CN103525548B - Degumming method for reducing content of chlorine sources and 3-monochlorpropane-1,2-diol ester precusor substances in vegetable oil - Google Patents
Degumming method for reducing content of chlorine sources and 3-monochlorpropane-1,2-diol ester precusor substances in vegetable oil Download PDFInfo
- Publication number
- CN103525548B CN103525548B CN201310545850.5A CN201310545850A CN103525548B CN 103525548 B CN103525548 B CN 103525548B CN 201310545850 A CN201310545850 A CN 201310545850A CN 103525548 B CN103525548 B CN 103525548B
- Authority
- CN
- China
- Prior art keywords
- oil
- content
- vegetable oil
- degumming method
- chlorine
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Fats And Perfumes (AREA)
- Edible Oils And Fats (AREA)
Abstract
The invention discloses a degumming method for reducing the content of chlorine sources and 3-monochlorpropane-1,2-diol ester precusor substances in vegetable oil. The degumming method includes the steps of taking crude vegetable oil as a raw material, conduct heating till the temperature reaches 80 DEG C to 87 DEG C, enabling the heated crude vegetable oil to enter a degumming device, adding 5% to 10% of hot water in a spraying mode under a stirring state, continuing to conduct stirring after water adding is completed, separating a water phase from an oil phase, cooling the oil phase through a heat exchanger till the temperature reaches 40 DEG C to 55 DEG C, adding 0.1% to 1.5% of a neutral absorbent and/or an alkaline absorbent, conducting filtration to remove the neutral absorbent and/or the alkaline absorbent after stirring is conducted, rapidly heating an oil phase obtained through filtration through the heat exchanger till the temperature reaches 90 DEG C to 120 DEG C, conducting dewatering and drying under the vacuum condition, and obtaining degummed vegetable oil with the content of the chlorine sources in the gummed vegetable oil lower than 100mg/kg and the content of the 3-monochlorpropane-1,2-diol ester precusor substances in the gummed vegetable oil lower than 3%. According to the degumming method, the content of the chlorine sources in the degummed vegetable oil and the content of the 3-monochlorpropane-1,2-diol ester precusor substances in the degummed vegetable oil are reduced, and reference is provided for the improvement of an existing vegetable oil refining technology.
Description
Technical field
The present invention relates to reduce the Degumming method in chlorine source and 3-chlorine-1,2-propylene glycol ester precursor substance content in vegetables oil, belong to the vegetable oil and fat refining field of coming unstuck.
Background technology
3-chloro-1,2-propylene glycol ester (3-MCPDE) is 3-chloro-1, the compound that one or two hydroxyl of 2-propylene glycol (3-MCPD) generates with lipid acid generation esterification respectively, there is 3-chloro-1,2-propylene glycol dibasic acid esters, 3-chloro-1, three kinds of 2-propylene glycol-1-monoesters, 3-chlorine-1,2-propylene glycol-2-monoesters, they easily form conventionally in grease and fatty foods hot procedure.3-MCPDE may be hydrolyzed the free 3-MCPD of generation under certain condition in vivo, thereby shows toxicity, and its safety issue has become one of focus of food safety.
In grease, the formation of 3-MCPDE be unable to do without chlorine source and precursor substance.Current viewpoint thinks that the formation of 3-MCPDE is because the chlorine source in fatty foods or its contact material (as chlorine disinfectant tap water or sodium-chlor etc.) (Watkins has occurred to react with grease in grease, C., Chloroesters in foods:an emerging issue.Inform Magazine of the AOCS.2009,4,1-3.).Recently, in hair plam oil and commodity refining plam oil, find organic and inorganic chloride (Craft, B.D., Nagy, K., Sandoz, L., Destaillats, F., Factors impacting the formation of Monochloropropanediol (MCPD) fatty acid diesters during palm (Elaeis guineensis) oil production.Food Addit Contam A.2012,29,354-361.).Inorganic chlorine source potential in plam oil machining chain has: the Repone K of as fertilizer sources composition, ammonium chloride (NG, S.K.:Nutrition and Nutrient Management of the Oil Palm – New Thrust for the Future Perspective, in:Potassium for sustainable crop production.International symposium on role of potassium in India.New Delhi:Potash Research Institute of India, and International Potash Institute Eds.I.Pasricha, B.S.NS, editors.2002, pp.415-429.), as the calcium chloride of the conventional flocculation agent of water treatment, magnesium chloride, iron protochloride and iron(ic) chloride (Nagy, K., Sandoz, L., Craft, B.D., Destaillats, F., Mass-defect filtering of isotope signatures to reveal the source of chlorinated palm oil contaminants.Food additives & contaminants.Part A, Chemistry, analysis, control, exposure & risk assessment.2011, 28, 1492-1500.), investigator infers that these inorganic chlorine sources can obtain enrichment in oil palm process of growth.The people such as Nagy (Nagy, K., Sandoz, L., Craft, B.D., Destaillats, F., Mass-defect filtering of isotope signatures to reveal the source of chlorinated palm oil contaminants.Food additives & contaminants.Part A, Chemistry, analysis, control, exposure & risk assessment.2011, 28, 1492-1500.) filter by the total quality defect of Mass-defect filtering of isotope signatures(isotopic characteristic) detect the natural palm fruit that is present in, chlorine-bearing compound in semi-refined and full refining plam oil, find that most chlorine-bearing compounds just exist in palm fruit, show that chlorine source is before processing just Already in palm fruit, structure and the phytosphingosine of a large amount of organochlorine donors are similar, and inorganic chloride has FeCl
3, FeCl
2, MgCl
2and CaCl
2, wherein FeCl
3and FeCl
2signal is the strongest.The data that provide from above-mentioned document can be reached a conclusion: chlorine source (form with inorganic or organochlorine exists) ubiquity raw plant oil.
