CN102241586B - Method for synthesizing and purifying high-purity fatty acyl monoglyceride - Google Patents
Method for synthesizing and purifying high-purity fatty acyl monoglyceride Download PDFInfo
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- -1 fatty acyl monoglyceride Chemical compound 0.000 title claims abstract description 65
- 230000002194 synthesizing effect Effects 0.000 title claims abstract 3
- 238000000034 method Methods 0.000 title abstract description 22
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 224
- 238000000199 molecular distillation Methods 0.000 claims abstract description 81
- 235000021588 free fatty acids Nutrition 0.000 claims abstract description 55
- 230000032050 esterification Effects 0.000 claims abstract description 39
- 238000005886 esterification reaction Methods 0.000 claims abstract description 39
- 238000010992 reflux Methods 0.000 claims abstract description 39
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000011949 solid catalyst Substances 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 238000004821 distillation Methods 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000498 cooling water Substances 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 235000011187 glycerol Nutrition 0.000 claims description 104
- 125000005908 glyceryl ester group Chemical group 0.000 claims description 68
- 238000002360 preparation method Methods 0.000 claims description 30
- 238000005809 transesterification reaction Methods 0.000 claims description 25
- 239000003921 oil Substances 0.000 claims description 22
- 235000019198 oils Nutrition 0.000 claims description 22
- 239000002253 acid Substances 0.000 claims description 21
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 20
- 229930195729 fatty acid Natural products 0.000 claims description 20
- 239000000194 fatty acid Substances 0.000 claims description 20
- 150000004665 fatty acids Chemical class 0.000 claims description 19
- 150000002632 lipids Chemical class 0.000 claims description 19
- 239000004519 grease Substances 0.000 claims description 17
- 239000003054 catalyst Substances 0.000 claims description 16
- 238000000746 purification Methods 0.000 claims description 14
- 238000013517 stratification Methods 0.000 claims description 13
- 239000007795 chemical reaction product Substances 0.000 claims description 11
- 239000007787 solid Substances 0.000 claims description 11
- 239000003930 superacid Substances 0.000 claims description 11
- 235000021355 Stearic acid Nutrition 0.000 claims description 9
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 9
- 239000008117 stearic acid Substances 0.000 claims description 9
- 239000002131 composite material Substances 0.000 claims description 8
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 8
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 claims description 7
- DCXXMTOCNZCJGO-UHFFFAOYSA-N Glycerol trioctadecanoate Natural products CCCCCCCCCCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCCCCCCCCCC)COC(=O)CCCCCCCCCCCCCCCCC DCXXMTOCNZCJGO-UHFFFAOYSA-N 0.000 claims description 7
- 235000020238 sunflower seed Nutrition 0.000 claims description 7
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 6
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 6
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 6
- 239000005642 Oleic acid Substances 0.000 claims description 6
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 6
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 6
- 235000021323 fish oil Nutrition 0.000 claims description 6
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 6
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 6
- 235000013311 vegetables Nutrition 0.000 claims description 6
- 238000010025 steaming Methods 0.000 claims description 5
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 4
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 4
- 239000002826 coolant Substances 0.000 claims description 4
- 239000008187 granular material Substances 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 235000012424 soybean oil Nutrition 0.000 claims description 4
- 239000003549 soybean oil Substances 0.000 claims description 4
- 235000019484 Rapeseed oil Nutrition 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- OYHQOLUKZRVURQ-HZJYTTRNSA-N Linoleic acid Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(O)=O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 claims description 2
- 235000019483 Peanut oil Nutrition 0.000 claims description 2
- GEIAQOFPUVMAGM-UHFFFAOYSA-N ZrO Inorganic materials [Zr]=O GEIAQOFPUVMAGM-UHFFFAOYSA-N 0.000 claims description 2
- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 claims description 2
- 235000020661 alpha-linolenic acid Nutrition 0.000 claims description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims description 2
- 229960004488 linolenic acid Drugs 0.000 claims description 2
- KQQKGWQCNNTQJW-UHFFFAOYSA-N linolenic acid Natural products CC=CCCC=CCC=CCCCCCCCC(O)=O KQQKGWQCNNTQJW-UHFFFAOYSA-N 0.000 claims description 2
- 239000000312 peanut oil Substances 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 229960002969 oleic acid Drugs 0.000 claims 2
- 229960004232 linoleic acid Drugs 0.000 claims 1
- 125000005456 glyceride group Chemical group 0.000 abstract description 7
- 125000004185 ester group Chemical group 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- OGBUMNBNEWYMNJ-UHFFFAOYSA-N batilol Chemical class CCCCCCCCCCCCCCCCCCOCC(O)CO OGBUMNBNEWYMNJ-UHFFFAOYSA-N 0.000 description 23
- 239000002994 raw material Substances 0.000 description 23
- 238000009833 condensation Methods 0.000 description 18
- 230000005494 condensation Effects 0.000 description 18
- 239000006227 byproduct Substances 0.000 description 17
- 239000000047 product Substances 0.000 description 16
- 239000007789 gas Substances 0.000 description 13
- 239000011973 solid acid Substances 0.000 description 11
- 239000003795 chemical substances by application Substances 0.000 description 9
- 238000004587 chromatography analysis Methods 0.000 description 9
- 239000002245 particle Substances 0.000 description 9
- 125000005457 triglyceride group Chemical group 0.000 description 9
- LDVVTQMJQSCDMK-UHFFFAOYSA-N 1,3-dihydroxypropan-2-yl formate Chemical compound OCC(CO)OC=O LDVVTQMJQSCDMK-UHFFFAOYSA-N 0.000 description 6
- 150000002148 esters Chemical class 0.000 description 6
- 235000003084 food emulsifier Nutrition 0.000 description 6
- 229920000223 polyglycerol Polymers 0.000 description 6
- 235000010469 Glycine max Nutrition 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000006386 neutralization reaction Methods 0.000 description 3
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- 235000019482 Palm oil Nutrition 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000002540 palm oil Substances 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 238000003828 vacuum filtration Methods 0.000 description 2
