel finally by deacidification dehydration.Because active hargil is just
Be bentonite acidic activated after the material that obtains, after using active hargil and bentonite adsorption, oils and fats can be with certain native raw meat
Taste, has an impact the taste of biodiesel.When again decolouring, use hydrogen peroxide as decolorising agent, need higher reaction temperature,
Just can give full play to its Oxidation, add energy consumption.
Chinese patent CN201210271002.5 discloses one and utilizes Preparation of biodiesel from waste oils discoloration method, and it is
Prepare biodiesel with waste oil for raw material, and use hydrogen peroxide oxidation method to dark grease-decolor, the grease-decolor obtained
Rate is 67.83%.But hydrogen peroxide is a kind of chemical oxidizing agent, the adsorption decolouriser that its cost is more general is higher, is not suitable for
Large-scale decolorization experiment, and hydrogen peroxide for decoloration, can only remove oxidizable dark matter, temperature and the biological bavin to reaction
The pH of oil requires higher.
Summary of the invention
It is an object of the invention to overcome defect of the prior art, it is provided that a kind of specific surface area improving decolorising agent and aperture
Size, the biodiesel solid of the cost filtering the easiest, minimizing oils and fats entrainment rate and biodiesel decolorization refining decolour
Agent and preparation method.
In order to realize foregoing invention purpose, the technical solution used in the present invention is: a kind of biodiesel solid decolorizer, its
It is characterised by, is the expanding agent of 1% ~ 2% and relative to acidifying by acidifying attapulgite, relative to acidifying attapulgite mass fraction
Attapulgite mass fraction be 3% ~ 8% active component be sufficiently mixed after add binding agent wet granulation and dry roasting and obtain.
Described mass fraction refers to that the quality of expanding agent and active constituent is respectively relative to be acidified the percent of the quality of attapulgite.
Such as, the quality of acidifying attapulgite is 100g, and the quality of expanding agent is 1-2g, and the quality of active component is 3-8g.
Described acidifying attapulgite through sodium hexameta phosphate purification process and adds the mineral acid that mass fraction is 1%-20%
Acidifying obtains.1%-20% refers to that the quality of mineral acid solute accounts for the mass percent of inorganic acid solution.
Described expanding agent be dodecylbenzene sodium sulfonate, starch, Polyethylene Glycol one or more；Described active group
It is divided into one or more of ferric nitrate, aluminum chloride or nickel nitrate.
The preparation method of a kind of biodiesel solid decolorizer, comprises the following steps:
(1) take attapulgite, add and be purified place relative to the sodium hexameta phosphate that attapulgite mass percent is 1% ~ 5%
Reason, is that 1:5 addition mineral acid carries out acidification to the attapulgite after purification process according to solid-liquid mass volume ratio (g/ml),
Make to be washed with deionized, be centrifuged off supernatant, make solid sediment be dried completely；The i.e. quality of attapulgite is 100g
Time, sodium hexameta phosphate is 1-5g；Described mineral acid includes the mineral acids such as hydrochloric acid, sulphuric acid or phosphoric acid；
(2) taking acidifying attapulgite, adding relative to acidifying attapulgite mass fraction is the expanding agent of 1% ~ 2% and relative to acid
Changing attapulgite mass fraction is the active component of 3% ~ 8%, is sufficiently mixed；
(3) addition accounts for the binding agent of mixture quality mark 1% ~ 5%, mixing granulation in wet granulator, obtains solid particle；
Described mixture is formed by being acidified attapulgite, active component and expanding agent；
(4) by above-mentioned solid particle dry after in Muffle furnace 200 ~ 600 DEG C of roasting 2 ~ 5h, obtain biodiesel solid decolouring
Agent.
Expanding agent described in step (2) be dodecylbenzene sodium sulfonate, starch, Polyethylene Glycol one or more.Step
Suddenly the active component described in (2) is one or more of ferric nitrate, aluminum chloride or nickel nitrate.Bonding described in step (3)
Agent is amidin or water.The particle diameter of described solid particle is 2 ~ 5mm.In step (2), attapulgite carrier, expanding agent and
Active component needs to be sufficiently mixed stirring 5 ~ 15min.
