CN104525101B - Preparation method for the attapulgite soil matrix adsorption decolouriser of soybean oil refine - Google Patents

Preparation method for the attapulgite soil matrix adsorption decolouriser of soybean oil refine Download PDF

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CN104525101B
CN104525101B CN201410678549.6A CN201410678549A CN104525101B CN 104525101 B CN104525101 B CN 104525101B CN 201410678549 A CN201410678549 A CN 201410678549A CN 104525101 B CN104525101 B CN 104525101B
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attapulgite
acid
soil matrix
calx
adsorption decolouriser
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CN104525101A (en
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陈新德
张海荣
罗军
吴伟
熊莲
黄超
郭海军
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Jiangsu Autobang International Co ltd
Guangzhou Institute of Energy Conversion of CAS
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Jiangsu Autobang International Co ltd
Guangzhou Institute of Energy Conversion of CAS
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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
    • 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
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • 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
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Dispersion Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Microbiology (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Fats And Perfumes (AREA)

Abstract

The invention discloses the preparation method of a kind of attapulgite soil matrix adsorption decolouriser for soybean oil refine, first attapulgite raw ore is carried out acid activation, calcination activation, pulverizing, it is subsequently adding lewis acid and a small amount of Calx mix homogeneously, sieves and obtain absorption property preferable attapulgite soil matrix adsorption decolouriser.Attapulgite soil matrix adsorption decolouriser prepared by the present invention has features such as can be easily separated, decolorizing efficiency is high, consumption is few, pollution-free, etching apparatus, product postprocessing be not easy with product.

