CN109022145A - A kind of preparation method of the serial grease of zero plasticiser Ω -3 of low-peroxide value, Ω -6 - Google Patents
A kind of preparation method of the serial grease of zero plasticiser Ω -3 of low-peroxide value, Ω -6 Download PDFInfo
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- CN109022145A CN109022145A CN201810958708.6A CN201810958708A CN109022145A CN 109022145 A CN109022145 A CN 109022145A CN 201810958708 A CN201810958708 A CN 201810958708A CN 109022145 A CN109022145 A CN 109022145A
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- Prior art keywords
- grease
- plasticiser
- peroxide value
- zero
- low
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- 239000004519 grease Substances 0.000 title claims abstract description 73
- 239000004014 plasticizer Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000004821 distillation Methods 0.000 claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 27
- 239000002253 acid Substances 0.000 claims abstract description 26
- 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 abstract description 13
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000001301 oxygen Substances 0.000 claims abstract description 10
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 10
- 150000002978 peroxides Chemical class 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 10
- 239000004615 ingredient Substances 0.000 claims abstract description 8
- 229930182558 Sterol Natural products 0.000 claims abstract description 7
- 235000020661 alpha-linolenic acid Nutrition 0.000 claims abstract description 7
- 229960004488 linolenic acid Drugs 0.000 claims abstract description 7
- 150000003432 sterols Chemical class 0.000 claims abstract description 7
- 235000003702 sterols Nutrition 0.000 claims abstract description 7
- 238000007599 discharging Methods 0.000 claims description 17
- 239000003344 environmental pollutant Substances 0.000 claims description 13
- 231100000719 pollutant Toxicity 0.000 claims description 13
- 238000002203 pretreatment Methods 0.000 claims description 13
- 238000000275 quality assurance Methods 0.000 claims description 8
- 239000012535 impurity Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 5
- 230000000694 effects Effects 0.000 claims description 4
- 239000000356 contaminant Substances 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- KQQKGWQCNNTQJW-UHFFFAOYSA-N linolenic acid Natural products CC=CCCC=CCC=CCCCCCCCC(O)=O KQQKGWQCNNTQJW-UHFFFAOYSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 24
- VMSLCPKYRPDHLN-UHFFFAOYSA-N (R)-Humulone Chemical class CC(C)CC(=O)C1=C(O)C(CC=C(C)C)=C(O)C(O)(CC=C(C)C)C1=O VMSLCPKYRPDHLN-UHFFFAOYSA-N 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000000050 nutritive effect Effects 0.000 abstract description 3
- 239000008171 pumpkin seed oil Substances 0.000 abstract description 2
- 230000000717 retained effect Effects 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 235000019495 Pecan oil Nutrition 0.000 abstract 1
- 235000021324 borage oil Nutrition 0.000 abstract 1
- 238000005265 energy consumption Methods 0.000 abstract 1
- 235000008524 evening primrose extract Nutrition 0.000 abstract 1
- 239000010475 evening primrose oil Substances 0.000 abstract 1
- 229940089020 evening primrose oil Drugs 0.000 abstract 1
- 239000008169 grapeseed oil Substances 0.000 abstract 1
- 235000021388 linseed oil Nutrition 0.000 abstract 1
- 239000000944 linseed oil Substances 0.000 abstract 1
- 239000010470 pecan oil Substances 0.000 abstract 1
- 239000001335 perilla frutescens leaf extract Substances 0.000 abstract 1
- 239000013557 residual solvent Substances 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 22
- 235000019198 oils Nutrition 0.000 description 22
- 230000008569 process Effects 0.000 description 10
- 238000012545 processing Methods 0.000 description 10
- 241000196324 Embryophyta Species 0.000 description 7
- 230000003647 oxidation Effects 0.000 description 7
- 238000007254 oxidation reaction Methods 0.000 description 7
- 238000000199 molecular distillation Methods 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 235000019197 fats Nutrition 0.000 description 5
- 239000000194 fatty acid Substances 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 230000006378 damage Effects 0.000 description 4
- 230000036541 health Effects 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000000498 cooling water Substances 0.000 description 3
- 235000014113 dietary fatty acids Nutrition 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229930195729 fatty acid Natural products 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 239000004803 Di-2ethylhexylphthalate Substances 0.000 description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical group CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 150000001299 aldehydes Chemical class 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 2
