CN103897811A - Production method for medium-chain and long-chain oil fatty acid - Google Patents
Production method for medium-chain and long-chain oil fatty acid Download PDFInfo
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Abstract
The invention discloses a production method for medium-chain and long-chain oil fatty acid. The production method comprises the following steps: carrying out transesterification reaction, saturated alkaline water neutralization, adsorbent desoaping, vacuum flashing and the like to medium-chain fatty acid triglycerides of C6-C12 and long-chain fatty acid triglycerides of C16-C24 in a reactor filled with lipase, to obtain the long-chain oil fatty acid in the product. The method solves the difficulty that the medium-chain and long-chain oil fatty acid in the prior art is complicated, and has the characteristics of being short in reaction time of the reactor, and low in energy consumption.
Description
Technical field
The present invention relates to the production method in the synthetic field, particularly a kind of fatty acid triglycercide of grease.
Background technology
Middle long-chain fat acid lipid is that middle chain fatty acid triglycerides is MLCT, be on triglyceride level respectively in conjunction with in, the new type functional grease that obtains of the lipid acid of long-chain.It has directly by human body portal vein and absorbs and enter liver fast to the feature of personal supplementing energy and nutrition, enteron aisle is not caused to burden, and can effectively reduce the concentration of total cholesterol and low-density lipoprotein, play the effect of the metabolic troubles such as fat-reducing and prophylactic treatment diabetes, hyperlipidemia.Prior art generally adopts long-chain fat acid lipid in ester exchange process production, use Triglycerides,C8-10 and chain fatty acid triglycerides, in the packed column that immobilized lipase is housed, realize transesterification reaction, because reaction is only carried out in packed column, in the time that grease flows out packed column, stop, therefore reaction time is long.Heated time affects the vigor of the lipase in packed column, if be heated for a long time, the vigor of lipase reduces, thereby has increased cost.The product obtaining after transesterification reaction is more complicated, removes the impurity in product, generally needs, through steps such as molecular distillation de-free fatty acids, decolouring and deodorizations, just can obtain the finished product, and whole process is produced line length, equipment investment costliness.
Summary of the invention
Technical problem to be solved by this invention is the defect that overcomes prior art, and a kind of production method of middle long-chain fat acid lipid is provided, and to solve a difficult problem for complex production process in prior art, described method has the advantages that the reactor reaction time is short, energy consumption is low.
Technical problem of the present invention realizes with following technical proposals:
A production method for middle long-chain fat acid lipid, comprises the steps:
A, by the 16-24 carbon chain fatty acid triglycerides of the 6-12 carbon Triglycerides,C8-10 of reaction raw materials 11-18 parts by weight and 80-100 parts by weight, be added in the reactor that is equiped with lipase, carry out continuously transesterification reaction 40 DEG C-70 DEG C of temperature; Reaction times 15-24 hour, termination reaction, obtaining middle chain fatty acid triglycerides composition is product A;
B, in product A, add saturated buck, stir, to acid value≤1.0mgKOH/g; The add-on of saturated buck is the 0.2%-2.0% of product A quality; Add sorbent material, fully stir, the add-on of sorbent material is the 0.5%-3.0% of product A quality, after filtering, extracts clear liquid B;
C, clear liquid B carry out vacuum flashing, obtain long-chain fat acid lipid in product through condensation fractionation.
The production method of above-mentioned middle long-chain fat acid lipid, described in described step (a), Triglycerides,C8-10 is the pungent Triglyceride DDD of 8-10 carbon, derives from palm-kernel oil or Oleum Cocois; The chain fatty acid triglycerides of 16-24 carbon derives from one or more in soybean oil in vegetables oil, Trisun Oil R 80, peanut oil, rapeseed oil, Semen Maydis oil, oleum lini, Thistle oil.