At present investigator generally believes that 3-MCPDE in grease forms with there being the amphiphatic micro substance that exists in natural fats and oils and has significant correlation as triglyceride (DAG), monoglyceride (MAG), phosphatide, glycolipid etc., especially DAG and MAG, most investigators are seen as the precursor substance of 3-MCPDE.Under the condition coexisting at chlorine source and precursor substance, can cause the generation of 3-MCPDE at the heat processing section of oil and fat refining.Therefore, the workshop section of coming unstuck of oil and fat refining take content that reasonable process reduces 3-MCPDE precursor substance for whole refinery practice in the minimizing of 3-MCPDE growing amount have vital impact.3-MCPDE precursor substance of the present invention is the summation of DAG and MAG content, and the polarity of these 3-MCPDE precursor substances is greater than the main ingredient triglyceride level (generally account for oil heavy more than 90%) of grease.
Crude oil belongs to colloidal dispersion, and phosphatide, protein, phlegmatic temperament and glycosyl triglyceride etc. wherein, because being called the peptized impurities of grease with sweet three esters compositions sol systems.The existence of peptized impurities not only affects the stability of grease, and affects the technological effect of oil and fat refining and deep processing.For example grease easily forms emulsification in alkali refining process, increases the difficulty of operation, strengthens the consumption of oil and fat refining loss and subsidiary material, and the quality of soap stock is reduced; In decolorization, can increase the consumption of sorbent material, reduce decolorizing effect; The grease not coming unstuck cannot carry out physical refining and deodorization operation, also cannot carry out deep processing.Therefore first, crude oil is refining must remove peptized impurities.
The technological process that Applied Physics, chemistry or physicochemical method remove in crude oil de-solubility impurity is called comes unstuck.The method of coming unstuck has that hydration degum, acid degumming, absorption are come unstuck, hot polymerization comes unstuck and chemical reagent comes unstuck etc., applies most often hydration degum and acid degumming on oil prodution industry.And refining hydration degum and phosphoric acid methods of adopting of food oils come unstuck more, strong acid acid degumming is refining for technical oils.
Hydration degum is the wetting ability of utilizing the peptized impurities such as phosphatide, by aqueous electrolyte liquids such as a certain amount of hot water or diluted alkaline, salt, phosphoric acid, under agitation add in hot crude oil, make peptized impurities water suction cohesion wherein, then a kind of settlement separate fat degumming method.In hydration degum process, can, by the material of flocking settling taking phosphatide as main, also have protein, glycosyl triglyceride, phlegmatic temperament and trace metal ion etc. together with phospholipids incorporate.What the workshop section of coming unstuck of oil and fat refining generally adopted at present is hydration degum (most phosphoric acid of 85% that uses), and in the process of coming unstuck, grease system is in weak acid environment.There are some researches show, in the refining plam oil of 0.1% phosphoric acid degumming, the decolouring of acid activation carclazyte, the content of 3-MCPDE will be higher than the content (Ramli of 3-MCPDE in the refining plam oil of hydration degum, the decolouring of natural discoloring clay, M.R., Siew, W.L., Ibrahim, N.A., Hussein, R., Kuntom, A., Razak, R.A.A., Nesaretnam, K., Effects of Degumming and Bleaching on3-MCPD Esters Formation During Physical Refining.J Am Oil Chem Soc.2011,88,1839-1844.).Also the slightly acidic that is grease system will contribute to the generation of 3-MCPDE in table oil, is because existing degumming technology cannot reduce the generation that the content in chlorine source and 3-MCPDE precursor substance in vegetables oil causes 3-MCPDE in the finished product thereby trace sth. to its source.For reducing the growing amount of 3-MCPDE in the finished product edible vegetable oil, need reduce chlorine source in vegetables oil and the content of 3-MCPDE precursor substance in the first Degumming Procedures of oil and fat refining.
Summary of the invention
The object of this part is to summarize some aspects of embodiments of the invention and briefly introduces some preferred embodiments.In this part and the application's specification digest and denomination of invention, may do a little simplification or omit to avoid the making object of this part, specification digest and denomination of invention fuzzy, and this simplification or omit and can not be used for limiting the scope of the invention.