Description

Preparation method for the attapulgite soil matrix adsorption decolouriser of soybean oil refine
Technical field
The present invention relates to the preparation method of a kind of attapulgite soil matrix adsorption decolouriser for soybean oil refine, belong to concavo-convex What rod was native utilizes technical field.
Background technology
Soybean oil is a kind of Vegetable oil lipoprotein produced by soybean seed milling process or solvent extraction method, is that yield is most in the world Oils and fats.Oils and fats, after degumming and neutralizing, still contains some materials not accepted by people, such as phospholipid, soaps, trace Metal, carotenoid, phylloxanthin, chlorophyll etc..The existence of these impurity affects Semen sojae atricolor cast of oil and quality, needs it Carry out refine to remove these impurity.
The method of grease-decolor is a lot, but industrial be most widely used is adsorption decoloring method.Conventional adsorbent has Activated carbon and active hargil etc..The price of activated carbon is higher, and the decolouring being applied to oils and fats is subject to certain restrictions.At present, oils and fats Decolorising agent mainly based on active hargil, have clay property ore deposit soil, such as bentonite, attapulgite clay (attapulgite Soil), kaolinite clay, meerschaum clay etc., all can commonly use bentonite at present as activity as the raw material of active hargil The raw material of hargil.But compared with other clay particularly attapulgite clay, bentonitic price is of a relatively high.
Attapulgite is a kind of natural nano inorganic matter with special layers chain structure, has bigger specific surface area, Adsorptivity is strong.Attapulgite has higher heat stability and stronger anti-salt property, and decoloring ability is strong, and absorbability is good, tool Have percent of decolourization high, without plurality of advantages such as residual acids, there is the good reputation of " kings of thousand soil ".Attapulgite itself has certain L Acid site and B-acid center, by modified, can strengthen the acidity of attapulgite, improves itself and free fatty, waxiness, pigment Deng the binding ability of impurity, it is thus possible to the impurity such as the pigment in absorption oils and fats effectively, be a kind of excellent performance adsorbent and Decolorising agent.As Chinese invention patent CN 101497026 B discloses a kind of attapulgite soil matrix for producing injection soybean oil Decolorising agent.Chinese invention patent CN 103055802A discloses one and has the decolouring of antioxygenic property attapulgite clay palm oil The preparation method of agent.
Summary of the invention
It is an object of the invention to: the preparation side of a kind of attapulgite soil matrix adsorption decolouriser for soybean oil refine is provided Method, the attapulgite soil matrix adsorption decolouriser prepared by the present invention has reaction condition gentleness, corrosivity when soybean oil refines The features such as little, pollution-free, decolorizing efficiency is high, consumption few and product can be easily separated, product postprocessing simplicity.
The technical solution of the present invention is: first attapulgite raw ore is carried out acid activation, calcination activation, pulverizing, then Add lewis acid and a small amount of Calx mix homogeneously, sieve, obtain attapulgite soil matrix adsorption decolouriser.
Wherein, described activation step is by 5 ~ 10 weight portion attapulgite raw ores, 1 ~ 5 weight portion acid and 15 ~ 50 weights Amount part water mixing, stirs 0.5 ~ 12 h in 30 ~ 90 DEG C of constant temperature.
Wherein, described acid is the one in sulphuric acid, hydrochloric acid, phosphoric acid, formic acid and acetic acid.
Wherein, described sintering temperature is 80 ~ 400 DEG C, and roasting time is 1 h ~ 24 h.
Wherein, after roasting, the hybrid mode of attapulgite and lewis acid, Calx is to grind or through bipyramid, V-Mixer Mixing.
Wherein, described Lewis acid is MgCl2、AlCl3、FeCl3In one or both, described Lewis acid mass fraction For attapulgite raw ore 1% ~ 20.0%.
Wherein, described Calx is quick lime or Calx, and the mass fraction of described Calx is attapulgite raw ore 0.1% ~ 5.0%.
Wherein, after sieving, attapulgite soil matrix adsorption decolouriser mesh number is 150 ~ 200 mesh.
The present invention compared with prior art, has the advantage that
(1) formation of the structural hydroxyl group in attapulgite Rotating fields Bronst acid site, and the Al exposed3+Ion then shape Become Lewis acid site, further enhance the BSuan HuoLSuan center of attapulgite by adding Lewis acid, improve adsorbent with The binding ability of the impurity such as free fatty, waxiness, pigment, thus improve the decoloration performance of decolorising agent.
(2) being filled with carbonate cement between crystal and in natural duct in natural attapulgite, absorbability is more weak, After acid activation processes, carbonate cement dissolution in attapulgite duct, duct is dredged；Meanwhile, radius is less Hydrion displace the metal ion in attapulgite interlayer portion, thus increase pore volume, thus improve its specific surface Long-pending, absorption property and ion-exchange capacity there are is facilitation, beneficially the impurity component in soybean oil is to the brilliant diffusion inside of rod, Prevent mutually bonding between impurity to form the jelly plastid of densification, reduce filtration resistance, at the most follow-up filtration Reason；Furthermore, after calcination process, further increase specific surface area and the pore volume of attapulgite.
(3) by adding the acidic materials produced in a certain amount of Calx and in decolorization, thus soybean oil is being taken off The acid in oil is removed while color, cost-effective.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but protection scope of the present invention is not limited in This.
Embodiment 1:5 kg attapulgite raw ore, 1 kg sulphuric acid and the mixing of 20 L water, at 80 DEG C, constant temperature stirs 120 min Rear solid-liquid centrifugation separates, and it is interior in 400 DEG C of calcination activation 1 h that rotary kiln sent into by filter cake, obtains roasting attapulgite；After roasting Attapulgite proceeds in ball mill, adds MgCl2 50 g and quick lime 5 g, stir, mixture are crossed 200 mesh sieves, obtain recessed Convex rod soil matrix adsorption decolouriser.
Weigh dry in 105 DEG C ± 3 DEG C attapulgite soil matrix adsorption decolouriser 0.4g, add fresh soyabean oil 40 g , filter after stirring decolouring 25min at 115 DEG C, obtain refined soybean oil.The percent of decolourization of this attapulgite soil matrix adsorption decolouriser is 98.9%。
Embodiment 2: 10 kg attapulgite raw ores, 3 kg hydrochloric acid and 40 L water are mixed, constant temperature stirring 60 at 60 DEG C After min, solid-liquid centrifugation separates, and it is interior in 80 DEG C of calcination activation 10 h that rotary kiln sent into by filter cake, obtains roasting attapulgite；By roasting After attapulgite proceed in V-Mixer, add AlCl3 2 kg and Calx 500 g, stir, mixture are crossed 150 Mesh sieve, obtains attapulgite soil matrix adsorption decolouriser.
Weigh dry in 105 DEG C ± 3 DEG C attapulgite soil matrix adsorption decolouriser 0.2g, add fresh soyabean oil 40 g , filter after stirring decolouring 25min at 115 DEG C, obtain refined soybean oil.The percent of decolourization of this attapulgite soil matrix adsorption decolouriser is 91.2%。
Embodiment 3: 10 kg attapulgite raw ores, 2 kg phosphoric acid and 50 L water are mixed, constant temperature stirring 180 at 90 DEG C After after min, solid-liquid centrifugation separates, and it is interior in 180 DEG C of calcination activation 4 h that rotary kiln sent into by filter cake, obtains roasting attapulgite；Will roasting Attapulgite after burning proceeds in double-cone mixer, adds MgCl2 0.3g、AlCl3 0.2g kg and quick lime 50 g, stirring is all Even, mixture is crossed 180 mesh sieves, obtains attapulgite soil matrix adsorption decolouriser.
Weigh dry in 105 DEG C ± 3 DEG C attapulgite soil matrix adsorption decolouriser 0.2g, add fresh soyabean oil 40 g , filter after stirring decolouring 25min at 115 DEG C, obtain refined soybean oil.The percent of decolourization of this attapulgite soil matrix adsorption decolouriser is 90.5%。
Embodiment 4: 10 kg attapulgite raw ores, 4 kg formic acid and 30 L water are mixed, constant temperature stirring 120 at 80 DEG C After min, solid-liquid centrifugation separates, and it is interior in 200 DEG C of calcination activation 6 h that rotary kiln sent into by filter cake, obtains roasting attapulgite；By roasting After attapulgite proceed in ball mill, add AlCl3, 0.1 kg and quick lime 100 g, stir, mixture crossed 200 Mesh sieve, obtains attapulgite soil matrix adsorption decolouriser.
Weigh dry in 105 DEG C ± 3 DEG C attapulgite soil matrix adsorption decolouriser 0.2g, add fresh soyabean oil 40 g , filter after stirring decolouring 25min at 115 DEG C, obtain refined soybean oil.The percent of decolourization of this attapulgite soil matrix adsorption decolouriser is 94.7%。
Embodiment 5: 6 kg attapulgite raw ores, 1.5 kg acetic acid and 30 L water are mixed, constant temperature stirring 90 at 70 DEG C After min, solid-liquid centrifugation separates, and it is interior in 250 DEG C of calcination activation 16 h that rotary kiln sent into by filter cake, obtains roasting attapulgite；By roasting After attapulgite proceed in ball mill, add FeCl3 0.8 kg and quick lime 200 g, stirs, mixture is crossed 200 Mesh sieve, obtains attapulgite soil matrix adsorption decolouriser.
Weigh dry in 105 DEG C ± 3 DEG C attapulgite soil matrix adsorption decolouriser 0.2g, add fresh soyabean oil 40 g , filter after stirring decolouring 25min at 115 DEG C, obtain refined soybean oil.The percent of decolourization of this attapulgite soil matrix adsorption decolouriser is 90.1%。
Embodiment 6: 8 kg attapulgite raw ores, 3.5 kg sulphuric acid and 45 L water are mixed, constant temperature stirring 60 at 80 DEG C After min, solid-liquid centrifugation separates, and it is interior in 300 DEG C of calcination activation 12 h that rotary kiln sent into by filter cake, obtains roasting attapulgite；By roasting After attapulgite proceed in ball mill, add AlCl3 600g、FeCl3400g and Calx 400 g, stirs, will be mixed Compound crosses 200 mesh sieves, obtains attapulgite soil matrix adsorption decolouriser.
Weigh dry in 105 DEG C ± 3 DEG C attapulgite soil matrix adsorption decolouriser 0.2g, add fresh soyabean oil 40 g , filter after stirring decolouring 25min at 115 DEG C, obtain refined soybean oil.The percent of decolourization of this attapulgite soil matrix adsorption decolouriser is 93.8%。