The preparation method of a kind of biodiesel solid decolorizer, comprises the following steps:
(1) take 600 ~ 1200g attapulgite, add and carry out pure relative to the sodium hexameta phosphate of attapulgite mass fraction 1% ~ 5%
Change processes, and is that 1:5 addition hydrochloric acid carries out acidification to purification attapulgite according to solid-liquid mass volume ratio, uses deionized water
Wash 3 ~ 4 times, until without Cl-, it is centrifuged off supernatant, solid sediment is put in baking oven and be dried completely；
(2) taking acidifying attapulgite 500 ~ 1000g that acidification obtains, addition relative to acidifying attapulgite mass fraction is
The expanding agent of 1% ~ 2% and be the active component of 3% ~ 8% relative to acidifying attapulgite mass fraction, uses stirring rod that it is abundant
5 ~ 15min is standby in mixing；
(3) addition accounts for the binding agent that mixture quality mark is 1% ~ 5%, mixing granulation in wet granulator, and obtaining particle diameter is 2
The solid particle of ~ 5mm；Described mixture is formed by being acidified attapulgite, active component and expanding agent；
(4), after above-mentioned solid particle is put into drying baker drying 12 ~ 24h, 200 ~ 600 DEG C of roasting 2 ~ 5h in Muffle furnace are sent into,
Obtain biodiesel solid decolorizer.
Compared with prior art, the invention has the beneficial effects as follows:
With acid attapulgite as carrier, use expanding agent and active component to be modified processing to it, thus improve decolorising agent
Specific surface area and pore size；Uniform solid decolorizer is obtained, it is possible to save filtration by the method such as pelletize, roasting
Link, effectively solves the problems such as powdery decolorising agent filtration difficulty, can effectively reduce the decolorising agent entrainment rate to oils and fats simultaneously,
Reduce the cost of decolorization refining, increase economic efficiency.The decolorising agent that this invention prepares prepares for raw material with dark oils and fats
Dark biodiesel have a preferable decolorizing effect, and technique is simple, and cost is relatively low.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be further described.
A kind of preparation method of biodiesel solid decolorizer, it comprises the following steps:
(1) take 600 ~ 1200g attapulgite, add and carry out relative to the sodium hexameta phosphate that attapulgite mass fraction is 1% ~ 5%
Purification process, is that 1:5 adds and accounts for the mineral acid of mass fraction 1%-20% and enter purification attapulgite according to solid-liquid mass volume ratio
Row acidification (solid masses refers to the quality of purification attapulgite, and liquid refers to inorganic acid solution), makes to be washed with deionized 3 ~ 4
Secondary, until supernatant is neutral, it is centrifuged off supernatant, solid sediment is put in 105 DEG C of baking ovens and be dried completely, obtain acid
Change attapulgite；
(2) take acidifying attapulgite 500 ~ 1000g that pretreatment obtains in 1000ml beaker, add and account for acidifying attapulgite soil property
Amount mark be 1% ~ 2% expanding agent and account for acidifying attapulgite mass fraction be the active component of 3% ~ 8%, use stirring rod will
It is standby that it is sufficiently mixed 5 ~ 15min；
(3) adding and account for the binding agent of mixture quality mark 1% ~ 5% by its mixing granulation in wet granulator, obtaining particle diameter is
The solid particle of 2 ~ 5mm；
(4), after above-mentioned solid particle is put into drying baker drying 12 ~ 24h, send into high-temperature roasting 2 ~ 5h in Muffle furnace, given birth to
Thing diesel oil solid decolorizer；
Expanding agent described in step (2) is that dodecylbenzene sodium sulfonate, starch, Polyethylene Glycol etc. have the organic of hole expansion function
One or more of thing are the most formulated.
Active component described in step (2) be ferric nitrate or other there is the reagent of identity function, such as: aluminum chloride, nitre
Acid nickel etc..
Binding agent described in step (3) is the material with attachment function, such as: amidin, pure water or meet life
The water that sanitary standard for drinking water of living requires.