In view of the problem existing in the above-mentioned and/or existing Degumming method for reducing chlorine source in vegetables oil and 3-chlorine-1,2-propylene glycol ester precursor substance content and application, the present invention is proposed.
Therefore, the object of this invention is to provide a kind of Degumming method for reducing chlorine source in vegetables oil and 3-chlorine-1,2-propylene glycol ester precursor substance content, have higher using value in the deodorization field of oil and fat refining.
For solving the problems of the technologies described above, the invention provides following technical scheme: a kind of for reducing chlorine source and 3-in vegetables oil chloro-1, the Degumming method of 2-propylene glycol ester precursor substance content, taking raw plant oil as raw material, raw plant oil is warming up to 80～87 DEG C via interchanger, then enter in degumming device, under whipped state, add in spray mode the hot water that is equivalent to described raw plant oil mass percent 5～10%, the complete continuation that adds water is stirred, then water phase separated and oil phase, oil phase is cooled to 40～55 DEG C through interchanger, add the neutrality and/or the alkaline adsorbent that are equivalent to described raw plant oil mass percent 0.1～1.5%, after stirring, remove by filter neutrality and/or alkaline adsorbent, oil phase after filtration is warming up to rapidly 90～120 DEG C through interchanger, under vacuum condition, dehydrate, obtain chlorine source content and be less than 100mg/kg, 3-chloro-1, the vegetables oil that comes unstuck that 2-propylene glycol ester precursor substance content is less than 3%.
As a kind of preferred version of Degumming method of the present invention, wherein: describedly add in spray mode the hot water that is equivalent to described raw plant oil mass percent 5～10% under whipped state, the temperature of hot water is 90～95 DEG C.
As a kind of preferred version of Degumming method of the present invention, wherein: described in add water complete continuation stir, its stirring velocity is 8～15 revs/min.
As a kind of preferred version of Degumming method of the present invention, wherein: remove by filter neutrality and/or alkaline adsorbent after described stirring, its stirring velocity is 30～55 revs/min.
As a kind of preferred version of Degumming method of the present invention, wherein: dehydrate the vacuum tightness < 400Pa dehydrating under described vacuum condition.
As a kind of preferred version of Degumming method of the present invention, wherein: described neutrality and/or alkaline adsorbent are one or more in cocoanut active charcoal-attapulgite clay mixture, alkali alumina, Magnesium Silicate q-agent-pure aluminium silicate mixture, neutral alumina and rice hull active carbon.
As a kind of preferred version of Degumming method of the present invention, wherein: described cocoanut active charcoal-attapulgite clay mixture, and by weight, its ratio is cocoanut active charcoal: attapulgite clay=0.3:1～1:1.
Compared with prior art, the invention has the advantages that: reduced the content in chlorine source and 3-chlorine-1,2-propylene glycol ester precursor substance in the vegetables oil that comes unstuck, and provide reference for improving existing vegetable oil fine sweetening process.
Embodiment
For above-mentioned purpose of the present invention, feature and advantage can be become apparent more, below in conjunction with specific embodiment, the specific embodiment of the present invention is described in detail.
A lot of details are set forth in the following description so that fully understand the present invention, but the present invention can also adopt other to be different from alternate manner described here and implement, those skilled in the art can do similar popularization without prejudice to intension of the present invention in the situation that, and therefore the present invention is not subject to the restriction of following public specific embodiment.
Secondly, alleged " embodiment " or " embodiment " refers to special characteristic, structure or the characteristic that can be contained at least one implementation of the present invention herein.Different local in this manual " in one embodiment " that occur not all refer to same embodiment, neither be independent or the embodiment mutually exclusive with other embodiment optionally.
In the present invention, the detection of chlorine source content in vegetables oil:
Chlorine source content in vegetables oil is to weigh with the content of the chlorion in sample after micro-wave digestion.Concrete detection method is as follows:
Take 150g vegetables oil in 500mL pear shape separatory funnel, and add 250mL acetonitrile, fully vibration mixes, then stratification (approximately 1 hour), lower floor's oil phase is emitted and discarded, and upper strata acetonitrile moves into that in 500mL round-bottomed flask, (round-bottomed flask, with front weighing, is designated as m mutually
0g), and clean pear shape separatory funnel inwall with appropriate acetonitrile (about 30mL), the acetonitrile that cleans use is incorporated in 500mL round-bottomed flask, in 55 DEG C, and under vacuum condition, rotary evaporation, (500mL round-bottomed flask thieving paper is dried outer wall, weighs, and is designated as m to volatilize solvent
1g), residue prepares to carry out micro-wave digestion.