The production method of above-mentioned middle long-chain fat acid lipid, in described step (a), lipase is immobilized lipase, lipase add-on is the 0.1%-6.0% of reaction raw materials quality, and immobilized lipase is that root enzyme belongs in mould, Aspergillus mould, Mucor mould, yeast and steapsase a kind or several.
The production method of above-mentioned middle long-chain fat acid lipid, in described step (a), transesterification reaction temperature is 50 DEG C-70 DEG C.
The production method of above-mentioned middle long-chain fat acid lipid, the saturated buck of described step (b) is the saturated aqueous solution of sodium hydroxide or potassium hydroxide; Sorbent material is a kind in silica gel, attapulgite clay or atlapulgite.
The production method of above-mentioned middle long-chain fat acid lipid, the vacuum flashing of described step (c), for clear liquid B is warming up to 150 DEG C-180 DEG C, enters the quick atomization of vacuum flashing still and carries out flash distillation with steam, and the vacuum tightness of flash vaporization kettle is 50Pa-200Pa.
The production method of above-mentioned middle long-chain fat acid lipid, the reactor in described step (a) is the closed reactor with lipase collection device.
A kind of middle long-chain fat acid lipid that utilizes the production method of above-mentioned middle long-chain fat acid lipid to produce, the content of the middle chain fatty acid triglycerides in described middle long-chain fat acid lipid is 20%-39%, the content of 6-12 carbon Triglycerides,C8-10 is 1.0%-3.0%, the content of 16-24 carbon chain fatty acid triglycerides is 60%-77%, the content of medium chain fatty acid is 11%-18%, and the acid value of product grease is≤1.0mgKOH/g.
The problems such as the present invention adopts technique scheme, effectively solves the complex production process of existing middle long-chain fat acid lipid combination, and the reactor reaction time is long, energy consumption is high.The present invention adopts and in closed reactor, carries out continuous ester interchange reaction, in saturated buck, close depickling, the operations such as sorbent material absorption Chinese honey locust, oily vapour flash distillation deodorization under high vacuum condition again, thereby obtain Triglycerides,C8-10 residue and be less than 2.5%, the high-quality product that middle chain fatty acid triglycerides is greater than 25%, and retained natural perfume base composition and the distinctive nutritive ingredient in longer chain fatty acid.Described method has production technique Simple And Practical, and the reactor reaction time is short, energy consumption is low, the advantage that equipment investment is few.
The present invention carries out the Non-intermittent successive reaction of catalyzer lipase and reactant in the closed reactor with lipase collection device, has improved reaction efficiency.Airtight reaction conditions does not contact lipase with air, can keep active and recycling, thereby has extended the catalysis time of lipase, reduces production and operation cost.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
A production method for middle long-chain fat acid lipid, comprises the steps:
A, by reaction raw materials according to the chain fatty acid triglycerides of the 16-24 carbon of the Triglycerides,C8-10 of the 6-12 carbon of 11-18 parts by weight, 80-100 parts by weight, be added in the closed reactor with immobilized lipase collection device, the add-on of enzyme is the 0.1%-6.0% of raw oil material quality.Carry out continuously transesterification reaction 40 DEG C-70 DEG C of temperature, the chain fatty acid triglycerides of the Triglycerides,C8-10 of 6-12 carbon and 16-24 carbon is combined on a glycerol backbone to chain fatty acid triglycerides in formation.Transesterification reaction temperature is preferably 50 DEG C-70 DEG C.Reaction times is 15-24 hour, and obtaining middle chain fatty acid triglycerides composition is product A.
When transesterification reaction, reaction raw materials is input to from the top of closed reactor in the net bucket that lipase is housed, in vacuum or fill under the condition of nitrogen and react, the material reacting completely is by netting a barrel filtering separation, and the lipase of collection can reuse.