Claims (1)

1. it is used for the preparation method of the attapulgite soil matrix adsorption decolouriser of soybean oil refine, first attapulgite raw ore is carried out acid and lives Change, calcination activation, pulverizing, be subsequently adding lewis acid and a small amount of Calx mix homogeneously, sieve, and obtains the absorption of attapulgite soil matrix de- Toner；Described activation step is 5 ~ 10 weight portion attapulgite raw ores, 1 ~ 5 weight portion acid and 15 ~ 50 weight parts waters to be mixed Even, stir 0.5 ~ 12 h in 30 ~ 90 DEG C of constant temperature；It is characterized in that: described acid is in sulphuric acid, hydrochloric acid, phosphoric acid, formic acid and acetic acid A kind of；Described sintering temperature is 80 ~ 400 DEG C, and roasting time is 1 h ~ 24 h；Attapulgite and lewis acid, Calx after roasting Hybrid mode for grind or through bipyramid, V-Mixer mixing；Described Lewis acid is MgCl2、AlCl3、FeCl3In one Plant or two kinds, mass fraction is attapulgite raw ore the 1% ~ 20.0% of described Lewis acid；Described Calx is quick lime or ripe Calx, the mass fraction of described Calx is the 0.1% ~ 5.0% of attapulgite raw ore；Attapulgite soil matrix adsorption decolouriser after sieving Mesh number be 150 ~ 200 mesh.
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CN106166475A (en) * 2016-07-27 2016-11-30 南京大学昆山创新研究院 A kind of biodiesel solid decolorizer and preparation method
CN109954477A (en) * 2017-12-26 2019-07-02 金昌红泉膨润土有限责任公司 A kind of atlapulgite acid lowering agent
CN111111608A (en) * 2019-12-27 2020-05-08 泰州医药城国科化物生物医药科技有限公司 Method for selectively removing traditional Chinese medicine notoginseng pigment by adopting silicate minerals
CN112076730A (en) * 2020-09-16 2020-12-15 盐城工学院 Dye wastewater decolorizer and preparation method and application thereof
CN112275262A (en) * 2020-11-16 2021-01-29 中国石油化工股份有限公司 Refinery anhydrous liquid ammonia decolorant and preparation method thereof

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CN101148282A (en) * 2007-08-31 2008-03-26 乐昌市银星化工有限公司 Waste acid modified discoloring agent
CN104028211A (en) * 2014-06-12 2014-09-10 中科院广州能源所盱眙凹土研发中心 Preparation method of attapulgite-based refining agent for lubricant base oil adsorption refining

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CN100574868C (en) * 2006-07-27 2009-12-30 宁守俭 Deacidification adsorbent for oil products and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101148282A (en) * 2007-08-31 2008-03-26 乐昌市银星化工有限公司 Waste acid modified discoloring agent
CN104028211A (en) * 2014-06-12 2014-09-10 中科院广州能源所盱眙凹土研发中心 Preparation method of attapulgite-based refining agent for lubricant base oil adsorption refining

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