- 244000068988 Glycine max Species 0.000 description 1
- 238000007171 acid catalysis Methods 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000005815 base catalysis Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000006471 dimerization reaction Methods 0.000 description 1
- 150000002190 fatty acyls Chemical group 0.000 description 1
- 235000020778 linoleic acid Nutrition 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
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 125000002811 oleoyl group Chemical group O=C([*])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])/C([H])=C([H])\C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 235000003441 saturated fatty acids Nutrition 0.000 description 1
- 150000004671 saturated fatty acids Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention discloses a method for synthesizing and purifying high-purity fatty acyl monoglyceride, which comprises the following steps: (1) mixing fat, free fatty acid and a solid catalyst, vacuumizing, stirring, heating, obtaining a mixture of fat, adding glycerol into the mixture of fat, performing refluxing esterification and ester exchange reactions, controlling the temperature of cooling water in a reflux condenser to allow water generated in esterification to be pumped out under vacuum and allow glycerol to be condensed and refluxed, and demixing the products of the reaction, wherein the upper layer is a glyceride layer; (2) removing unreacted free fatty acid and glycerol from the glyceride layer through primary molecular distillation; and (3) subjecting the glyceride layer from which the free fatty acid and glycerol are removed to secondary molecular distillation, and obtaining a distillate and a distillation residue, wherein the distillate is high-purity fatty acyl monoglyceride and the distillation residue is diglyceride or triglyceride. When the method is used, the process is shortened, equipment investment is saved, and the primary yield of the product is increased greatly.
Description
Technical field
The invention belongs to food emulsifier preparation field, be specifically related to the synthetic and purification process of a kind of fatty acyl monoglyceride (fatty acid monoacylglycerol).
Background technology
Food emulsifier is the most popular tensio-active agent of food service industry, and within the scope of our times, the consumption of food emulsifier surpasses 400,000 tons, and the consumption of China's food emulsifier is 3～50,000 tons of left and right.Fatty acyl monoglyceride (abbreviation mono-glycerides) is a series products maximum in food emulsifier, and China's mono-glycerides output has reached 2.5～30,000 tons, occupies 40～60% left and right of food emulsifier.The molecule distillating monoglyceride product that share of market is the highest is stearyl direactive glyceride.
The technique of existing suitability for industrialized production high purity molecule distillating monoglyceride as shown in Figure 1 (Liang Zhenming. molecule distillating monoglyceride generating process, modern food science and technology, 2005,83 (1): 97-98,102).Technology profile is as follows: after (1) winterized stearin and glycerine and basic catalyst mix; at 220～230 ℃, under nitrogen protection, react with excess of glycerol solution; generate mono-glycerides product and byproduct triglyceride and unreacted winterized stearin, because the existence of alkali can be produced a small amount of Polyglycerine and polyglycerol ester byproduct.(2) after reaction finishes, staticly settle, reaction solution is divided into two-layer, the glycerin layer of polarity and nonpolar glyceryl ester layer.Glycerin layer is returned to reaction as reaction raw materials, glyceryl ester layer acid neutralization basic catalyst, by wiped film vaporization to glyceryl ester pull-up gas and dehydration.(3) lipid acid of producing by the free glycerol in molecular distillation deglycerizin ester for the first time and a small amount of neutralization.The glyceryl ester layer that contains mono-glycerides carries out molecular distillation for the second time again, steams highly purified molecular distillation stearic acid monoglycerides.Obtain steaming remaining byproduct triglyceride, winterized stearin and a small amount of polyglycerol ester simultaneously.Steaming remaining byproduct can recycle in Returning reactor, until the content of polyglycerol ester surpasses certain limit.
The main drawback of the technique of existing molecule distillating monoglyceride is: the content of monoglyceride in the glyceryl ester layer that (1) glycerolysis reaction once obtains, generally 40～50%, is difficult to break through 60%.Cause a productive rate lower.(2) adopt basic catalyst, under high temperature, reaction easily makes glycerol polymerization, forms even polyglycerol of dimerization, produces polyglycerol ester byproduct.Affect the composition of product and follow-up separation.(3) due to a small amount of water of the alkaline catalytic production of neutralization, need luwa evaporator to dewater, increase the complicacy of technique.
Summary of the invention
In order to solve above-mentioned the deficiencies in the prior art part, primary and foremost purpose of the present invention is to provide a kind of synthetic and purification process of high-purity fatty acyl monoglyceride.
The high-purity fatty acyl monoglyceride that provides aforesaid method to prepare is provided a further object of the present invention.
Object of the present invention is achieved through the following technical solutions: a kind of synthetic and purification process of high-purity fatty acyl monoglyceride, comprises following operation steps:
(1) fatty acyl monoglyceride is synthetic: after grease, free fatty acids and solid catalyst are mixed, reaction system is evacuated to pressure 400～10000Pa, stirs and is warming up to 170～230 ℃, obtains rich mixture; Adopt dropping mode to add in rich mixture glycerine, esterification and transesterification reaction reflux under vacuum condition; Control the temperature of cooling water in reflux exchanger, the water that esterification is generated is taken away by vacuum, glycerine condensing reflux; By reaction product layering, upper strata is glyceryl ester layer;
(2) de-free fatty acids and the glycerine of glyceryl ester layer: step (1) gained glyceryl ester layer is removed to unreacted free fatty acids and glycerine by first step molecular distillation;
(3) preparation of high-purity fatty acyl monoglyceride: the glyceryl ester layer of step (2) gained being removed to lipid acid and glycerine enters second stage molecular distillation, obtains distillment and steams excess; Described distillment is high-purity fatty acyl monoglyceride, and steaming excess is triglyceride and triglyceride level.
