CN112156760A - Method for decolorizing rapeseed oil by using composite diatomite - Google Patents
Method for decolorizing rapeseed oil by using composite diatomite Download PDFInfo
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- CN112156760A CN112156760A CN202011014229.2A CN202011014229A CN112156760A CN 112156760 A CN112156760 A CN 112156760A CN 202011014229 A CN202011014229 A CN 202011014229A CN 112156760 A CN112156760 A CN 112156760A
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- diatomite
- rapeseed oil
- decoloring
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- composite
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 138
- 239000002131 composite material Substances 0.000 title claims abstract description 55
- 235000019484 Rapeseed oil Nutrition 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 23
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 50
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- 239000000203 mixture Substances 0.000 claims abstract description 32
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- 239000000843 powder Substances 0.000 claims abstract description 6
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- 238000004042 decolorization Methods 0.000 claims description 9
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 5
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- OENHQHLEOONYIE-JLTXGRSLSA-N β-Carotene Chemical compound CC=1CCCC(C)(C)C=1\C=C\C(\C)=C\C=C\C(\C)=C\C=C\C=C(/C)\C=C\C=C(/C)\C=C\C1=C(C)CCCC1(C)C OENHQHLEOONYIE-JLTXGRSLSA-N 0.000 abstract description 12
- 238000001179 sorption measurement Methods 0.000 description 16
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- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
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- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
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- 240000002791 Brassica napus Species 0.000 description 1
- 235000004977 Brassica sinapistrum Nutrition 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- OYHQOLUKZRVURQ-HZJYTTRNSA-N Linoleic acid Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(O)=O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 108010009736 Protein Hydrolysates Proteins 0.000 description 1
- 229910002800 Si–O–Al Inorganic materials 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 229930003427 Vitamin E Natural products 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
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- 239000008394 flocculating agent Substances 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- WIGCFUFOHFEKBI-UHFFFAOYSA-N gamma-tocopherol Natural products CC(C)CCCC(C)CCCC(C)CCCC1CCC2C(C)C(O)C(C)C(C)C2O1 WIGCFUFOHFEKBI-UHFFFAOYSA-N 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
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- 229910052742 iron Inorganic materials 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical group O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 229910052622 kaolinite Inorganic materials 0.000 description 1
- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 description 1
- 235000020778 linoleic acid Nutrition 0.000 description 1
- 238000000622 liquid--liquid extraction Methods 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
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- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
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- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 235000021313 oleic acid Nutrition 0.000 description 1
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
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- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
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- 238000007670 refining Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
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- CCEKAJIANROZEO-UHFFFAOYSA-N sulfluramid Chemical group CCNS(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F CCEKAJIANROZEO-UHFFFAOYSA-N 0.000 description 1
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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
- B01J20/14—Diatomaceous 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
- B01J20/22—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
- C11B3/10—Refining fats or fatty oils by adsorption
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Microbiology (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Fats And Perfumes (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a method for decoloring rapeseed oil by using composite diatomite, which comprises the following steps: (1) adding diatomite, a modifier, water and a pickling agent sulfuric acid into a container, wherein the concentration of the sulfuric acid is 20% -30%, heating and stirring the mixture in a water bath in a constant-temperature magnetic stirring pot for 0.5-1 h at the temperature of 50-60 ℃, repeatedly washing the mixture with distilled water until the pH value is 5-6, performing suction filtration, aging the mixture with absolute ethyl alcohol for 24h, drying the mixture in a dryer for 24h, and grinding the dried mixture into powder to obtain composite diatomite; (2) adding composite diatomite into the rapeseed oil, wherein the adding amount of the diatomite is 1-3% of the oil amount of the rapeseed oil, and decoloring for 10-20 min at a decoloring temperature of 60-70 ℃; compared with the original soil, the modified diatomite has the advantages that the removal rate of the pigment in the rapeseed oil is increased by more than 2 times, the removal rate of the beta-carotene is increased by nearly 2 times, and the composite diatomite can be effectively applied to the removal of the natural pigment in the rapeseed oil.