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- VZCCETWTMQHEPK-UHFFFAOYSA-N gamma-Linolensaeure Natural products CCCCCC=CCC=CCC=CCCCCC(O)=O VZCCETWTMQHEPK-UHFFFAOYSA-N 0.000 description 2
- VZCCETWTMQHEPK-QNEBEIHSSA-N gamma-linolenic acid Chemical compound CCCCC\C=C/C\C=C/C\C=C/CCCCC(O)=O VZCCETWTMQHEPK-QNEBEIHSSA-N 0.000 description 2
- 235000020664 gamma-linolenic acid Nutrition 0.000 description 2
- 229960002733 gamolenic acid Drugs 0.000 description 2
- 150000002432 hydroperoxides Chemical class 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 238000005502 peroxidation Methods 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 239000011782 vitamin Substances 0.000 description 2
- 229940088594 vitamin Drugs 0.000 description 2
- 229930003231 vitamin Natural products 0.000 description 2
- 235000013343 vitamin Nutrition 0.000 description 2
- 150000003722 vitamin derivatives Chemical class 0.000 description 2
- 244000144730 Amygdalus persica Species 0.000 description 1
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- CTKINSOISVBQLD-UHFFFAOYSA-N Glycidol Chemical compound OCC1CO1 CTKINSOISVBQLD-UHFFFAOYSA-N 0.000 description 1
- 240000006240 Linum usitatissimum Species 0.000 description 1
- 235000004431 Linum usitatissimum Nutrition 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 235000004347 Perilla Nutrition 0.000 description 1
- 244000124853 Perilla frutescens Species 0.000 description 1
- 235000006040 Prunus persica var persica Nutrition 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000007059 acute toxicity Effects 0.000 description 1
- 231100000403 acute toxicity Toxicity 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- -1 alcohol epoxides Chemical class 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 238000006701 autoxidation reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000019636 bitter flavor Nutrition 0.000 description 1
- 208000026106 cerebrovascular disease Diseases 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007665 chronic toxicity Effects 0.000 description 1
- 231100000160 chronic toxicity Toxicity 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 239000008157 edible vegetable oil Substances 0.000 description 1
- 230000002526 effect on cardiovascular system Effects 0.000 description 1
- 229940011871 estrogen Drugs 0.000 description 1
- 239000000262 estrogen Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 210000001161 mammalian embryo Anatomy 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 150000003022 phthalic acids Chemical class 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000010773 plant oil Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 230000001850 reproductive effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 210000001625 seminal vesicle Anatomy 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 235000010692 trans-unsaturated fatty acids Nutrition 0.000 description 1
- 210000001177 vas deferen Anatomy 0.000 description 1
- 201000010653 vesiculitis Diseases 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/12—Refining fats or fatty oils by distillation
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/008—Refining fats or fatty oils by filtration, e.g. including ultra filtration, dialysis
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention proposes a kind of preparation methods of the serial grease of zero plasticiser Ω -3 of low-peroxide value, Ω -6, while reducing the peroxide value and acid value of the serial grease (such as evening primrose oil, Purple Perilla Seed Oil, pumpkin seed oil, linseed oil, pecan oil, borage oil, grape seed oil) of Ω -3, Ω -6.Using the method for second distillation, the removal rate of plasticiser can achieve 100%.This method uses physical separation method, the characteristics of being distilled using low temperature molecular, it can effectively reduce acid value and peroxide value, it is completely removed plasticiser and residual solvent, it is effectively retained natural battalion's oxygen composition in material simultaneously, effectively the nutritive value of holding alpha linolenic acid, acid and gamma-linolenic and natural ingredient VE, sterol substance etc..This method saves energy consumption, simple and effective, and production cost can be greatly reduced, obtain the food-grade grease of high quality.
Description
Technical field
The present invention relates to the removal technology fields of plasticiser, concretely relate to a kind of zero plasticiser of low-peroxide value
The preparation method of Ω -3, Ω -6 series grease.