The described grease of step (1) is winterized stearin, vegetables oil or fish oil; Described free fatty acids is a kind of or its mixture of the unsaturated fatty acidss such as the saturated fatty acids such as stearic acid, oleic acid, palmitinic acid, linoleic acid plus linolenic acid and oleic acid.
Described vegetables oil is a kind of or its mixture in soybean oil, peanut oil, sunflower seed oil, plam oil and rapeseed oil.
Described in step (1), be layered as centrifugal layering, stratification or filter rear stratification; If adopt centrifugal layering or stratification, the lower floor obtaining is solid catalyst and glycerin layer; Stratification after filtering if adopt, the lower floor obtaining is glycerin layer.
The described free fatty acids of step (1) accounts for 20～100% of grease and free fatty acids total mass; Lipid acid mole number in described grease and free fatty acids, with the ratio of the mole number of glycerine be 1: 1～1: 3; The addition of described solid catalyst is 0.1～0.5% of grease and free fatty acids total mass; It is described that glycerine is adopted to the time that dropping mode adds is 20～45min; The temperature of described esterification and transesterification reaction is 170～230 ℃, and the reaction times is 1～5 hour, and reaction pressure is 400～10000Pa; The temperature of the water coolant in described reflux exchanger is 30～80 ℃; The time of described stratification is 30～60min; The centrifugal speed of described centrifugal layering is 3000r/min, and the time is 10～15min.
More preferably, the described free fatty acids of step (1) accounts for 40% of grease and free fatty acids total mixture quality; Lipid acid mole number in described grease and free fatty acids, with the ratio of the mole number of glycerine be 1: 1.5; The addition of described solid catalyst is 0.2% of free fatty acids and grease total mass; It is described that glycerine is adopted to the time that dropping mode adds is 30min; The temperature of described esterification and transesterification reaction is 200 ℃, and the reaction times is 4 hours, and reaction pressure is 5000Pa; The temperature of the water coolant in described reflux exchanger is 50 ℃; The described stratification time is 45min; The centrifugal speed of described centrifugal layering is 3000r/min, and the time is 15min.
Unreacted free fatty acids and glycerol molecule that the described first step molecular distillation of step (2) is removed, can be used as in the reaction that raw material turns back to step (1) and go.
The described steaming excess of step (3) also can be used as in the reaction that reaction raw materials turns back to step (1) and goes.
The temperature of the described first step molecular distillation of step (2) is 120～160 ℃, and distillation pressure is 1～20Pa; The temperature of the described second stage of step (3) molecular distillation is 180～220 ℃, and distillation pressure is 0.1～5Pa.
More preferably, the temperature of the described first step molecular distillation of step (2) is 150 ℃, and distillation pressure is 5Pa; The temperature of the described second stage of step (3) molecular distillation is 200 ℃, and distillation pressure is 0.5Pa.
The described solid catalyst of step (1) is granule type SO
4 2-/ M
xo
ytype solid super acid catalyst, its granule type carrier is carrier is Al
2o
3, SiO
2or Al
2o
3-SiO
2composite oxides, its active carrier is ZrO
2, TiO
2, SnO
2, ZrO
2-TiO
2composite oxides, ZrO
2-SnO
2composite oxides or TiO
2-SnO
2composite oxides.
The high-purity fatty acyl monoglyceride preparing according to aforesaid method, purity >=90% of described high-purity fatty acyl monoglyceride.
Compared with prior art, tool has the following advantages and beneficial effect in the present invention:
(1) the present invention adopts the mixture of the sweet oil and grease of solid acid catalysis and lipid acid to carry out esterification and transesterification reaction; The content of the first mono-glycerides of primary first-order equation can reach more than 60%, than traditional base catalyzed reactions, has greatly improved a yield of product.
(2) the solid catalyst consumption of esterification employing is few, catalytic efficiency is high, is 20～40% of traditional alkaline catalysts consumption; After reaction finishes, solid catalyst can be removed by filtration or centrifugal method, has the potentiality of recycling.
(3) due to without to removing the further neutralizing treatment of reaction solution of catalyzer, follow-up purification step is compared with traditional base catalysis, can be saved the degassed step of knifing, shorten operation, save facility investment; The unreacted lipid acid of byproduct and glycerine that simultaneously the first step obtains, can be used as in the reaction that raw material all turns back to (1) step and go; The acid byproduct fatty of traditional base catalyzed reactions cannot return to reaction.
(4) owing to adopting solid acid catalyst, can there is not the side reaction of catalyzed polymerization in glycerine, thus do not have byproduct polyglycerol ester to produce, thus further improved the utilization ratio of raw material.
Accompanying drawing explanation
Fig. 1 is the production technique figure of existing industrialization molecule distillating monoglyceride.
Fig. 2 is the synthetic and purifying process route map of high-purity fatty acyl monoglyceride of the present invention.