Description
Technical Field
The invention relates to a method for decoloring rapeseed oil by using composite diatomite, which is used for decoloring the rapeseed oil.
Background
Almost 20 countries in the world have diatomite ore, China has abundant diatomite resources, the amount of the diatomite resources exceeds 20 hundred million tons, 354 mining areas for detecting the resource amount have 3.85 hundred million tons of total reserves, and the second place in the world is located after the United states. The domestic diatomite deposit types mainly include volcano source sedimentary deposit and land source sedimentary deposit. The mineral component of diatomaceous earth is mainly opal and its variants, clay mineral-hydrate, kaolinite and mineral fragments are less abundant. The main chemical component of the diatomite is SiO2,SiO2SiO, one of the indicators of the quality of diatomite ore2High content of SiO, the quality of the product is excellent2Usually more than 80 percent, and the high-quality diatomite contains SiO2Over 87%, and further contains Al2O3,Fe2O3And minor amounts of calcium, magnesium, sodium and potassium compounds. The diatomite is mostly white, gray, off-white, light grayish brown and the like, has a unique ordered layered microporous structure, has special physical properties such as fineness, looseness, light weight, more pores, large pore volume, large specific surface area, low heat conductivity, strong permeability and the like due to the special structure, and can absorb impurities by 3-4 times of the weight of the diatomite. Therefore, siliconThe diatomite is widely applied to the industries of light industry, food, chemical industry, medicine, sanitation and the like.
Diatomite is an important adsorption treatment material, can effectively adsorb and fix impurities such as pigments or metal ions in water, yellow wine, beverages and grease, has the advantages of rich sources, low price, easy regeneration, porous structure, numerous active groups, large specific surface area and the like, and is often used as an adsorption treatment material in various fields such as light industry, food, chemical industry and the like. However, as the surface of the natural diatomite is densely distributed with micropores, and some of the pores are often covered by impurities, the adsorption sites are blocked, and ions in the solution are difficult to enter the diatomite pores, so that the adsorption capacity is reduced to a certain extent, and the adsorption effect is influenced. Therefore, it is necessary to modify diatomaceous earth to improve its adsorption properties. At present, the common modification method for diatomite at home and abroad generally comprises the following steps: conventional modification, such as acid washing and roasting; inorganic modification, such as modification of diatomite with metal ions with positive charges such as iron, aluminum, calcium and the like or a flocculating agent; the organic modification is the modification of diatomite by using different macromolecular organic substances (such as surfactants).
Based on the characteristics of strong adsorption capacity of diatomite, capability of adsorbing inorganic ions, toxic substances and organic pollutants without generating harmful substances, the diatomite is widely applied to the aspects of food processing such as clarification of beverages and wines, decoloration of grains and oils and the like as a high-quality low-price environment-friendly material. In addition, blueberry juice is taken as a raw material by Wangfang, Dengqi and the like, diatomite-gelatin is taken as a composite clarifier, the clarifying effect of the composite clarifier on the blueberry juice is researched, and the result shows that: under the optimized conditions that the proportion of the composite clarifying agent is 2:1, the water bath temperature is 50 ℃ and the water bath time is 50min, the light transmittance of the blueberry juice is improved by 37.80 percent compared with that of the juice without clarification, which shows that the composite clarifying agent can effectively clarify the blueberry juice. The influence of diatomite on the clarity and components of yellow wine by Liuge, Pengyi and the like is researched, and the result shows that: the diatomite can effectively assist in clarifying the yellow wine. Jinweili, Zhengguo and the like use rice residues as raw materials, diatomite as a decoloring agent and diatomite to optimize and research the decoloring process of rice residue protein enzymatic hydrolysate, and the results show that: the removal rate was 81.8% in the case where the amount of diatomaceous earth used was 1.6g, the decoloring time was 25min, the decoloring pH was 6.0, and the decoloring temperature was 60 ℃.