Background technique
Phthalate plasticiser (Phthalic Acid Esters, PAEs) is a kind of Environmental estrogen substance,
PAEs is generally colorless and transparent oily thick liquid, is soluble in organic solvent, and synthesis is usually to be urged by naphthalene and ortho-xylene
Change oxidation and generates phthalic anhydride, then phthalic anhydride and various alcohols are esterified and obtain, although, though PAEs is to human body
There is no acute toxicity so, but the chronic toxicity of long-term accumulation especially can not be ignored the toxicity of reproductive development in human body.Research
It was found that adjacent benzene class plasticiser can cause buck vas deferens, seminal vesicle and prostatic function abnormal, embryo furthermore may also result in
Tire slow growth and deformity.
Oxidation of Fat and Oils is to take hydrogen atom away on easily-activated unsaturated double-bond alpha-methylene and be oxidized to fat certainly first
It by base (R), and is further oxidized to peroxylradicals (ROO), the latter forms hydroperoxides with non-oxidation of fat again
(ROOH) and fatty free radical, such successive reaction make fatty constantly oxidation.Hydroperoxides are main as lipid autoxidation
Initial stage product less stable, it through it is many it is complicated divide and interaction, ultimately form small molecule volatile substance, as aldehyde, ketone,
Acid, alcohol epoxides such as aggregate into polymer, while promoting pigment fragrance matter and vitamin at the oxidation, cause grease completely sour
It loses.Often with having special foul smell and bitter flavour, extreme influence grease organoleptic properties make these rancid products produced by Oxidation of Fat and Oils
It declines to a great extent at its nutritive value；Very big harm is generated to human health simultaneously, such as promotes aging, cause cardiovascular and cerebrovascular disease and
Tumour etc..Ω -3, Ω -6 series oil peroxidation value are indicated with active oxygen milliequivalent in every kilogram of grease, therefore peroxide
Change value is to judge grease freshness and credit rating major criterion.
Acid value is one important sanitary index of grease.Under normal circumstances, slightly raising will not for acid value in edible vegetable oil
It causes damages to human health, but such as occurs serious rotten, generated aldehyde, ketone, acid can destroy liposoluble vitamin, make oil
The nutritive value of rouge is greatly lowered, and eats the digestion and absorption function of rear shadow noon human normal, and may generate to the health of human body
Adverse effect.In order to ensure oil quality and edible safety, defined in China food plant oil standard at present more stringent
The limitation of acid value of oil and fat.Dissolvent residual in oil production increases the financial burden of enterprise, wastes non-renewable
Resource can not only cause great harm if cannot effectively recycle to environment, can also endanger to the health care belt of consumer
Evil, and there may be the disasters such as explosion for a large amount of dissolvent residual.Countries in the world man, grease production enterprise, consumer, Chinese Ministry of Environmental Protection
Door and security department etc. treat the problem of solvent residual of grease all most seriously.
Chinese invention patent (application publication number: CN105925371A, data of publication of application: 2016.09.07) reports entitled
A kind of serial grease processing technique of Ω -3, the Ω -6 for reducing content of trans fatty acids and removing plasticiser, discloses bleached oil
Filtering is then by deacid-deodoring, the de- modeling of level-one, the de- modeling of second level, fatty acid and plasticiser trapping processing product oil is cooling, filtering
The step of the product oil plasticiser index produced lower than national standard, wherein DBP≤0.04ppm, DEHP≤0.4ppm, trans-
Fatty acid rising value < 0.5%.Processing technology of the invention inhibits the formation of trans-fatty acid while removing plasticiser,
Reduce the content of trans-fatty acid.
Chinese invention patent (application publication number: CN205759880U, data of publication of application: 2016.12.07) reports entitled
A kind of drinks and the serial grease use plasticiser filtering fine purification machine of Ω -3, Ω -6 disclose drinks and the serial grease of Ω -3, Ω -6
With plasticiser filtering fine purification machine, including filter vat group is removed, the filter vat group includes filter vat, filter medium, inlet tube and goes out
Mouth pipe, the filter medium are contained in the filter vat, and the inlet tube is set to the filter vat relatively above, the outlet
Set on the opposite lower section of the filter vat, the filter vat group includes active carbon filter vat and sieve pore filter vat, the active carbon
Filter vat and the sieve pore filter vat are sequentially connected, and the filter medium includes active carbon and sieve pore filter medium, the activity
Charcoal and the sieve pore filter medium are respectively arranged on the active carbon filter vat and the sieve pore filter vat.The wine of the utility model
The serial grease of class and Ω -3, Ω -6 adds molecular sieve to add micro-porous resin with removing plasticiser filtering fine purification machine using active carbon, and absorption is former
Reason removes the exceeded content of plasticiser inside wine body and the serial grease of Ω -3, Ω -6.