The pungent Triglyceride DDD of the preferred 8-10 carbon of Triglycerides,C8-10, derives from palm-kernel oil or Oleum Cocois; The chain fatty acid triglycerides of 16-24 carbon derives from one or more in soybean oil in vegetables oil, sunflower seed oil, peanut oil, rapeseed oil, Semen Maydis oil, oleum lini, Thistle oil.Lipase is immobilized lipase, and immobilized lipase is that root enzyme belongs in mould, Aspergillus mould, Mucor mould, yeast and steapsase a kind or several.The lipase using in embodiment is the immobilized lipase purchased from Novozymes Company.
B, according to the acid value of GB/T5530 animal-plant oil acid number and acid test standard detection product A, if when acid value > 1.0mgKOH/g, in product A, add saturated buck to carry out neutralization reaction, temperature is controlled at 40 DEG C-60 DEG C, add while stirring, the add-on of saturated buck is the 0.2%-2.0% of product A quality; Saturated buck is the saturated aqueous solution of sodium hydroxide or potassium hydroxide.Add rear continuation to stir 0.5-1.0 hour, sampling detects, if acid value > is 1.0mgKOH/g, repeats preceding paragraph operation, is qualified to be down to≤1.0mgKOH/g of acid value.In grease, add sorbent material, add while stirring, after stirring starts, grease is cooled to 30 DEG C-40 DEG C, the add-on of sorbent material is the 0.5%-3.0% of product A quality.Sorbent material is a kind in silica gel, attapulgite clay or atlapulgite.Sorbent material granularity is 20 order-100 orders, and stirring velocity is 30-130 rev/min, and churning time 0.5-1.0 hour has adsorbed and carried out solid-liquid separation with filter afterwards, after filtration clear liquid B.
C, clear liquid B is preheated to 150 DEG C-180 DEG C, with the steam of 180 DEG C of-220 DEG C of degree with the vaporific flash vaporization kettle that sprays into, flash distillation under the condition of vacuum, vacuum tightness 50Pa-200Pa, remove volatile matter and excessive Triglycerides,C8-10, collect and separator recovery through condenser, overhead product is longer chain fatty acid food oils in the finished product again.
The specific targets of middle longer chain fatty acid food oils are: the content of middle chain fatty acid triglycerides that high performance liquid chromatography detects be 20%-39%(by percentage to the quality, as follows), the content of 6-12 carbon Triglycerides,C8-10 is 1.0%-3.0%, the content of 16-24 carbon chain fatty acid triglycerides is 60%-77%, the content of the medium chain fatty acid of gas chromatographic detection is 11%-18%, and the acid value of product grease is≤1.0mgKOH/g.
Embodiment 1
Reaction raw materials is the Triglycerides,C8-10 of 8-10 carbon and the chain fatty acid triglycerides of the 16-24 carbon that soybean oil is extracted that palm-kernel oil extracts, the parts by weight of reactant are 87 parts of the chain fatty acid triglycerides of 13 parts of Triglycerides,C8-10s, the 16-24 carbon of 8-10 carbon, above-mentioned reactant is packed in the closed reactor with lipase collection device, lipase used is Novozyme 435 immobilized lipases of Novozymes Company, and consumption is raw materials quality 1%.At 55 DEG C of temperature, inflated with nitrogen carries out transesterification reaction, and 15 hours reaction times termination reaction, obtains product A.Export sampling by reactor bottom, the acid value value 2.2mgKOH/g of detected result product A.
Product A is put into depickling container, add the potassium hydroxide saturated aqueous solution of product A quality 1.5%, add while stirring, stirring velocity is 50r/min, and temperature 50 C continued to stir after 1 hour, and sampling detects, and acid value is 0.8mgKOH/g.After acid value is qualified, add the silica gel that accounts for oil quality 2.0%, add while stirring, stirring velocity is 30r/min, and after stirring starts, grease cools to 40 DEG C, stirs 40min; After stirring finishes, separate with filter; The diameter of silica gel particle is 0.8mm(granularity 20 orders), after filtration, obtain clear liquid B.