The research on the vegetable oil decolorization is developed to remove the pigment in the vegetable oil, which is a crucial link in the vegetable oil refining process, and the good and bad decolorization effect directly influences the quality of the oil and the market sale condition of the oil, which is a problem continuously paid attention by vegetable oil manufacturers. The purpose of decolorization is to remove pigments, trace metals, colloids, pesticide residues and other impurities. The decoloring method mainly comprises liquid-liquid extraction, adsorbent, reduction, heating oxidation, ion exchange and the like, and the decoloring method is mainly industrially adopted for decoloring the vegetable oil by utilizing the adsorption effect of the adsorbent, and the characteristic of the vegetable oil, the decoloring process and the process condition influence the adsorption characteristic of the adsorbent. The factors influencing adsorption and decoloration are many, such as decoloration temperature, decoloration time, addition amount of an adsorbent and the like, and Zhang Yuan weight, the southern wild goose finds in a test of the tea oil decoloration process that the added white soil amount and the decoloration temperature are the most significant factors influencing the tea oil decoloration process, the decoloration time is a secondary condition, and the optimized process parameters are as follows: the content of the added clay is 6 percent, the decoloring temperature is 110 ℃, the decoloring time is 15min, and under the condition, the tea oil observed by naked eyes is nearly colorless and reaches the use standard.
Vegetable oil is an indispensable substance in human life, wherein the rapeseed oil contains abundant unsaturated fatty acids such as oleic acid and linoleic acid and vitamin E, which can soften blood vessels and delay aging, and the rapeseed oil has low cholesterol, so people controlling the intake of cholesterol can eat the rapeseed oil with confidence. However, the rapeseed oil has quite complex components, and contains various pigments, such as chlorophyll, beta-carotene, trace metals, soap granules, colloid, residual pesticides and other organic substances and other impurities, which not only affects the sense of the rapeseed oil, but also seriously harms the health of people. With the gradual improvement of the living standard of people, the requirements on the quality, the purity and the taste of the vegetable oil are higher and higher, so that the vegetable oil is required to be subjected to impurity removal, pigment removal and deodorization, and the shelf life of the finished oil is prolonged.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for decoloring rapeseed oil by using composite diatomite, which is effectively applied to the removal of natural pigments in the rapeseed oil.
In order to solve the technical problem, the method for decoloring the rapeseed oil by using the composite diatomite comprises the following steps:
(1) adding kieselguhr, a modifier, water and pickling agent sulfuric acid into a container, wherein the mass ratio of the kieselguhr to the modifier to the water to the pickling agent sulfuric acid is (8-15): 0.3-1.4:90-110: 3-7, heating and stirring the mixture in a water bath in a constant-temperature magnetic stirring pot for 0.5-1 h at the temperature of 50-60 ℃, repeatedly washing the mixture with distilled water until the pH value is 5-6, performing suction filtration, aging and standing the mixture with absolute ethyl alcohol, drying the mixture in a dryer, and grinding the dried mixture into powder to obtain the composite diatomite.
After the diatomite is subjected to sulfuric acid pickling, with the increase of the concentration of sulfuric acid, iron oxide, aluminum oxide, magnesium oxide and other components in the diatomite react with the sulfuric acid to generate soluble salts, the impurity content in the diatomite can be obviously reduced, and the SiO of the diatomite is improved2. However, when the concentration of sulfuric acid is too high (more than 30%), the diatomite is dissolved in a large area at the edge and incomplete, so that the structure of the diatomite is damaged, and SiO in the diatomite is generated2And (4) descending.
Preferably, the modifier consists of cetyltrimethylammonium bromide and a silane coupling agent.