Chinese invention patent (application publication number: CN105779122A, data of publication of application: 2016.07.20) reports one kind
Control or reduce grease in plasticiser technique and thus obtained grease, disclose by be added amino acids adsorbent and/
Or specific acid, the adsorbent content of phthalate plasticiser in grease can be reduced to it is permitted most
In the range of big residual quantity, operating process is simple, save the cost, fails all to deviate from the plasticiser in grease.
The method of existing removal plasticiser is less, and means are single, and equipment investment amount is larger, expensive, equipment loss
Seriously.And obtained oil peroxidation value, acid value is higher, or even part has dissolvent residual phenomenon, and oil quality is caused to decline.
The method of removing plasticiser prepared by the present invention, passes through the low temperature molecular distillation means of different temperatures gradient, it is ensured that obtain
Grease in zero content of plasticizing agent, meanwhile, can effectively ensure that low mistake in grease by the outlet temperature of the equipment means that sharply cool down
Oxidation number, low acid value are a kind of physical separating process for completely removing plasticiser and dissolvent residual, and can all retain in material
Natural battalion's oxygen composition (natural ingredient VE, sterol substance), do not lose alpha linolenic acid and acid and gamma-linolenic.The method section
The energy is saved, it is simple and effective, production cost can be greatly reduced, obtain the oil plant of high quality.
Summary of the invention
The invention discloses by Ω -3, Ω -6 grease is sequentially sent to pre-treatment steaming after accurately measuring by charging metering pump
Device, the distillation of primary distillation device, rectifier, energy-saving heat exchanger, fine filter are sent out, reaches and completely removes plasticiser and dissolvent residual purpose
Physical separating process.Guarantee to reduce peroxide value, low acid value simultaneously, all natural battalion oxygen composition retained in material is (natural
Antioxidant composition VE, sterol substance), alpha linolenic acid, gamma-linolenic acid content are not lost, obtain the oil plant of high quality；
A kind of preparation method of the serial grease of zero plasticiser Ω -3 of low-peroxide value, Ω -6, includes the following steps:
(1) equipment is opened, Ω -3, Ω -6 grease are pumped into flowmeter by charging metering, after metering pump precisely measures
By Ω -3, Ω -6 series grease is sequentially sent to energy-saving heat exchanger, pre-treatment evaporator；
(2) through pre-treatment evaporator treated Ω -3, Ω -6 series grease is sent into primary distillation device by intermediate pump 1 and is steamed
It evaporates, Ω -3 after being distillated some of the contaminants, Ω -6 series grease are sent into rectifier by intermediate pump 2；
(3) high-temperature material in rectifier sends energy-saving heat exchanger back to by discharging pump 3, and the effect of a preheating is played to charging
Fruit；
(4) by by the high-temperature grease after energy-saving heat exchanger be rapidly cooled to after quality assurance heat exchanger 25 DEG C with
Under；
(5) grease after cooling down passes through fine filter finally to guarantee that mechanicalness impurity is not exceeded.