Take 100mg(and be equivalent to [0.1 ÷ (m
1-m
0) × 150] g vegetables oil sample) above-mentioned residue puts into TeflonPFA container (volume is 7mL), and adding 0.5mL concentration is the sodium hydroxide solution of 0.5mol/L; 0.5mL water is poured in outside PTEF container, and Teflon PFA container is placed in PTFE reaction vessel, the screw that screws up with a wrench is so that its sealing.A 50mL beaker that water is housed is placed by disk central authorities, then sample is heated to 2min together with beaker under the power of 100-200W; Remove beaker, again sample is heated to 2min; After cooling, in existing partly soluble sample, add the hydrogen peroxide that 100-200 μ L concentration is 30%, hydrogen peroxide and sample vigorous reaction, place until reaction stops.Again sample is sealed in counteracting tank as stated above, in microwave oven, under the power of 200W, heats 2min; Monitor the variation of sample pH value value with pH test paper, making its variation range is 2-4.Then sample solution is crossed to C18 solid-phase extraction column, then used 1.5mL deionized water rinsing, washing lotion is incorporated in sample solution, is settled to 1.5mL respectively after the membrane filtration of 0.5 μ m and 0.2 μ m, prepares to carry out chromatography of ions (IC) analysis.
Ion chromatography condition: select IonpacAS23 separator column (internal diameter 4mm, long 150mm), IonpacAG23 guard column (internal diameter 4mm, long 50mm); Leacheate is the NaCO of 4.5mmol/L
3naHCO with 0.8mmol/L
3mixed aqueous solution, flow velocity 1.0mL/min, sample size 10 μ L, 30 DEG C of column temperatures.
Note: draw the typical curve of chlorion with top grade pure sodium chloride, sample peak area is brought the bent conversion of mark into can draw chloride ion content in sample.
The detection of 3-chlorine-1,2-propylene glycol ester precursor substance content:
Reference " high acid value Rice pollard oil enzyme process esterification deacidification technical study ", Li Lei etc., Chinese oil, the 35th the 10th phase of volume, 34-37 page, 2010 years.
Embodiment 1
Degumming method for reducing chlorine source in vegetables oil and 3-chlorine-1,2-propylene glycol ester precursor substance content:
Taking raw corn oil as raw material, raw corn oil is warming up to 80 DEG C via interchanger, then enter in glue kettle, under 8 revs/min of stirring velocitys, add oil to weigh 5% in spray mode, the water that temperature is 90 DEG C, 5min is stirred in the complete continuation that adds water, then via separating centrifuge water phase separated and oil phase, oil phase is cooled to 40 DEG C through interchanger, add oil and weigh 0.5% cocoanut active charcoal: attapulgite clay=0.3:1(is by weight) cocoanut active charcoal-attapulgite clay mixture, stir 15min under 30 revs/min of speed after, remove by filter cocoanut active charcoal-attapulgite clay mixture, oil phase after filtration is warming up to 90 DEG C through interchanger, be less than in vacuum tightness after dehydrating under the condition of 400Pa and obtain the Semen Maydis oil that comes unstuck that precursor substance content is less than 3%.
Detecting gained chlorine source content is 20mg/kg, and the content of 3-chlorine-1,2-propylene glycol ester precursor substance is 1.5%.
In this embodiment, neutrality and/or alkaline adsorbent are selected cocoanut active charcoal-attapulgite clay mixture.Because the pore texture prosperity of cocoanut active charcoal, be 5 times of common gac, its specific surface area is 1500m
2the general gac specific surface area of/g(is 700m
2/ g), particularly pore structure is unusual, pore diameter be greater than 0.45nm and be less than 2nm micropore account for sum more than 90%.Attapulgite clay refers to a kind of clay mineral taking attapulgite (attapulgite) as main ingredient.Attapulgite is a kind of crystalloid hydrous magnesium aluminium silicate mineral, has unique layer chain-like structure feature, in its structure, has crystal lattice, the Na that contains non-quantitative in side crystal
+, Ca
2+, Fe
3+, Al
3+, crystal is needle-like, fibrous or fiber collection shape; Have unique dispersion, high temperature resistant, the anti-good colloidal property such as saline and alkaline and higher adsorption bleaching ability and have certain plasticity-and cohesive force, its desirable chemical molecular formula is: Mg
5si
8o
20(OH)
2(OH2)
44H
2o.There is the intermediate structure between chain-like structure and laminate structure.The structure of this uniqueness of cocoanut active charcoal and attapulgite clay makes it have special materialization and processing performance, uses it for plant oil degumming workshop section and can reduce significantly the content in chlorine source and 3-chlorine-1,2-propylene glycol ester precursor substance in vegetables oil.