When stirring, the concentrated sulfuric acid and the components in the diatomite react faster along with the increase of the stirring temperature to generate more soluble salts, so that SiO in the diatomite is generated2The content is increased, but the stirring temperature is over 60 ℃, which can cause the instability of the layered structure of the diatomite and further cause the structural damage, so that the SiO of the diatomite is ensured2The content is reduced, so the stirring temperature is selected to be 50-60 ℃.
With the increase of the stirring time, the concentrated sulfuric acid and the components in the diatomite react faster to generate more soluble salts, so that SiO in the diatomite is generated2The content increases, but too long stirring (more than 1 hour) will lead to siliconStructural destruction of diatomaceous earth to SiO2The content is reduced.
To improve SiO content of diatomite2The concentration of the sulfuric acid is preferably 25%, the stirring temperature is preferably 60 ℃, and the stirring time is preferably 1 h.
(2) Adding composite diatomite into the rapeseed oil, wherein the addition amount of the composite diatomite is 1-3% of the oil amount of the rapeseed oil, and decoloring for 10-20 min at a decoloring temperature of 60-70 ℃.
With the increase of the adding amount of the composite diatomite, the diatomite adsorbs more pigments in the rapeseed oil, the pigment removal rate is further increased, and when the adding amount of the composite diatomite exceeds 3% of the oil amount of the rapeseed oil, the adsorption of the pigments is in a saturated state, so that the removal rate is reduced. With the increase of the decolorizing temperature, the adsorption speed of the pigment and the diatomite is increased, so that the pigment removal rate is further increased, and when the decolorizing temperature is too high (over 70 ℃), the structure of the composite diatomite is damaged, the adsorption performance of the diatomite is further damaged, and the pigment removal rate is reduced.
With the prolonging of the decoloring time, the adsorption of the pigment and the diatomite is accelerated, so that the pigment removal rate is further improved, when the decoloring time is too long (more than 20min), the adsorption of the pigment by the diatomite is in a saturated state, and the adsorption balance is destroyed after the further prolonging of the time, so that the removal rate is reduced.
In order to improve the removal rate (mainly the removal rate of beta-carotene and chlorophyll), the addition amount of the composite diatomite is 3 percent of the oil amount of the rapeseed oil, the decoloring temperature is 70 ℃, and the decoloring time is 20 min.
After modification, composite diatomaceous earth (SiO)2The content reaches 79.99 percent), the structure has intermediate states of quinoid structure and benzene structure, and the modifier is attached to the surface of the diatomite. Compared with the original soil, the modified diatomite has the advantages that the removal rate of the pigment in the rapeseed oil is increased by more than 2 times, the removal rate of the beta-carotene is increased by nearly 2 times, and the composite diatomite can be effectively applied to the removal of the natural pigment in the rapeseed oil.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
FIG. 1 is the concentration of sulfuric acid versus SiO2Influence of the content.
FIG. 2 is a graph of stirring temperature versus SiO2Influence of the content.
FIG. 3 is a graph of stirring time versus SiO2Influence of the content.
FIG. 4 is an infrared spectrum of raw soil and composite diatomite.
Fig. 5 is a graph showing the effect of raw soil and composite diatomite on the removal rate of chlorophyll and beta-carotene from rapeseed oil.
FIG. 6 is a graph showing the effect of the amount of added soil on the removal rate.
FIG. 7 is a graph showing the effect of decoloring temperature on the removal rate.
FIG. 8 is a graph showing the effect of decoloring time on the removal rate.
Detailed Description
The products obtained were determined using the following method:
SiO2measurement of content (%)
Precisely weighing about 0.2000g (sample for determining ignition weight loss) of 550 ℃ calcined diatomite into a crucible with constant weight at the temperature, adding 5mL of hydrofluoric acid and 2 drops of sulfuric acid (1: 2), slowly evaporating to dryness, and cooling to room temperature; then adding 5mL of hydrofluoric acid, and continuously heating and evaporating to dryness; burning at 550 deg.C, cooling, and weighing to constant weight. The calculation formula is as follows:
in the formula: x-silica content in grams per hundred grams (g/100 g);
W0-crucible mass in grams (g);
W1the total mass of the crucible and the sample before hydrofluoric acid treatment is in grams (g);
W2the total mass of the crucible and the sample after hydrofluoric acid treatment is given in grams (g).