Preferably, the preparation method of the serial grease of a kind of zero plasticiser Ω -3 of low-peroxide value, Ω -6, which is characterized in that
Include the following steps:
(1) setting of device parameter: machine parameter includes pre-treatment evaporator optimum temperature section: 150 DEG C~180 DEG C；
The optimum temperature section of primary distillation device, rectifier: 170 DEG C~180 DEG C；Vacuum degree≤10.0pa of primary distillation device, rectifying
Vacuum degree≤5.0pa of device；The best section of mass flow: 90~160L/H；Material outlet optimum temperature≤25 DEG C；Cooling follows
Ring coolant-temperature gage≤25 DEG C；
(2) the serial grease of Ω -3, Ω -6 pre-treatment evaporator: be can handle into water in material by pre-treatment evaporator
Point and some light component escaping gas, and preheated for the oil plant that will distill；
(3) primary distillation device: by the serial grease of the Ω -3 of primary distillation device, Ω -6 it is retortable go out about 70% plasticiser
It is distillated with pollutants such as dissolvent residuals by discharging pump 1；
(4) rectifier: rectifier can distill out the plasticiser and solvent of residue about 30% in the serial grease of Ω -3, Ω -6
Remaining pollutant is distillated by discharging pump 2；
(5) energy-saving heat exchanger: de- modeling treated high-temperature material is sent into after 100% removing pollutant by discharging pump 3
After energy-saving heat exchanger, it can play and recover energy, energy-efficient purpose；
(6) quality assurance heat exchanger: about 180 DEG C after de- modeling processing of high-temperature material is sent into quality assurance heat exchanger,
It is set to be rapidly cooled to 25 DEG C hereinafter, can effectively reduce the natural battalion in the acid value and peroxide value and whole reservation materials of grease
Oxygen composition (natural ingredient VE, sterol substance, alpha linolenic acid and acid and gamma-linolenic)；
(7) fine filter: the serial grease of obtained Ω -3, Ω -6 finally need to be by fine filter, to guarantee mechanicalness in oil plant
Impurity is not exceeded.
Beneficial effects of the present invention
1. of the present invention carry out separation plasticiser for pure physical method, it is ensured that residual without any chemical component
It stays, does not have the residual of solvent；
2. the method that the present invention uses molecular distillation, isolated temperature is relatively low, does not generate in subtractive process trans-
Fatty acid and glycidol rouge；For Ω -3, in Ω -6 course of oil processing, peroxide value, acid value is effectively reduced, can take off completely
Except plasticiser and remaining solvent；
3. the method that the present invention uses can all retain the natural composition in grease and not lose α flax
The content of acid, acid and gamma-linolenic, does not lose any beneficiating ingredient；
The novelty of invention:
1. molecular distillation technique is introduced into the serial grease of Ω -3, Ω -6, which can effectively remove Ω -3, Ω -6
Plasticiser in serial grease, the plasticiser in Ω -3, Ω -6 series grease processed using the technology and equipment can drop
It is as low as zero.Processing method takes physical method, exempts the harm of chemical reagent bring, reduces processing program, and step processing can be with
Complete multiple functions.
2. the equipment while plasticiser, retains nutritional ingredient in reducing the serial grease of Ω -3, Ω -6 to the greatest extent
(natural ingredient VE, sterol substance), does not lose alpha linolenic acid and acid and gamma-linolenic), it can effectively ensure that Ω -3, Ω -6
Low-peroxide value in serial grease.
Detailed description of the invention
The present invention will be further described below with reference to the drawings.
The process flow chart of the preparation method of a kind of zero plasticiser Ω -3 of low-peroxide value of Fig. 1, Ω -6 series grease；
The equipment schematic diagram of the preparation method of a kind of zero plasticiser Ω -3 of low-peroxide value of Fig. 2, Ω -6 series grease.
Specific embodiment
It describes the specific embodiments of the present invention in detail below with reference to the accompanying drawings.
In order to be more clear the objectives, technical solutions, and advantages of the present invention, below with reference to embodiment, the present invention is carried out
It is further described.It should be appreciated that described herein, the specific embodiments are only for explaining the present invention, is not used to limit this
Invention.