Fig. 3 is the gas chromatogram of embodiment 5 gained high purity fatty acyl mono-glyceridess.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Embodiment 1
Synthetic and the purifying process route map of the present embodiment high-purity fatty acyl monoglyceride is as shown in Figure 2:
(1) fatty acyl monoglyceride is synthetic: get soybean oil 60g, soy(a)-bean oil fatty acid 40g adds in reactor, adds SO
4 2-/ ZrO
2-Al
2o
3(preparation method is CN02151526.3 with reference to publication number to solid acid catalyst, name is called the Chinese patent of < < catalyzed by particle type solid superacid agent and preparation method > >) 0.3g, it is 2000Pa that reactor is evacuated down to pressure, constantly stir simultaneously, when reaching 170 ℃ of temperature, temperature starts timing, by glycerine 40g (the lipid acid mole number in soybean oil and soy(a)-bean oil fatty acid, with the ratio of glycerine mole number be 1: 1.25) be added drop-wise in reactor, time for adding is 30min, esterification and transesterification reaction reflux, control the temperature of cooling water in reflux exchanger, the water that esterification is generated is taken away by vacuum, glycerine condensing reflux, esterification and transesterification reaction are after 5 hours, and by reaction product stratification 45min, upper strata is glyceryl ester layer, and lower floor is glycerine and solid catalyst layer, emit successively glycerine and solid catalyst layer (30g) and glyceryl ester layer (108g).Glyceryl ester layer is by gas chromatographic analysis, and it consists of free fatty acids mass content is 0.45%, mono-glycerides mass content 60.56%, triglyceride mass content 31.29%, triglyceride level mass content 7.70%.Glycerine and solid catalyst layer turn back to step (1) and use as raw material.
(2) de-free fatty acids and the glycerine of glyceryl ester layer: will proceed to the charging stock tank of molecular distillation apparatus from the glyceryl ester layer of step (1) gained, the distillation temperature of first step molecular distillation is set as to 130 ℃, pressure is 1.0Pa, and the inner condenser temperature of first step molecular distillation is 60 ℃; Continuously feeding, unreacted glycerine and free fatty acids are distilled out of, and are collected as light phase byproduct (0.5g) after inner condenser condensation.Glyceryl ester, as the heavy phase not being distilled out of, continues to enter second stage molecular distillation.
(3) preparation of high-purity fatty acyl monoglyceride: the heavy phase glyceryl ester that step (2) gained is removed free fatty acids and glycerine enters in the molecular distillation of the second stage continuously, by the Temperature Setting of second stage molecular distillation, be 190 ℃, pressure is that the inner condenser temperature of 0.1Pa second stage molecular distillation is 70 ℃.Continuously feeding, fatty acyl monoglyceride is distilled out of, and is collected as light phase product 58g, mono-glycerides purity 94.64% after inner condenser condensation.Heavy phase is triglyceride and triglyceride level 49g, returns to step (1) and continues to use as raw material.
Embodiment 2
Synthetic and the purifying process route map of the present embodiment high-purity fatty acyl monoglyceride is as shown in Figure 2:
(1) fatty acyl monoglyceride is synthetic: get winterized stearin 80g, stearic acid 20g adds in reactor, adds SO
4 2-/ ZrO
2-Al
2o
3(preparation method is CN02151526.3 with reference to publication number to solid acid catalyst, name is called the Chinese patent of < < catalyzed by particle type solid superacid agent and preparation method > >) 0.2g, it is 400Pa that reactor is evacuated down to pressure, constantly stir simultaneously, when reaching 200 ℃ of temperature, temperature starts timing, by glycerine 48g (the lipid acid mole number in winterized stearin and stearic acid, with the ratio of glycerine mole number be 1: 1.5) be added drop-wise in reactor, time for adding is 40min, esterification and transesterification reaction reflux, control the temperature of cooling water in reflux exchanger, the water that esterification is generated is taken away by vacuum, glycerine condensing reflux, esterification and transesterification reaction are after 2 hours, by reaction product centrifugal 10min under 3000rpm.Upper strata is glyceryl ester layer (104g), and lower floor is glycerine and solid catalyst layer (43g).Glyceryl ester layer is by gas chromatographic analysis, and it consists of free fatty acids mass content is 0.29%, mono-glycerides mass content 52.14%, triglyceride mass content 31.64%, triglyceride level mass content 15.92%.Glycerine and solid catalyst layer turn back to step (1) and use as raw material.
(2) de-free fatty acids and the glycerine of glyceryl ester layer: will proceed to the charging stock tank of molecular distillation apparatus from the glyceryl ester layer of step (1) gained, the distillation temperature of first step molecular distillation is set as to 140 ℃, pressure is 10.0Pa, and the inner condenser temperature of first step molecular distillation is 70 ℃; Continuously feeding, unreacted glycerine and free fatty acids are distilled out of, and are collected as light phase byproduct (0.4g) after inner condenser condensation.Glyceryl ester, as the heavy phase not being distilled out of, continues to enter second stage molecular distillation.
(3) preparation of high-purity fatty acyl monoglyceride: the heavy phase glyceryl ester that step (2) gained is removed free fatty acids and glycerine enters in the molecular distillation of the second stage continuously, by the Temperature Setting of second stage molecular distillation, be 185 ℃, pressure is that the inner condenser temperature of 5.0Pa second stage molecular distillation is 70 ℃.Continuously feeding, fatty acyl monoglyceride is distilled out of, and is collected as light phase product 51g, mono-glycerides purity 97.87% after inner condenser condensation.Heavy phase is triglyceride and triglyceride level 50g, returns to step (1) for raw material continuation use.
Synthetic and the purifying process route map of the present embodiment high-purity fatty acyl monoglyceride is as shown in Figure 2:
(1) fatty acyl monoglyceride is synthetic: get stearic acid 100g and add in reactor, add SO
4 2-/ ZrO
2-Al
2o
3(preparation method is CN02151526.3 with reference to publication number to solid acid catalyst, name is called the Chinese patent of < < catalyzed by particle type solid superacid agent and preparation method > >) 0.5g, it is 10000Pa that reactor is evacuated down to pressure, constantly stir simultaneously, when reaching 230 ℃ of temperature, temperature starts timing, by glycerine 32g (the lipid acid mole number in stearic acid, with the ratio of glycerine mole number be 1: 1) be added drop-wise in reactor, time for adding is 45min, esterification and transesterification reaction reflux, control the temperature of cooling water in reflux exchanger, the water that esterification is generated is taken away by vacuum, glycerine condensing reflux, esterification and transesterification reaction, after 1 hour, by the standing 20min of reaction product, are emitted glycerine and solid catalyst layer (6.5g) and glyceryl ester layer (125g) successively.Glyceryl ester layer is by gas chromatographic analysis, and it consists of free fatty acids mass content is 2.18%, mono-glycerides mass content 67.01%, triglyceride mass content 22.25%, triglyceride level mass content 9.01%.Glycerine and solid catalyst layer turn back to step (1) and use as raw material.