Infrared spectroscopic analysis
Accurately weighing 0.003g of each of dry diatomite and composite diatomite, grinding the dry diatomite and the composite diatomite according to a certain proportion, tabletting the mixture after grinding the mixture with potassium bromide (KBr), and tabletting the mixture at 400-4000cm-1And (4) infrared spectrum scanning is carried out, and the infrared spectrums of the original soil and the composite diatomite are measured.
Measurement of pigment removal (%) ratio
Taking supernatant, respectively measuring absorbances of beta-carotene and chlorophyll at 457nm and 649nm by using a spectrophotometer, calculating removal rate according to the absorbances, and using distilled water as a blank, wherein the formula is as follows:
in the formula: a. the1-absorbance of rapeseed oil before decolorization; a. the2Absorbance of rapeseed oil after decolorization
Example 1
Adding 10g of kieselguhr, a modifier (cetyl trimethyl ammonium bromide and a silane coupling agent KH570) and water into a 250mL beaker, adding a pickling agent sulfuric acid with the concentration of 20%, wherein the mass ratio of the kieselguhr to the modifier to the water to the pickling agent sulfuric acid is 10: 1:100: and 5, heating and stirring the mixture in a water bath in a constant-temperature magnetic stirring kettle for 1 hour at the temperature of 60 ℃, repeatedly washing the mixture with distilled water until the pH value is 5-6, performing suction filtration by using a circulating water type vacuum pump, aging and standing the mixture for 24 hours by using absolute ethyl alcohol, drying the mixture for 24 hours in an electric heating constant-temperature blast drier at the temperature of 70 ℃, and grinding the mixture into powder to obtain the composite diatomite.
Examples 2-5, identical to example 1, except that: the concentration of sulfuric acid is 15%, 20%, 25% and 30% respectively.
SiO for examples 1 to 52The measurement of the content (%) is shown in FIG. 1: sulfuric acid concentration to SiO2The trend line of the concentration (%) shows a tendency of rising first and then falling as a whole, and SiO increases with the increase of the sulfuric acid concentration2The content of the SiO gradually increases, and when the concentration of the sulfuric acid is 25 percent2The content reaches a maximum and then decreases. According to the national standard for the safety of GB 14936-2The content is the largest.
Example 6
Adding 10g of kieselguhr, a modifier (cetyl trimethyl ammonium bromide and a silane coupling agent KH570) and water into a 250mL beaker, adding acid washing agent sulfuric acid with the concentration of 25%, wherein the mass ratio of the kieselguhr to the modifier to the water to the acid washing agent sulfuric acid is 8: 1:100: and 7, heating and stirring the mixture in a water bath in a constant-temperature magnetic stirring kettle for 1 hour at the temperature of 40 ℃, repeatedly washing the mixture with distilled water until the pH value is 5-6, performing suction filtration by using a circulating water type vacuum pump, aging and standing the mixture for 24 hours by using absolute ethyl alcohol, drying the mixture for 24 hours in an electric heating constant-temperature blast drier at the temperature of 70 ℃, and grinding the dried mixture into powder to obtain the composite diatomite.
Examples 7-10, identical to example 6, except that: the stirring temperature is 50 ℃, 60 ℃, 70 ℃ and 80 ℃ in sequence.
SiO for examples 6 to 102The measurement of the content (%) is shown in FIG. 2: stirring temperature to SiO2Influence of the content, SiO with increasing stirring temperature2The content curve as a whole shows a tendency of rising first and then falling, and SiO is generated along with the rise of the stirring temperature2The content of SiO gradually increases when the stirring temperature is 60 DEG C2The content reaches the maximum.