Embodiment 1
The preparation method of a kind of biodiesel solid decolorizer, comprises the steps:
Step one: take 800g attapulgite, the sodium hexameta phosphate adding 2% is purified process, is that 1:5 adds according to solid-to-liquid ratio
Mass fraction be 1% hydrochloric acid carry out acidification to purification is concavo-convex, make to be washed with deionized 3 ~ 4 times, until during supernatant is
Property, it is centrifuged off supernatant, solid sediment is put in 105 DEG C of baking ovens and be dried completely；
Step 2: taking acidifying attapulgite 500g that pretreatment obtains in 1000ml beaker, adding mass fraction is the ten of 3%
Dialkyl benzene sulfonic acids sodium and mass fraction are the ferric nitrate of 5%, use stirring rod to be sufficiently mixed 10min standby；
Step 3: adding and account for the pure water of mixture quality mark 3% by its mixing granulation in wet granulator, obtaining particle diameter is 2
The solid particle of ~ 5mm；
Step 4: after above-mentioned solid particle is put into drying baker drying 14h, roasting 2.5h at 500 DEG C in feeding Muffle furnace,
To biodiesel solid decolorizer；
Decolorizing effect is checked: take 200g Rapeseed Biodiesel, uses peristaltic pump to be pumped into the chromatography equipped with solid decolorizer
In post, adsorption bleaching 60min at 60 DEG C, chromatographic column underlying collection to color is flaxen oils and fats.Use ultraviolet spectrometry light
Degree method measures the absorbance before and after Rapeseed Biodiesel decolouring, utilizes the computing formula of percent of decolourization, obtains Oleum Brassicae campestris biology bavin
The percent of decolourization of oil is 96.0%.
Embodiment 2
The method using embodiment 1 same carries out decolorising agent preparation and decolorizing effect is checked, except that prepared by decolorising agent
In journey, the addition of expanding agent dodecylbenzene sodium sulfonate is 3%.Rapeseed Biodiesel is after bleaching agent bleaching, and it decolours
Rate has reached 94.6%.
Embodiment 3
The method using embodiment 1 same carries out decolorising agent preparation and decolorizing effect is checked, except that prepared by decolorising agent
In journey, the addition of active component ferric nitrate is 5%.Rapeseed Biodiesel is after decolorising agent adsorption bleaching, and its percent of decolourization reaches
To 93.5%.
Embodiment 4
The method using embodiment 1 same carries out the preparation of decolorising agent, except that replace Semen Allii Tuberosi with trench oil biodiesel
The decolorizing effect of decolorising agent is tested by oil biodiesel, and the percent of decolourization obtaining waste oil biodiesel is 86%.
The ultimate principle of the present invention, principal character and advantage have more than been shown and described.The technical staff of the industry should
This understanding, the present invention is not restricted to the described embodiments, and simply says that the present invention's is former described in above-described embodiment and description
Reason, without departing from the spirit and scope of the present invention, the present invention also has various changes and modifications, these changes and improvements
All drop in the claimed scope of the invention.Claimed scope is by appending claims and equivalent circle thereof
Fixed.
Claims (10)
1. a biodiesel solid decolorizer, it is characterised in that by acidifying attapulgite, relative to acidifying attapulgite quality
Mark is the expanding agent of 1% ~ 2% and adds relative to being acidified after the active component that attapulgite mass fraction is 3% ~ 8% is sufficiently mixed
Enter binding agent wet granulation and dry roasting and obtain.
A kind of biodiesel solid decolorizer the most according to claim 1, it is characterised in that described acidifying attapulgite
Through sodium hexameta phosphate purification process and to add mass fraction be that the mineral acid acidified of 1%-20% obtains.
A kind of biodiesel solid decolorizer the most according to claim 1, it is characterised in that described expanding agent is 12
Sodium alkyl benzene sulfonate, starch, Polyethylene Glycol one or more；Described active component is ferric nitrate, aluminum chloride or nickel nitrate
One or more.