(2) de-free fatty acids and the glycerine of glyceryl ester layer: will proceed to the charging stock tank of molecular distillation apparatus from the glyceryl ester layer of step (1) gained, the distillation temperature of first step molecular distillation is set as to 120 ℃, pressure is 3.0Pa, and the inner condenser temperature of first step molecular distillation is 70 ℃; Continuously feeding, unreacted glycerine and free fatty acids are distilled out of, and are collected as light phase byproduct (2.5g) after inner condenser condensation.Glyceryl ester, as the heavy phase not being distilled out of, continues to enter second stage molecular distillation.
(3) preparation of high-purity fatty acyl monoglyceride: the heavy phase glyceryl ester that step (2) gained is removed free fatty acids and glycerine enters in the molecular distillation of the second stage continuously, by the Temperature Setting of second stage molecular distillation, be 180 ℃, pressure is that the inner condenser temperature of 0.2Pa second stage molecular distillation is 75 ℃.Continuously feeding, fatty acyl monoglyceride is distilled out of, and is collected as light phase product 82g, mono-glycerides purity 96.46% after inner condenser condensation.Heavy phase is triglyceride and triglyceride level 42g, returns to step (1) for raw material continuation use.
Embodiment 4
Synthetic and the purifying process route map of the present embodiment high-purity fatty acyl monoglyceride is as shown in Figure 2:
(1) fatty acyl monoglyceride is synthetic: get stearic acid 100g and add in reactor, add SO
4 2-/ ZrO
2-Al
2o
3(preparation method is CN02151526.3 with reference to publication number to solid acid catalyst, name is called the Chinese patent of < < catalyzed by particle type solid superacid agent and preparation method > >) 0.5g, it is 10000Pa that reactor is evacuated down to pressure, constantly stir simultaneously, when reaching 230 ℃ of temperature, temperature starts timing, by glycerine 32g (the lipid acid mole number in stearic acid, with the ratio of glycerine mole number be 1: 1) be added drop-wise in reactor, time for adding is 45min, esterification and transesterification reaction reflux, control the temperature of cooling water in reflux exchanger, the water that esterification is generated is taken away by vacuum, glycerine condensing reflux, esterification and transesterification reaction, after 1 hour, by the standing 20min of reaction product, are emitted glycerine and solid catalyst layer (6.5g) and glyceryl ester layer (125g) successively.Glyceryl ester layer is by gas chromatographic analysis, and it consists of free fatty acids mass content is 2.18%, mono-glycerides mass content 67.01%, triglyceride mass content 22.25%, triglyceride level mass content 9.01%.Glycerine and solid catalyst layer turn back to step (1) and use as raw material.
(2) de-free fatty acids and the glycerine of glyceryl ester layer: will proceed to the charging stock tank of molecular distillation apparatus from the glyceryl ester layer of step (1) gained, the distillation temperature of first step molecular distillation is set as to 120 ℃, pressure is 3.0Pa, and the inner condenser temperature of first step molecular distillation is 70 ℃; Continuously feeding, unreacted glycerine and free fatty acids are distilled out of, and are collected as light phase byproduct (2.5g) after inner condenser condensation.Glyceryl ester, as the heavy phase not being distilled out of, continues to enter second stage molecular distillation.
(3) preparation of high purity stearyl direactive glyceride: the heavy phase glyceryl ester that step (2) gained is removed free fatty acids and glycerine enters in the molecular distillation of the second stage continuously, by the Temperature Setting of second stage molecular distillation, be 180 ℃, pressure is that the inner condenser temperature of 0.2Pa second stage molecular distillation is 75 ℃.Continuously feeding, stearyl direactive glyceride is distilled out of, and is collected as light phase product 82g, mono-glycerides purity 96.46% after inner condenser condensation.Heavy phase is triglyceride and triglyceride level 42g, returns to step (1) for raw material continuation use.
Embodiment 5
Synthetic and the purifying process route map of the present embodiment high-purity fatty acyl monoglyceride is as shown in Figure 2:
(1) fatty acyl monoglyceride is synthetic: get 40g fish oil and 60g fish oil fatty acid adds in reactor, add SO
4 2-/ ZrO
2-Al
2o
3(preparation method is CN02151526.3 with reference to publication number to solid acid catalyst, name is called the Chinese patent of < < catalyzed by particle type solid superacid agent and preparation method > >) 0.2g, it is 10000Pa that reactor is evacuated down to pressure, constantly stir simultaneously, when reaching 220 ℃ of temperature, temperature starts timing, by glycerine 96g (the lipid acid mole number in fish oil and fish oil fatty acid, with the ratio of glycerine mole number be 1: 3) be added drop-wise in reactor, time for adding is 40min, esterification and transesterification reaction reflux, control the temperature of cooling water in reflux exchanger, the water that esterification is generated is taken away by vacuum, glycerine condensing reflux, esterification and transesterification reaction, after 5 hours, by the standing 30min of reaction product, are emitted glycerine and solid catalyst layer (83g) and glyceryl ester layer (112g) successively.Glyceryl ester layer is by gas chromatographic analysis, and it consists of free fatty acids mass content is 0.47%, mono-glycerides mass content 62.05%, triglyceride mass content 30.49%, triglyceride level mass content 7.03%.Glycerine and solid catalyst layer turn back to step (1) and use as raw material.