Embodiment 2
Degumming method for reducing chlorine source in vegetables oil and 3-chlorine-1,2-propylene glycol ester precursor substance content:
Taking sunflower seeds crude oil as raw material, sunflower seeds crude oil is warming up to 87 DEG C via interchanger, then enter in glue kettle, under 15 revs/min of stirring velocitys, add oil to weigh 10% in spray mode, the water that temperature is 95 DEG C, 5min is stirred in the complete continuation that adds water, then via separating centrifuge water phase separated and oil phase, oil phase is cooled to 55 DEG C through interchanger, add oil and weigh 1.5% cocoanut active charcoal: attapulgite clay=0.5:1(is by weight) cocoanut active charcoal-attapulgite clay mixture, stir 20min under 55 revs/min of speed after, remove by filter cocoanut active charcoal-attapulgite clay mixture, oil phase after filtration is warming up to 120 DEG C through interchanger, be less than in vacuum tightness after dehydrating under the condition of 400Pa and obtain the sunflower seed oil that comes unstuck that precursor substance content is less than 3%.
Detecting gained chlorine source content is 10mg/kg, and the content of 3-chlorine-1,2-propylene glycol ester precursor substance is 0.1%.
Embodiment 3
Degumming method for reducing chlorine source in vegetables oil and 3-chlorine-1,2-propylene glycol ester precursor substance content:
Taking crude oil of soybean as raw material, crude oil of soybean is warming up to 85 DEG C via interchanger, then enter in glue kettle, under 10 revs/min of stirring velocitys, add oil to weigh 8% in spray mode, the water that temperature is 92 DEG C, 8min is stirred in the complete continuation that adds water, then via separating centrifuge water phase separated and oil phase, oil phase is cooled to 45 DEG C through interchanger, add oil and weigh 0.1% cocoanut active charcoal: attapulgite clay=0.5:1(is by weight) cocoanut active charcoal-attapulgite clay mixture, stir 30min under 45 revs/min of speed after, remove by filter cocoanut active charcoal-attapulgite clay mixture, oil phase after filtration is warming up to 105 DEG C through interchanger, be less than in vacuum tightness after dehydrating under the condition of 400Pa and obtain the soybean oil of coming unstuck that precursor substance content is less than 3%.
Detecting gained chlorine source content is 5mg/kg, and the content of 3-chlorine-1,2-propylene glycol ester precursor substance is 2%.
Embodiment 4
Degumming method for reducing chlorine source in vegetables oil and 3-chlorine-1,2-propylene glycol ester precursor substance content:
Taking crude rapeseed oil as raw material, crude rapeseed oil is warming up to 80 DEG C via interchanger, then enter in glue kettle, under 12 revs/min of stirring velocitys, add oil to weigh 6% in spray mode, the water that temperature is 93 DEG C, 10min is stirred in the complete continuation that adds water, then via separating centrifuge water phase separated and oil phase, oil phase is cooled to 47 DEG C through interchanger, add oil and weigh 0.8% cocoanut active charcoal: attapulgite clay=0.7:1(is by weight) cocoanut active charcoal-attapulgite clay mixture, stir 25min under 35 revs/min of speed after, remove by filter cocoanut active charcoal-attapulgite clay mixture, oil phase after filtration is warming up to 105 DEG C through interchanger, be less than in vacuum tightness after dehydrating under the condition of 400Pa and obtain the rapeseed oil that comes unstuck that precursor substance content is less than 3%.
Detecting gained chlorine source content is 15mg/kg, and the content of 3-chlorine-1,2-propylene glycol ester precursor substance is 1.6%.
Embodiment 5
Degumming method for reducing chlorine source in vegetables oil and 3-chlorine-1,2-propylene glycol ester precursor substance content:
Taking crude peanut oil as raw material, crude peanut oil is warming up to 86 DEG C via interchanger, then enter in glue kettle, under 13 revs/min of stirring velocitys, add oil to weigh 7% in spray mode, the water that temperature is 95 DEG C, 7min is stirred in the complete continuation that adds water, then via separating centrifuge water phase separated and oil phase, oil phase is cooled to 55 DEG C through interchanger, add oil and weigh 1% cocoanut active charcoal: attapulgite clay=0.8:1(is by weight) cocoanut active charcoal-attapulgite clay mixture, stir 20min under 35 revs/min of speed after, remove by filter cocoanut active charcoal-attapulgite clay mixture, oil phase after filtration is warming up to 100 DEG C through interchanger, be less than in vacuum tightness after dehydrating under the condition of 400Pa and obtain the peanut oil that comes unstuck that precursor substance content is less than 3%.
Detecting gained chlorine source content is 30mg/kg, and the content of 3-chlorine-1,2-propylene glycol ester precursor substance is 0.7%.
Embodiment 6
Degumming method for reducing vegetables oil chlorine source and middle 3-chlorine-1,2-propylene glycol ester precursor substance content:
Taking rice bran crude oil as raw material, rice bran hair is warming up to 80 DEG C via interchanger, then enter in glue kettle, under 15 revs/min of stirring velocitys, add oil to weigh 6% in spray mode, the water that temperature is 90 DEG C, 10min is stirred in the complete continuation that adds water, then via separating centrifuge water phase separated and oil phase, oil phase is cooled to 50 DEG C through interchanger, add oil and weigh 1.2% cocoanut active charcoal: attapulgite clay=1:1(is by weight) cocoanut active charcoal-attapulgite clay mixture, stir 25min under 50 revs/min of speed after, remove by filter cocoanut active charcoal-attapulgite clay mixture, oil phase after filtration is warming up to 110 DEG C through interchanger, be less than in vacuum tightness after dehydrating under the condition of 400Pa and obtain the Rice pollard oil that comes unstuck that precursor substance content is less than 3%.