Clear liquid B is warming up to 160 DEG C of atomizations together with steam, and spurts into and in flash vaporization kettle, carry out deodorization and remove medium chain triglyceride residue, the vacuum tightness 50Pa of flash vaporization kettle, 180 DEG C of vapor temperatures.The evaporant that vacuum reclaims is collected by condenser and by separator fractionation, fraction is longer chain fatty acid food oils in product.
The detection index of the finished product is: the middle chain fatty acid triglycerides content that the medium chain fatty acid content of gas chromatographic detection is 12.6%, high performance liquid chromatography detects is 25%, chain fatty acid triglycerides content is 72.6%, Triglycerides,C8-10 content is 2.4%.
Embodiment 2
In Oleum Cocois, extract 8-10 carbon Triglycerides,C8-10, in peanut oil, extract 16-24 carbon chain fatty acid triglycerides, both mass fractions are 11 parts of 8-10 carbon Triglycerides,C8-10s, 80 parts of 16-24 carbon chain fatty acid triglycerides, the Lipozyme TL IM immobilized lipase that accounts for raw materials quality 6% is joined in the reactor with lipase collection device, and at 60 DEG C of temperature, 150Pa vacuum is carried out transesterification reaction, 20 hours reaction times termination reaction, obtains product A.Its acid value is 2.4 mgKOH/g.
Reclaim reaction product A to depickling container, add the saturated buck of sodium hydroxide, add-on is 0.8% of product A quality, add while stirring, stirring velocity is 45r/min, 40 DEG C of temperature, add rear continuation to stir, stir sampling after 0.5 hour and detect, acid value drops to 1.3mgKOH/g.Add the saturated sodium hydroxide solution of product A quality 0.3% to repeat previous action, now acid value of lipids is 0.5mgKOH/g again.After depickling is qualified, add the attapulgite clay that accounts for product A quality 0.5%, add while stirring, stirring velocity is 35r/min, stirs and starts rear oil supply and cool to 30 DEG C, stirs 60min, stirs and finishes to separate with filter afterwards; The diameter of attapulgite clay particle is 0.2mm(granularity 80 orders), after filtration, obtain clear liquid B.
Clear liquid B enters steam flash vaporization kettle, under vacuum tightness 100Pa, 180 DEG C of clear liquid B temperature, 210 DEG C of conditions of vapor temperature, carry out deodorization and de-medium chain fatty acid residue, the evaporant that vacuum reclaims is collected by condenser, and fraction is longer chain fatty acid food oils in product.
The finished product index is: gas chromatographic detection medium chain fatty acid is 12.8%, high performance liquid chromatography detect in chain fatty acid triglycerides be 26.3%, chain fatty acid triglycerides is 71.6%, Triglycerides,C8-10 is 2.1%.
Embodiment 3
By extracting 6-12 carbon Triglycerides,C8-10 in palm-kernel oil, in rapeseed oil, extract 16-24 carbon chain fatty acid triglycerides, wherein the parts by weight of Triglycerides,C8-10 are 15, the parts by weight of chain fatty acid triglycerides are 90.Above-mentioned raw materials grease is joined in the reactor that Lipozyme RM IM immobilized enzyme collection device is housed, and the add-on of lipase is raw materials quality 3%.At 65 DEG C of temperature, inflated with nitrogen carries out transesterification reaction, and 24 hours reaction times termination reaction, obtains product A.By the sampling of reaction outlet at bottom, inspection acid value 1.8mgKOH/g.
Reclaim reaction product A to depickling container, add saturated sodium hydroxide solution, alkali lye accounts for 2.0% of product A quality, and temperature adds while stirring at 60 DEG C, and stirring velocity is 45 r/min, adds rear lasting stirring 1 hour.Sampling detects, and acid value drops to 0.85mgKOH/g, and depickling is qualified.In grease, add the atlapulgite that accounts for oil quality 1.0%, add while stirring, stirring velocity is 35r/min, and stirring starts rear oil supply and cools to 30 DEG C, stirs 60min.Stirring finishes to separate with filter afterwards.The granularity of atlapulgite particle is 50 orders, obtains clear liquid B after filtration.