(2) de-free fatty acids and the glycerine of glyceryl ester layer: will proceed to the charging stock tank of molecular distillation apparatus from the glyceryl ester layer of step (1) gained, the distillation temperature of first step molecular distillation is set as to 160 ℃, pressure is 20.0Pa, and the inner condenser temperature of first step molecular distillation is 70 ℃; Continuously feeding, unreacted glycerine and free fatty acids are distilled out of, and are collected as light phase byproduct (0.5g) after inner condenser condensation.Glyceryl ester, as the heavy phase not being distilled out of, continues to enter second stage molecular distillation.
(3) preparation of high-purity fatty acyl monoglyceride: the heavy phase glyceryl ester that step (2) gained is removed free fatty acids and glycerine enters in the molecular distillation of the second stage continuously, by the Temperature Setting of second stage molecular distillation, be 200 ℃, pressure is that the inner condenser temperature of 0.5Pa second stage molecular distillation is 75 ℃.Continuously feeding, fatty acyl monoglyceride is distilled out of, and is collected as light phase product 66g, mono-glycerides purity 95.64% after inner condenser condensation.Heavy phase is triglyceride and triglyceride level 45g, returns to step (1) for raw material continuation use.The gas chromatogram of product as shown in Figure 3.
The gas chromatogram of Fig. 3 high product purity fatty acyl mono-glycerides, wherein FFA represents free fatty acids, and MAG represents fatty acyl monoglyceride, and DAG represents triglyceride.
Embodiment 6
Synthetic and the purifying process route map of the present embodiment high-purity fatty acyl monoglyceride is as shown in Figure 2:
(1) fatty acyl monoglyceride is synthetic: get 50g plant blend oil (compound lard of soya-bean oil, plam oil, rapeseed oil and sunflower seed oil) and 50g vegetable fatty acids and add in reactor, add SO
4 2-/ ZrO
2-Al
2o
3(preparation method is CN02151526.3 with reference to publication number to solid acid catalyst, name is called the Chinese patent of < < catalyzed by particle type solid superacid agent and preparation method > >) 0.4g, it is 10000Pa that reactor is evacuated down to pressure, constantly stir simultaneously, when reaching 190 ℃ of temperature, temperature starts timing, by glycerine 48g (the lipid acid mole number in plant blend oil and vegetable fatty acids, with the ratio of glycerine mole number be 1: 1.5) be added drop-wise in reactor, time for adding is 20min, esterification and transesterification reaction reflux, control the temperature of cooling water in reflux exchanger, the water that esterification is generated is taken away by vacuum, glycerine condensing reflux, esterification and transesterification reaction, after 2.5 hours, are filtered reaction product while hot by vacuum filtration, the standing 35min of filtrate emits glycerine (36g) and glyceryl ester layer (110g) successively.Glyceryl ester layer is by gas chromatographic analysis, and it consists of free fatty acids mass content is 0.39%, mono-glycerides mass content 57.38%, triglyceride mass content 31.37%, triglyceride level mass content 10.57%.Glycerin layer turns back to step (1) and uses as raw material.
(2) de-free fatty acids and the glycerine of glyceryl ester layer: will proceed to the charging stock tank of molecular distillation apparatus from the glyceryl ester layer of step (1) gained, the distillation temperature of first step molecular distillation is set as to 150 ℃, pressure is 10.0Pa, and the inner condenser temperature of first step molecular distillation is 70 ℃; Continuously feeding, unreacted glycerine and free fatty acids are distilled out of, and are collected as light phase byproduct (0.5g) after inner condenser condensation.Glyceryl ester, as the heavy phase not being distilled out of, continues to enter second stage molecular distillation.
(3) preparation of high-purity fatty acyl monoglyceride: the heavy phase glyceryl ester that step (2) gained is removed free fatty acids and glycerine enters in the molecular distillation of the second stage continuously, by the Temperature Setting of second stage molecular distillation, be 220 ℃, pressure is that the inner condenser temperature of 1.0Pa second stage molecular distillation is 75 ℃.Continuously feeding, fatty acyl monoglyceride is distilled out of, and is collected as light phase product 63g, mono-glycerides purity 92.28% after inner condenser condensation.Heavy phase is triglyceride and triglyceride level 36g, returns to step (1) for raw material continuation use.
Embodiment 7
Synthetic and the purifying process route map of the present embodiment high-purity fatty acyl monoglyceride is as shown in Figure 2:
(1) fatty acyl monoglyceride is synthetic: get 70g plam oil and 30g palm oil fatty acid adds in reactor, add SO
4 2-/ ZrO
2-Al
2o
3(preparation method is CN02151526.3 with reference to publication number to solid acid catalyst, name is called the Chinese patent of < < catalyzed by particle type solid superacid agent and preparation method > >) 0.4g, it is 1000Pa that reactor is evacuated down to pressure, constantly stir simultaneously, when reaching 190 ℃ of temperature, temperature starts timing, by glycerine 64g (the lipid acid mole number in plam oil and palm oil fatty acid, with the ratio of glycerine mole number be 1: 2) be added drop-wise in reactor, time for adding is 30min, esterification and transesterification reaction reflux, control the temperature of cooling water in reflux exchanger, the water that esterification is generated is taken away by vacuum, glycerine condensing reflux, esterification and transesterification reaction, after 2 hours, are filtered reaction product while hot by vacuum filtration, the standing 40min of filtrate emits glycerine (48g) and glyceryl ester layer (115g) successively.Glyceryl ester layer is by gas chromatographic analysis, and it consists of free fatty acids mass content is 0.89%, mono-glycerides mass content 61.97%, triglyceride mass content 24.23%, triglyceride level mass content 12.90%.Glycerin layer turns back to step (1) and uses as raw material.