Detecting gained chlorine source content is 12mg/kg, and the content of 3-chlorine-1,2-propylene glycol ester is 2.2%.
Embodiment 7
Degumming method for reducing chlorine source in vegetables oil and 3-chlorine-1,2-propylene glycol ester precursor substance content:
Taking crude rapeseed oil as raw material, crude rapeseed oil is warming up to 80 DEG C via interchanger, then enter in glue kettle, under 12 revs/min of stirring velocitys, add oil to weigh 6% in spray mode, the water that temperature is 93 DEG C, 10min is stirred in the complete continuation that adds water, then via separating centrifuge water phase separated and oil phase, oil phase is cooled to 47 DEG C through interchanger, add oil and weigh 0.8% alkali alumina, stir 25min under 35 revs/min of speed after, remove by filter alkali alumina, oil phase after filtration is warming up to 105 DEG C through interchanger, be less than in vacuum tightness after dehydrating under the condition of 400Pa and obtain the rapeseed oil that comes unstuck that precursor substance content is less than 3.2%.
Detecting gained chlorine source content is 25mg/kg, and the content of 3-chlorine-1,2-propylene glycol ester precursor substance is 2.6%.
Embodiment 8
Degumming method for reducing vegetables oil chlorine source and middle 3-chlorine-1,2-propylene glycol ester precursor substance content:
Taking rice bran crude oil as raw material, rice bran hair is warming up to 80 DEG C via interchanger, then enter in glue kettle, under 15 revs/min of stirring velocitys, add oil to weigh 6% in spray mode, the water that temperature is 90 DEG C, 10min is stirred in the complete continuation that adds water, then via separating centrifuge water phase separated and oil phase, oil phase is cooled to 50 DEG C through interchanger, add oil and weigh Magnesium Silicate q-agent-pure aluminium silicate mixture of 1.2%, stir 25min under 50 revs/min of speed after, remove by filter Magnesium Silicate q-agent-pure aluminium silicate mixture, oil phase after filtration is warming up to 110 DEG C through interchanger, be less than in vacuum tightness after dehydrating under the condition of 400Pa and obtain the Rice pollard oil that comes unstuck that precursor substance content is less than 3%.
Detecting gained chlorine source content is 22mg/kg, and the content of 3-chlorine-1,2-propylene glycol ester is 2.7%.
Embodiment 9
Degumming method for reducing chlorine source in vegetables oil and 3-chlorine-1,2-propylene glycol ester precursor substance content:
Taking crude peanut oil as raw material, crude peanut oil is warming up to 86 DEG C via interchanger, then enter in glue kettle, under 13 revs/min of stirring velocitys, add oil to weigh 7% in spray mode, the water that temperature is 95 DEG C, 7min is stirred in the complete continuation that adds water, then via separating centrifuge water phase separated and oil phase, oil phase is cooled to 55 DEG C through interchanger, add oil and weigh 1% neutral alumina, stir 20min under 35 revs/min of speed after, remove by filter neutral alumina, oil phase after filtration is warming up to 100 DEG C through interchanger, be less than in vacuum tightness after dehydrating under the condition of 400Pa and obtain the peanut oil that comes unstuck that precursor substance content is less than 3%.
Detecting gained chlorine source content is 28mg/kg, and the content of 3-chlorine-1,2-propylene glycol ester precursor substance is 1.2%.
Embodiment 10
Degumming method for reducing chlorine source in vegetables oil and 3-chlorine-1,2-propylene glycol ester precursor substance content:
Taking crude rapeseed oil as raw material, crude rapeseed oil is warming up to 80 DEG C via interchanger, then enter in glue kettle, under 12 revs/min of stirring velocitys, add oil to weigh 6% in spray mode, the water that temperature is 93 DEG C, 10min is stirred in the complete continuation that adds water, then via separating centrifuge water phase separated and oil phase, oil phase is cooled to 47 DEG C through interchanger, add oil and weigh 0.8% rice hull active carbon (the pre-carbonization of warp, the molten silica removal of alkali and activated sintering make), stir 25min under 35 revs/min of speed after, remove by filter rice hull active carbon, oil phase after filtration is warming up to 105 DEG C through interchanger, be less than in vacuum tightness after dehydrating under the condition of 400Pa and obtain the rapeseed oil that comes unstuck that precursor substance content is less than 3%.
Detecting gained chlorine source content is 17mg/kg, and the content of 3-chlorine-1,2-propylene glycol ester precursor substance is 1.9%.