Clear liquid B is warming up to 170 DEG C, after atomization, enter in the flash vaporization kettle of vacuum tightness 170Pa deodorization and the excessive residue of de-medium chain fatty acid in flash process together with 220 DEG C of steam, the evaporant that vacuum reclaims is collected fractionation by condenser, obtains longer chain fatty acid food oils in product.
The index of the finished product is: with chain fatty acid triglycerides 32.23%, chain fatty acid triglycerides 65.54%, Triglycerides,C8-10 2.23% in gas chromatographic detection medium chain fatty acid 14.2%, liquid chromatographic detection.
Embodiment 4
The 8-10 carbon Triglycerides,C8-10 that palm-kernel oil extracts, the 16-24 carbon chain fatty acid triglycerides that Semen Maydis oil extracts, wherein the parts by weight of Triglycerides,C8-10 are 18, the parts by weight of chain fatty acid triglycerides are 85.Join in the vacuum reactor with immobilized lipase collection device, the immobilized lipase of use is Novozyme 435, and the add-on of enzyme is oil quality 5%.Under 45 DEG C of temperature vacuum (vacuum tightness 55Pa) condition, carry out transesterification reaction, 18 hours reaction times termination reaction, obtains product A.Export sampling by reactor bottom, detecting acid value is 2.5 mgKOH/g.
Reclaim reaction product A to depickling container, add the saturated buck of sodium hydroxide of product A quality 0.5%, add while stirring, oil temperature remains on 45 DEG C, and stirring velocity is 50 r/min, stirs sampling after 1 hour and detects, and acid value drops to 1.3mgKOH/g; Repeat previous action, then add the saturated sodium hydroxide solution of product A quality 0.5%, now acid value of lipids is 0.4mgKOH/g.After depickling is qualified, grease cools to 35 DEG C, adds the attapulgite clay (granularity 100 orders of attapulgite clay particle) that accounts for oil quality 3.0% in grease, add while stirring, stirring velocity is 55r/min, stirs 60min, stirs and finishes to separate with filter afterwards again; Obtain clear liquid B.
Clear liquid B after filtering is entered to flash vaporization kettle and carry out steam flash process, deodorization and de-excessive medium chain triglyceride residue, vacuum tightness 100Pa, 155 DEG C of grease temperature, 210 DEG C of vapor temperatures, the evaporant that vacuum reclaims is collected by condenser, obtains longer chain fatty acid food oils in product.。
The finished product index is: gas chromatographic detection medium chain fatty acid is 14.8%, high performance liquid chromatography detect in chain fatty acid triglycerides be 34.3%, chain fatty acid triglycerides is 63.3%, Triglycerides,C8-10 is 2.4%.
Embodiment 5
In palm-kernel oil, extract 6-12 carbon Triglycerides,C8-10, in Thistle oil and Semen Maydis oil, extract the fatty acid triglycercide of 16-24 carbon, both ratio of weight and number 16:100.Raw oil material is added in the Lipozyme RM IM immobilized lipase enzyme reactor being equipped with, and lipase accounts for 6% of oil quality, 70 DEG C of temperature, carries out transesterification reaction under the condition of vacuum tightness 50Pa, and 20 hours reaction times termination reaction, obtains product A.Sampling is surveyed acid value and is equaled 1.8mgKOH/g.
Reclaim reaction product A to depickling container, add saturated potassium hydroxide aqueous solution, add-on is 0.9% of product A quality, adds while stirring, and stirring velocity is 45 r/min.Add rear oil temperature to remain on 55 DEG C, continue to stir sampling after 1 hour and detect, acid value drops to 0.85mgKOH/g.The silica gel (granularity is 0.2 order) that adds product A quality 0.8% in the qualified backward reactant of depickling, adds while stirring, and stirring velocity is 40r/min, stirs and starts rear oil supply and cool to 30 DEG C, stirs 60min, stirs and finishes to separate with filter afterwards; Obtain clear liquid B.