Example 11
Adding 10g of kieselguhr, a modifier (cetyl trimethyl ammonium bromide and a silane coupling agent KH570) and water into a 250mL beaker, adding 30% of pickling agent sulfuric acid, wherein the mass ratio of the kieselguhr to the modifier to the water to the pickling agent sulfuric acid is 15: 1:100: and 3, heating and stirring the mixture in a water bath in a constant-temperature magnetic stirring kettle for 0.5h at the temperature of 60 ℃, repeatedly washing the mixture with distilled water until the pH value is 5-6, performing suction filtration by using a circulating water type vacuum pump, aging and standing the mixture for 24h by using absolute ethyl alcohol, drying the mixture for 24h at the temperature of 70 ℃ in an electric heating constant-temperature air blast dryer, and grinding the mixture to powder to obtain the composite diatomite.
Examples 12-15, identical to example 11, except that: the stirring time is 1h, 1.5h, 2h and 2.5h in sequence.
SiO for examples 11 to 152The measurement of the content (%) is shown in FIG. 3:stirring time for SiO2Influence of the content, SiO with increasing stirring time2The content shows a tendency to rise first and then fall and then to flatten. When the stirring time is 1h, SiO2The content reaches the maximum. According to the national standard for the safety of the GB 14936-2The content is minimum, which indicates that the diatomite is modified best when the stirring time is 1 h.
The infrared spectrum analysis of the composite diatomaceous earth obtained in example 12 and conventional diatomaceous earth was performed, and in fig. 4, (a) is the infrared spectrum of raw diatomaceous earth, and (b) is the infrared spectrum of composite diatomaceous earth. The bending vibration absorption peak of O-H is 1630cm-1Here, Si-O-Si bonds contained in diatomaceous earth have been caused at 468 and 1096cm-1The peak of absorption of stretching vibration. At 531 and 792cm-1The absorption peak of the stretching vibration is due to Si-O-Al bond in impurity components of clay in the diatomite, and the absorption peaks of the modified composite diatomite are weakened. (b) Upper 1200cm-1And 1100cm-1The C-N stretching vibration peaks of the benzene structure and the quinoid structure are shown respectively, which shows that after the modification, the composite diatomite structure has intermediate states of the quinoid structure and the benzene structure, and the modifier is attached to the surface of the diatomite.
The composite diatomaceous earth obtained in example 12 was subjected to measurement of pigment removal (%) with conventional diatomaceous earth: as can be seen from the figure 5, the removal effect of the modified composite diatomite on the beta-carotene and the chlorophyll in the rapeseed oil is improved. The removal effect of the composite diatomite on the beta-carotene is more obvious, and compared with the original diatomite, the removal rate of the composite diatomite on the beta-carotene is increased by more than 2 times; the removal rate of chlorophyll by the composite diatomite is increased by nearly 2 times compared with that of the original diatomite, which shows that the composite diatomite can be effectively applied to rapeseed oil pigment removal.
Example 16
In a 100mL colorimetric bottle, the composite diatomite obtained in example 12 was added to rapeseed oil in an amount of 1% of the oil content, and the mixture was heated in a water bath at 70 ℃ for 20 min.
Examples 17-20, identical to example 16, except that: the addition amount of the diatomite is 2%, 3%, 4% and 5% of the oil amount of the rapeseed respectively.
The removal rates (%) of the pigments in examples 16 to 20 were measured, and as can be seen from FIG. 6, the curves of the removal rates of β -carotene were relatively flat as a whole in the trend lines of the influence of the addition amount of clay (composite diatomaceous earth) on the removal rates, indicating that the influence of the addition amount of clay on the removal rates was small and the removal rate was the highest when the addition amount of clay was 3%; with the increase of the soil addition amount, the chlorophyll removal rate tends to increase first and then decrease, and the removal rate is highest when the soil addition amount is 3%. Therefore, the most suitable soil addition amount is 3%.