It should be noted that, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although the present invention is had been described in detail with reference to preferred embodiment, those of ordinary skill in the art is to be understood that, can modify or be equal to replacement technical scheme of the present invention, and not departing from the spirit and scope of technical solution of the present invention, it all should be encompassed in the middle of claim scope of the present invention.
Claims (6)
1. for reducing a Degumming method for chlorine source in vegetables oil and 3-chlorine-1,2-propylene glycol ester precursor substance content, it is characterized in that,
Taking raw plant oil as raw material, raw plant oil is warming up to 80～87 DEG C via interchanger, then enter in degumming device, under whipped state, add in spray mode the hot water that is equivalent to described raw plant oil mass percent 5～10%, the temperature of described hot water is 90～95 DEG C, the complete continuation that adds water is stirred, then water phase separated and oil phase, oil phase is cooled to 40～55 DEG C through interchanger, add the neutrality and/or the alkaline adsorbent that are equivalent to described raw plant oil mass percent 0.1～1.5%, after stirring, remove by filter neutrality and/or alkaline adsorbent, oil phase after filtration is warming up to rapidly 90～120 DEG C through interchanger, under vacuum condition, dehydrate, obtain chlorine source content and be less than 100mg/kg, 3-chloro-1, the vegetables oil that comes unstuck that 2-propylene glycol ester precursor substance content is less than 3%.
2. Degumming method according to claim 1, is characterized in that, described in add water complete continuation stir, its stirring velocity is 8～15 revs/min.
3. Degumming method according to claim 1, is characterized in that, removes by filter neutrality and/or alkaline adsorbent after described stirring, and its stirring velocity is 30～55 revs/min.
4. Degumming method according to claim 1, is characterized in that, under described vacuum condition, dehydrates, the vacuum tightness < 400Pa dehydrating.
5. Degumming method according to claim 1, it is characterized in that, described neutrality and/or alkaline adsorbent are one or more in cocoanut active charcoal-attapulgite clay mixture, alkali alumina, Magnesium Silicate q-agent-pure aluminium silicate mixture, neutral alumina and rice hull active carbon.
6. Degumming method according to claim 5, is characterized in that, described cocoanut active charcoal-attapulgite clay mixture, and by weight, its ratio is cocoanut active charcoal: attapulgite clay=0.3:1～1:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310545850.5A CN103525548B (en) | 2013-11-06 | 2013-11-06 | Degumming method for reducing content of chlorine sources and 3-monochlorpropane-1,2-diol ester precusor substances in vegetable oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310545850.5A CN103525548B (en) | 2013-11-06 | 2013-11-06 | Degumming method for reducing content of chlorine sources and 3-monochlorpropane-1,2-diol ester precusor substances in vegetable oil |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103525548A CN103525548A (en) | 2014-01-22 |
| CN103525548B true CN103525548B (en) | 2014-10-01 |
Family
ID=49927903
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310545850.5A Active CN103525548B (en) | 2013-11-06 | 2013-11-06 | Degumming method for reducing content of chlorine sources and 3-monochlorpropane-1,2-diol ester precusor substances in vegetable oil |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103525548B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104531349A (en) * | 2015-01-23 | 2015-04-22 | 上海交通大学 | Method for reducing 3-chlorine-1,2-propylene glycol ester during grease processing |
| CN106916630B (en) * | 2015-12-25 | 2021-05-18 | 丰益(上海)生物技术研发中心有限公司 | Method for controlling generation of grease noxious substances |
| CN114729282A (en) * | 2019-11-15 | 2022-07-08 | 雀巢产品有限公司 | Prevention of MCPD formation by assisted degumming |
| CN112592761A (en) * | 2020-09-30 | 2021-04-02 | 天津南侨食品有限公司 | Control method for reducing content of 3-chloropropanol ester in beef tallow |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010063450A1 (en) * | 2008-12-02 | 2010-06-10 | Süd-Chemie AG | Method for reducing the 3-mcpd content in refined vegetable oils |
| CN102334563A (en) * | 2010-07-16 | 2012-02-01 | 丰益(上海)生物技术研发中心有限公司 | Method for controlling content of 3-chloro-1,2-propanediol or ester thereof in oil |
| KR101207413B1 (en) * | 2011-06-09 | 2012-12-04 | 씨제이제일제당 (주) | A method of process for edible oil reduced with 3-chloro-1,2-propanediol forming substances and product prepared thereby |
| EP2586854A1 (en) * | 2009-06-30 | 2013-05-01 | Sime Darby Malaysia Berhad | Process for removing unwanted propanol components from unused triglyceride oil |