Clear liquid B after filtration carries out deodorization and de-excessive Triglycerides,C8-10 at steam flash process, 200 DEG C of vacuum tightness 70Pa, vapor temperatures, and 170 DEG C of clear liquid temperature, the evaporant that vacuum reclaims is collected by condenser.Be longer chain fatty acid food oils in product.
Final inspection product index is: with chain fatty acid triglycerides 34.23%, chain fatty acid triglycerides 64.54%, Triglycerides,C8-10 1.23% in gas chromatographic detection medium chain fatty acid 15.7%, liquid chromatographic detection.
Claims (8)
1. in, a production method for long-chain fat acid lipid, is characterized in that, it comprises the steps:
A, by the 16-24 carbon chain fatty acid triglycerides of the 6-12 carbon Triglycerides,C8-10 of reaction raw materials 11-18 parts by weight and 80-100 parts by weight, be added in the reactor that is equiped with lipase, carry out continuously transesterification reaction 40 DEG C-70 DEG C of temperature; Reaction times 15-24 hour, termination reaction, obtaining middle chain fatty acid triglycerides composition is product A;
B, in product A, add saturated buck, stir, to acid value≤1.0mgKOH/g; The add-on of saturated buck is the 0.2%-2.0% of product A quality; Add sorbent material, fully stir, the add-on of sorbent material is the 0.5%-3.0% of product A quality, after filtering, extracts clear liquid B;
C, clear liquid B carry out vacuum flashing, obtain long-chain fat acid lipid in product through condensation fractionation.
2. the production method of middle long-chain fat acid lipid according to claim 1, is characterized in that, Triglycerides,C8-10 described in described step a is the pungent Triglyceride DDD of 8-10 carbon, derives from palm-kernel oil or Oleum Cocois; The chain fatty acid triglycerides of 16-24 carbon derives from one or more in soybean oil in vegetables oil, Trisun Oil R 80, peanut oil, rapeseed oil, Semen Maydis oil, oleum lini, Thistle oil.
3. the production method of middle long-chain fat acid lipid according to claim 2, it is characterized in that, in described step a, lipase is immobilized lipase, lipase add-on is the 0.1%-6.0% of reaction raw materials quality, and immobilized lipase is that root enzyme belongs in mould, Aspergillus mould, Mucor mould, yeast and steapsase a kind or several.
4. the production method of middle long-chain fat acid lipid according to claim 3, is characterized in that, in described step a, transesterification reaction temperature is 50 DEG C-70 DEG C.
5. the production method of middle long-chain fat acid lipid according to claim 4, is characterized in that, the saturated buck of described step b is the saturated aqueous solution of sodium hydroxide or potassium hydroxide; Sorbent material is a kind in silica gel, attapulgite clay or atlapulgite.
6. the production method of middle long-chain fat acid lipid according to claim 5, it is characterized in that, the vacuum flashing of described step c, for clear liquid B is warming up to 150 DEG C-180 DEG C, enters the quick atomization of vacuum flashing still and carries out flash distillation with steam, and the vacuum tightness of flash vaporization kettle is 50Pa-200Pa.
7. according to the production method of the middle long-chain fat acid lipid described in claim 1-6 any one, it is characterized in that, the reactor in described step a is the closed reactor with lipase collection device.
8. the middle long-chain fat acid lipid that the production method of a middle long-chain fat acid lipid according to claim 7 is produced, it is characterized in that, the content of the middle chain fatty acid triglycerides in described middle long-chain fat acid lipid is 20%-39%, the content of 6-12 carbon Triglycerides,C8-10 is 1.0%-3.0%, the content of 16-24 carbon chain fatty acid triglycerides is 60%-77%, the content of medium chain fatty acid is 11%-18%, and the acid value of product grease is≤1.0mgKOH/g.
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