Example 21
In a 100mL colorimetric bottle, the composite diatomite obtained in example 12 was added to rapeseed oil in an amount of 3% of the oil content, and the mixture was heated in a water bath at 50 ℃ for 20 min.
Examples 22-25, the same as example 21, except that: the decolorizing temperature is 60 deg.C, 70 deg.C, 80 deg.C, and 90 deg.C, respectively.
In examples 21 to 25, the removal rate (%) of the pigment was measured, and as can be seen from FIG. 7, the removal rate curve of β -carotene tended to increase and decrease with the increase of the amount of soil added in the trend of the influence of the decoloring temperature on the removal rate, and the removal rate was the highest at the decoloring temperature of 70 ℃; the chlorophyll removal rate curve is in a trend of firstly rising, then being gentle and then falling, and the removal rate is higher when the decolorizing temperature is 70-80 ℃. Therefore, the optimum decolorization temperature is 70 ℃ in combination with the above analysis.
Example 26
In a 100mL colorimetric bottle, the composite diatomite obtained in example 12 was added to rapeseed oil in an amount of 3% of the oil content, and the mixture was heated in a water bath at 70 ℃ for 10 min.
Examples 27-30, identical to example 17, except that: the decolorizing time is 20min, 30min, 40min, and 50min respectively.
In examples 26 to 30, the removal rates (%) of the pigments were measured, and as can be seen from fig. 8, the removal rate trend lines for β -carotene and chlorophyll tended to increase and decrease with increasing soil addition in the removal rate trend lines for the decoloring time, and the removal rate was the highest at 20min, and the removal rate was slightly better than the removal rate for chlorophyll. Therefore, the optimum decolorization time is 20 min.
The above embodiments do not limit the present invention in any way, and all technical solutions obtained by means of equivalent substitution or equivalent transformation fall within the protection scope of the present invention.
Claims (8)
1. The method for decoloring rapeseed oil by using composite diatomite is characterized by comprising the following steps:
(1) adding kieselguhr, a modifier, water and pickling agent sulfuric acid into a container, wherein the mass ratio of the kieselguhr to the modifier to the water to the pickling agent sulfuric acid is (8-15): 0.3-1.4:90-110: 3-7, heating and stirring the mixture in a water bath in a constant-temperature magnetic stirring pot for 0.5-1 h at the temperature of 50-60 ℃, repeatedly washing the mixture with distilled water until the pH value is 5-6, performing suction filtration, aging and standing the mixture with absolute ethyl alcohol, drying the mixture in a dryer, and grinding the dried mixture into powder to obtain the composite diatomite;
(2) adding composite diatomite into the rapeseed oil, wherein the adding amount of the diatomite is 1-3% of the oil amount of the rapeseed oil, and decoloring for 10-20 min at a decoloring temperature of 60-70 ℃.
2. The method for decoloring rapeseed oil by using composite diatomite according to claim 1, characterized in that: the modifier consists of hexadecyl trimethyl ammonium bromide and a silane coupling agent.
3. The method for decoloring rapeseed oil by using composite diatomite according to claim 1, characterized in that: the concentration of the sulfuric acid is 25%.
4. The method for decoloring rapeseed oil by using composite diatomite according to claim 1, characterized in that: the temperature during stirring was 60 ℃.
5. The method for decoloring rapeseed oil by using composite diatomite according to claim 1, characterized in that: the stirring time is 1 h.
6. The method for decoloring rapeseed oil by using composite diatomite according to claim 1, characterized in that: the addition amount of the composite diatomite is 3% of the amount of the rapeseed oil.
7. The method for decoloring rapeseed oil by using composite diatomite according to claim 1, characterized in that: the decolorization temperature was 70 ℃.
8. The method for decoloring rapeseed oil by using composite diatomite according to claim 1, characterized in that: the decolorization time is 20 min.
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