-
2013
- 2013-11-06 CN CN201310545850.5A patent/CN103525548B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010063450A1 (en) * | 2008-12-02 | 2010-06-10 | Süd-Chemie AG | Method for reducing the 3-mcpd content in refined vegetable oils |
| EP2586854A1 (en) * | 2009-06-30 | 2013-05-01 | Sime Darby Malaysia Berhad | Process for removing unwanted propanol components from unused triglyceride oil |
| CN102334563A (en) * | 2010-07-16 | 2012-02-01 | 丰益(上海)生物技术研发中心有限公司 | Method for controlling content of 3-chloro-1,2-propanediol or ester thereof in oil |
| KR101207413B1 (en) * | 2011-06-09 | 2012-12-04 | 씨제이제일제당 (주) | A method of process for edible oil reduced with 3-chloro-1,2-propanediol forming substances and product prepared thereby |
Non-Patent Citations (6)
| Title |
|---|
| 吴克刚等.花生油水化脱胶工艺条件的研究.《食品工业科技》.2012,第33卷(第7期),第257-259页. |
| 氯丙醇酯-油脂食品中新的潜在危害因子;金青哲等;《中国粮油学报》;20111130;第26卷(第11期);第119-123页 * |
| 脱胶效果对油脂精炼影响;赵军;《粮食与油脂》;20020630(第6期);第40-42页 * |
| 花生油水化脱胶工艺条件的研究;吴克刚等;《食品工业科技》;20120731;第33卷(第7期);第257-259页 * |
| 赵军.脱胶效果对油脂精炼影响.《粮食与油脂》.2002,(第6期),第40-42页. |
| 金青哲等.氯丙醇酯-油脂食品中新的潜在危害因子.《中国粮油学报》.2011,第26卷(第11期),第119-123页. |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103525548A (en) | 2014-01-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| TW212141B (en) | ||
| JP6671396B2 (en) | Method for removing metals from metal-containing glyceride oils, comprising a basic quaternary ammonium salt treatment | |
| CN103525548B (en) | Degumming method for reducing content of chlorine sources and 3-monochlorpropane-1,2-diol ester precusor substances in vegetable oil | |
| Didi et al. | Colza oil bleaching through optimized acid activation of bentonite. A comparative study | |
| EP2449070B1 (en) | Process for removing unwanted propanol components from unused triglyceride oil | |
| JP5803671B2 (en) | Method for reducing chloropropanols and their forming substances and glycidol fatty acid esters in glyceride oils and fats | |
| CN105916969B (en) | Removal of free fatty acids from glyceride oils | |
| Wiedermann | Degumming, refining and bleaching soybean oil | |
| JP2018517814A (en) | Method for removing chloropropanol and / or glycidol, or fatty acid esters thereof from glyceride oil, and a method for purifying an improved glyceride oil comprising them | |
| CN103805337B (en) | A kind of Testa oryzae oil process for purification | |
| Mana et al. | Removal of basic dyes from aqueous solutions with a treated spent bleaching earth | |
| CN105462687B (en) | Method for purifying olive oil by adopting mixed adsorbent | |
| JP2018517037A (en) | Method for removing metal contaminants from glyceride oil and method for purifying glyceride oil incorporating the same | |
| CN103060088A (en) | Method for controlling glycidyl ester in grease | |
| CN102936533A (en) | Method for refining silybum marianum seed oil by enzymic-method degumming | |
| WO2013018412A1 (en) | Purified glyceride composition and method for producing purified glyceride composition | |
| US20140012025A1 (en) | Method for removing phosphorus-containing compounds from triglyceride-containing compositions | |
| Ushedo et al. | Synthesis of N, N (1, 3-phenylene) dimethanimine: a useful resource for the removal of free fatty acid in waste vegetable oil | |
| EP0646162A4 (en) | Process for reducing contaminants in glyceride oils. | |
| CA1298853C (en) | Method for treating caustic refined glyceride oils for removal of soaps and phospholipids | |
| Karim et al. | Vegetable oil refining | |
| CN107022413A (en) | A kind of method of pigment and metal ion in removing vegetable oil | |
| Gnanasambandam et al. | Structure and performance of soy hull carbon adsorbents as affected by pyrolysis temperature | |
| Chew et al. | Principal formation and mitigation strategies for 3-MCPDE in palm oil processing | |
| CN106916630B (en) | Method for controlling generation of grease noxious substances |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20170906 Address after: Food College of Jiangnan University No. 1800 224122 Jiangsu city of Wuxi Province Li Lake Avenue Co-patentee after: The 93 group Harbin Wellcome Food Co. Ltd. Patentee after: Jiangnan University Address before: Food College of Jiangnan University No. 1800 224122 Jiangsu city of Wuxi Province Li Lake Avenue Patentee before: Jiangnan University |
|
| TR01 | Transfer of patent right | ||
| CP01 | Change in the name or title of a patent holder |
Address after: Food College of Jiangnan University, 1800 Lihu Avenue, Wuxi City, Jiangsu Province, 224122 Patentee after: Jiangnan University Patentee after: Jiusan Food Co.,Ltd. Address before: Food College of Jiangnan University, 1800 Lihu Avenue, Wuxi City, Jiangsu Province, 224122 Patentee before: Jiangnan University Patentee before: THE NINE THREE GROUP HARBIN WELLCOME FOOD Co.,Ltd. |
|
| CP01 | Change in the name or title of a patent holder |