4. a preparation method for biodiesel solid decolorizer, comprises the following steps:
(1) take attapulgite, add and be purified place relative to the sodium hexameta phosphate that attapulgite mass percent is 1% ~ 5%
Reason, is that 1:5 addition mineral acid carries out acidification to the attapulgite after purification process according to solid-liquid mass volume ratio, makes to spend
Ionized water washs, and is centrifuged off supernatant, makes solid sediment be dried completely；
(2) taking acidifying attapulgite, adding relative to acidifying attapulgite mass fraction is the expanding agent of 1% ~ 2% and relative to acid
Changing attapulgite mass fraction is the active component of 3% ~ 8%, is sufficiently mixed；
(3) addition accounts for the binding agent of mixture quality mark 1% ~ 5%, mixing granulation in wet granulator, obtains solid particle；
Described mixture is formed by being acidified attapulgite, active component and expanding agent；
(4) by above-mentioned solid particle dry after in Muffle furnace 200 ~ 600 DEG C of roasting 2 ~ 5h, obtain biodiesel solid decolouring
Agent.
The preparation method of a kind of biodiesel solid decolorizer the most according to claim 4, it is characterised in that step (2)
Described in expanding agent be dodecylbenzene sodium sulfonate, starch, Polyethylene Glycol one or more.
The preparation method of a kind of biodiesel solid decolorizer the most according to claim 4, it is characterised in that step (2)
Described in active component is ferric nitrate, aluminum chloride or nickel nitrate one or more.
The preparation method of a kind of biodiesel solid decolorizer the most according to claim 4, it is characterised in that step (3)
Described in binding agent be amidin or water.
The preparation method of a kind of biodiesel solid decolorizer the most according to claim 4, it is characterised in that described solid
The particle diameter of granule is 2 ~ 5mm.
The preparation method of a kind of biodiesel solid decolorizer the most according to claim 4, it is characterised in that step (2)
In, attapulgite carrier, expanding agent and active component need to be sufficiently mixed stirring 5 ~ 15min.
10. a preparation method for biodiesel solid decolorizer, comprises the following steps:
(1) take 600 ~ 1200g attapulgite, add and carry out pure relative to the sodium hexameta phosphate of attapulgite mass fraction 1% ~ 5%
Change processes, and is that 1:5 addition mineral acid carries out acidification to purification attapulgite according to solid-liquid mass volume ratio, uses deionization
Water washs 3 ~ 4 times, until supernatant is neutral, is centrifuged off supernatant, is put into by solid sediment in baking oven and be dried completely；
(2) taking acidifying attapulgite 500 ~ 1000g that acidification obtains, addition relative to acidifying attapulgite mass fraction is
The expanding agent of 1% ~ 2% and be the active component of 3% ~ 8% relative to acidifying attapulgite mass fraction, uses stirring rod that it is abundant
5 ~ 15min is standby in mixing；
(3) addition accounts for the binding agent that mixture quality mark is 1% ~ 5%, mixing granulation in wet granulator, and obtaining particle diameter is 2
The solid particle of ~ 5mm；Described mixture is formed by being acidified attapulgite, active component and expanding agent；
(4), after above-mentioned solid particle is put into drying baker drying 12 ~ 24h, 200 ~ 600 DEG C of roasting 2 ~ 5h in Muffle furnace are sent into,
Obtain biodiesel solid decolorizer.
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Cited By (2)
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| CN108179060A (en) * | 2018-01-07 | 2018-06-19 | 南京审计大学 | A kind of grease efficient decolorizing composition and its application |
| CN114749191A (en) * | 2022-03-24 | 2022-07-15 | 淮阴工学院 | Ni/P-attapulgite clay catalyst and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108179060A (en) * | 2018-01-07 | 2018-06-19 | 南京审计大学 | A kind of grease efficient decolorizing composition and its application |
| CN114749191A (en) * | 2022-03-24 | 2022-07-15 | 淮阴工学院 | Ni/P-attapulgite clay catalyst and preparation method and application thereof |
| CN114749191B (en) * | 2022-03-24 | 2023-06-30 | 淮阴工学院 | Ni/P-attapulgite clay catalyst and preparation method and application thereof |
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Application publication date: 20161130 |