(2) de-free fatty acids and the glycerine of glyceryl ester layer: will proceed to the charging stock tank of molecular distillation apparatus from the glyceryl ester layer of step (1) gained, the distillation temperature of first step molecular distillation is set as to 140 ℃, pressure is 2.0Pa, and the inner condenser temperature of first step molecular distillation is 70 ℃; Continuously feeding, unreacted glycerine and free fatty acids are distilled out of, and are collected as light phase byproduct (1.0g) after inner condenser condensation.Glyceryl ester, as the heavy phase not being distilled out of, continues to enter second stage molecular distillation.
(3) preparation of high-purity fatty acyl monoglyceride: the heavy phase glyceryl ester that step (2) gained is removed free fatty acids and glycerine enters in the molecular distillation of the second stage continuously, by the Temperature Setting of second stage molecular distillation, be 210 ℃, pressure is that the inner condenser temperature of 0.5Pa second stage molecular distillation is 75 ℃.Continuously feeding, fatty acyl monoglyceride is distilled out of, and is collected as light phase product 68g, mono-glycerides purity 93.67% after inner condenser condensation.Heavy phase is triglyceride and triglyceride level 35g, returns to step (1) for raw material continuation use.
Embodiment 8
Synthetic and the purifying process route map of the present embodiment high-purity fatty acyl monoglyceride is as shown in Figure 2:
(1) fatty acyl monoglyceride is synthetic: get 60g sunflower seed oil and 40g sunflower seed oil lipid acid adds in reactor, add SO
4 2-/ ZrO
2-Al
2o
3(preparation method is CN02151526.3 with reference to publication number to solid acid catalyst, name is called the Chinese patent of < < catalyzed by particle type solid superacid agent and preparation method > >) 0.3g, it is 2000Pa that reactor is evacuated down to pressure, constantly stir simultaneously, when reaching 200 ℃ of temperature, temperature starts timing, by glycerine 48g (the lipid acid mole number in sunflower seed oil and sunflower seed oil lipid acid, with the ratio of the mole number of glycerine be 1: 1.5) be added drop-wise in reactor, time for adding is 30min, esterification and transesterification reaction reflux, control the temperature of cooling water in reflux exchanger, the water that esterification is generated is taken away by vacuum, glycerine condensing reflux, esterification and transesterification reaction, after 3 hours, by the standing 60min of reaction product, are emitted glycerine (31g) and glyceryl ester layer (116g) successively.Glyceryl ester layer is by gas chromatographic analysis, and it consists of free fatty acids mass content is 0.37%, mono-glycerides mass content 63.27%, triglyceride mass content 23.25%, triglyceride level mass content 13.13%.Glycerin layer turns back to step (1) and uses as raw material.
(2) de-free fatty acids and the glycerine of glyceryl ester layer: will proceed to the charging stock tank of molecular distillation apparatus from the glyceryl ester layer of step (1) gained, the distillation temperature of first step molecular distillation is set as to 130 ℃, pressure is 1.0Pa, and the inner condenser temperature of first step molecular distillation is 70 ℃; Continuously feeding, unreacted glycerine and free fatty acids are distilled out of, and are collected as light phase byproduct (0.4g) after inner condenser condensation.Glyceryl ester, as the heavy phase not being distilled out of, continues to enter second stage molecular distillation.
(3) preparation of high-purity fatty acyl monoglyceride: the heavy phase glyceryl ester that step (2) gained is removed free fatty acids and glycerine enters in the molecular distillation of the second stage continuously, by the Temperature Setting of second stage molecular distillation, be 200 ℃, pressure is that the inner condenser temperature of 0.5Pa second stage molecular distillation is 75 ℃.Continuously feeding, fatty acyl monoglyceride is distilled out of, and is collected as light phase product 69g, mono-glycerides purity 95.25% after inner condenser condensation.Heavy phase is triglyceride and triglyceride level 35g, returns to step (1) for raw material continuation use.
Embodiment 9
Synthetic and the purifying process route map of the present embodiment high-purity fatty acyl monoglyceride is as shown in Figure 2:
(1) fatty acyl monoglyceride is synthetic: get oleic acid 100g and add in reactor, add SO
4 2-/ ZrO
2-Al
2o
3(preparation method is CN02151526.3 with reference to publication number to solid acid catalyst, name is called the Chinese patent of < < catalyzed by particle type solid superacid agent and preparation method > >) 0.3g, it is 1000Pa that reactor is evacuated down to pressure, constantly stir simultaneously, when reaching 230 ℃ of temperature, temperature starts timing, by glycerine 32g (the lipid acid mole number in oleic acid, with the ratio of glycerine mole number be 1: 1) be added drop-wise in reactor, time for adding is 40min, esterification and transesterification reaction reflux, control the temperature of cooling water in reflux exchanger, the water that esterification is generated is taken away by vacuum, glycerine condensing reflux, esterification and transesterification reaction, after 2.5 hours, by the standing 20min of reaction product, are emitted glycerine and solid catalyst layer (6.3g) and glyceryl ester layer (125g) successively.Glyceryl ester layer is by gas chromatographic analysis, and it consists of free fatty acids mass content is 1.94%, mono-glycerides mass content 64.52%, triglyceride mass content 25.50%, triglyceride level mass content 9.04%.Glycerine and solid catalyst layer turn back to step (1) and use as raw material.
(2) de-free fatty acids and the glycerine of glyceryl ester layer: will proceed to the charging stock tank of molecular distillation apparatus from the glyceryl ester layer of step (1) gained, the distillation temperature of first step molecular distillation is set as to 130 ℃, pressure is 2.0Pa, and the inner condenser temperature of first step molecular distillation is 70 ℃; Continuously feeding, unreacted glycerine and free fatty acids are distilled out of, and are collected as light phase byproduct (2.3g) after inner condenser condensation.Glyceryl ester, as the heavy phase not being distilled out of, continues to enter second stage molecular distillation.
(3) preparation of high purity oleoyl direactive glyceride: the heavy phase glyceryl ester that step (2) gained is removed free fatty acids and glycerine enters in the molecular distillation of the second stage continuously, by the Temperature Setting of second stage molecular distillation, be 185 ℃, pressure is that the inner condenser temperature of 0.3Pa second stage molecular distillation is 60 ℃.Continuously feeding, fatty acyl monoglyceride is distilled out of, and is collected as light phase product 81g, mono-glycerides purity 96.68% after inner condenser condensation.Heavy phase is triglyceride and triglyceride level 43g, returns to step (1) for raw material continuation use.
Above-described embodiment is preferably embodiment of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and principle, substitutes, combination, simplify; all should be equivalent substitute mode, within being included in protection scope of the present invention.
Claims (9)
1. synthesizing and a purification process of high-purity fatty acyl monoglyceride, it is characterized in that comprising following operation steps:
(1) fatty acyl monoglyceride is synthetic: after grease, free fatty acids and solid catalyst are mixed, reaction system is evacuated to pressure 400～10000Pa, stirs and is warming up to 170～230 ℃, obtains rich mixture; Adopt dropping mode to add in rich mixture glycerine, esterification and transesterification reaction reflux under vacuum condition; Control the temperature of cooling water in reflux exchanger, the water that esterification is generated is taken away by vacuum, glycerine condensing reflux; By reaction product layering, upper strata is glyceryl ester layer; The addition of described solid catalyst is 0.1～0.5% of grease and free fatty acids total mass;
(2) de-free fatty acids and the glycerine of glyceryl ester layer: step (1) gained glyceryl ester layer is removed to unreacted free fatty acids and glycerine by first step molecular distillation;
(3) preparation of high-purity fatty acyl monoglyceride: the glyceryl ester layer of step (2) gained being removed to free fatty acids and glycerine enters second stage molecular distillation, obtains distillment and steams excess; Described distillment is high-purity fatty acyl monoglyceride, and steaming excess is triglyceride and triglyceride level; Purity >=92.28% of described high-purity fatty acyl monoglyceride.
2. the synthetic and purification process of a kind of high-purity fatty acyl monoglyceride according to claim 1, is characterized in that: the described grease of step (1) is winterized stearin, vegetables oil or fish oil; Described free fatty acids is a kind of or its mixture in stearic acid, oleic acid, palmitinic acid, linolic acid, linolenic acid and oleic acid.
3. the synthetic and purification process of a kind of high-purity fatty acyl monoglyceride according to claim 2, is characterized in that: described vegetables oil is a kind of or its mixture in soybean oil, peanut oil, sunflower seed oil, plam oil and rapeseed oil.
4. the synthetic and purification process of a kind of high-purity fatty acyl monoglyceride according to claim 1, is characterized in that: described in step (1), be layered as centrifugal layering, stratification or filter rear stratification; If adopt centrifugal layering or stratification, the lower floor obtaining is solid catalyst and glycerin layer; Stratification after filtering if adopt, the lower floor obtaining is glycerin layer.
5. the synthetic and purification process of a kind of high-purity fatty acyl monoglyceride according to claim 1, is characterized in that: the described free fatty acids of step (1) accounts for 20～100% of grease and free fatty acids total mass; Lipid acid mole number in described grease and free fatty acids, with the ratio of the mole number of glycerine be 1:1～1:3; It is described that glycerine is adopted to the time that dropping mode adds is 20～45min; The temperature of described esterification and transesterification reaction is 170～230 ℃, and the reaction times is 1～5 hour, and reaction pressure is 400～10000Pa; The temperature of the water coolant in described reflux exchanger is 30～80 ℃; The time of described stratification is 30～60min; The centrifugal speed of described centrifugal layering is 3000r/min, and the time is 10～15min.
6. the synthetic and purification process of a kind of high-purity fatty acyl monoglyceride according to claim 1, is characterized in that: the described free fatty acids of step (1) accounts for 40% of grease and free fatty acids total mixture quality; Lipid acid mole number in described grease and free fatty acids, with the ratio of the mole number of glycerine be 1:1.5; The addition of described solid catalyst is 0.2% of free fatty acids and grease total mass; It is described that glycerine is adopted to the time that dropping mode adds is 30min; The temperature of described esterification and transesterification reaction is 200 ℃, and the reaction times is 4 hours, and reaction pressure is 5000Pa; The temperature of the water coolant in described reflux exchanger is 50 ℃; The described stratification time is 45min; The centrifugal speed of described centrifugal layering is 3000r/min, and the time is 15min.
7. the synthetic and purification process of a kind of high-purity fatty acyl monoglyceride according to claim 1, is characterized in that: the temperature of the described first step molecular distillation of step (2) is 120～160 ℃, and distillation pressure is 1～20Pa; The temperature of the described second stage of step (3) molecular distillation is 180～220 ℃, and distillation pressure is 0.1～5Pa.
8. the synthetic and purification process of a kind of high-purity fatty acyl monoglyceride according to claim 1, is characterized in that: the temperature of the described first step molecular distillation of step (2) is 150 ℃, and distillation pressure is 5Pa; The temperature of the described second stage of step (3) molecular distillation is 200 ℃, and distillation pressure is 0.5Pa.
9. the synthetic and purification process of a kind of high-purity fatty acyl monoglyceride according to claim 1, is characterized in that: the described solid catalyst of step (1) is granule type SO
4 2-/ M
xo
ytype solid super acid catalyst, its granule type carrier is carrier is Al
2o
3, SiO
2or Al
2o
3-SiO
2composite oxides, its active carrier is ZrO
2, TiO
2, SnO
2, ZrO
2-TiO
2composite oxides, ZrO
2-SnO
2composite oxides or TiO
2-SnO
2composite oxides.
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