Process equipment figure of the invention referring to Fig. 1, operating process referring to Fig. 2, the embodiment of the present invention includes:
Embodiment 1
Low temperature molecular distillation removing Ω -3 is opened, the equipment of plasticiser, adjusts the technological parameter of equipment in Ω -6 grease,
Middle flowmeter 135L/H, 175 DEG C of primary distillation device temperature, 180 DEG C of rectifier temperature, the vacuum degree of primary distillation device≤
10.0pa, vacuum degree≤5.0pa of rectifier, 25 DEG C of cooling water temperature；It is fed when equipment executes when parameter reaches setting value
Material.Pumpkin seed oil is pumped into flowmeter by charging metering, and energy-saving heat exchanger is sent into after precisely measuring, and is re-fed into pre-treatment evaporation
Device is sent into the distillation of primary distillation device through intermediate pump 1, and primary distillation device distills out the pollutants such as about 70% plasticiser and dissolvent residual
It is distillated by discharging pump 1, remaining oil plant is sent into rectifier by intermediate pump 2, distills out remaining about 30% plasticiser, solvent by rectifier
Remaining pollutant is distillated by discharging pump 2, and the high-temperature material after 100% removing pollutant is sent into energy-saving heat exchanger by discharging pump 3
Afterwards, it is re-fed into quality assurance heat exchanger and about 180 DEG C of high-temperature material is rapidly cooled to 25 DEG C hereinafter, guaranteeing to reduce peroxidating
Value, acid value and full price retain natural battalion's oxygen composition in material, finally completely remove mechanicalness impurity by fine filter, obtain height
Quality grease.
Embodiment 2
Low temperature molecular distillation removing Ω -3 is opened, the equipment of plasticiser, adjusts the technological parameter of equipment in Ω -6 grease,
Middle flowmeter 90L/H, 175 DEG C of primary distillation device temperature, 180 DEG C of rectifier temperature, primary distillation device vacuum degree≤10.0pa,
25 DEG C of vacuum degree≤5.0pa, the cooling water temperature of rectifier；Feeding is carried out when equipment executes when parameter reaches setting value.Mountain core
Peach oil is pumped into flowmeter by charging metering, and energy-saving heat exchanger is sent into after precisely measuring, pre-treatment evaporator is re-fed into, in
Between pump 1 be sent into the distillation of primary distillation device, primary distillation device distills out the pollutants such as about 70% plasticiser and dissolvent residual by discharging
Pump 1 distillates, and remaining oil plant is sent into rectifier by intermediate pump 2, distills out remaining about 30% plasticiser, dissolvent residual by rectifier
Pollutant is distillated by discharging pump 2, after the high-temperature material after 100% removing pollutant is sent into energy-saving heat exchanger by discharging pump 3, then is sent
Enter quality assurance heat exchanger by about 180 DEG C of high-temperature material be rapidly cooled to 25 DEG C hereinafter, guarantee reduce peroxide value, acid value and
Full price retains natural battalion's oxygen composition in material, finally completely removes mechanicalness impurity by fine filter, obtains high quality grease.
Embodiment 3
Low temperature molecular distillation removing Ω -3 is opened, the equipment of plasticiser, adjusts the technological parameter of equipment in Ω -6 grease,
Middle flowmeter 90L/H, 175 DEG C of primary distillation device temperature, 180 DEG C of rectifier temperature, primary distillation device vacuum degree≤10.0pa,
25 DEG C of vacuum degree≤5.0pa, the cooling water temperature of rectifier；Feeding is carried out when equipment executes when parameter reaches setting value.Purple perilla
Oil is pumped into flowmeter by charging metering, and energy-saving heat exchanger is sent into after precisely measuring, pre-treatment evaporator is re-fed into, through centre
Pump 1 is sent into the distillation of primary distillation device, and primary distillation device distills out the pollutants such as about 70% plasticiser and dissolvent residual by discharging pump 1
It distillates, remaining oil plant is sent into rectifier by intermediate pump 2, and the dirt of remaining about 30% plasticiser, dissolvent residual is distilled out by rectifier
Dye object is distillated by discharging pump 2, after the high-temperature material after 100% removing pollutant is sent into energy-saving heat exchanger by discharging pump 3, is re-fed into
About 180 DEG C of high-temperature material is rapidly cooled to 25 DEG C hereinafter, guaranteeing to reduce peroxide value, acid value and complete by quality assurance heat exchanger
Valence retains natural battalion's oxygen composition in material, finally completely removes mechanicalness impurity by fine filter, obtains high quality grease.
Ω -3 of de- modeling processing is not carried out according to present invention process, the measurement data of Ω -6 grease is as shown in table 1.
Table 1 does not deviate from Ω -3 of plasticizer treats, the measurement index of Ω -6 grease
De- modeling is carried out treated Ω -3 according to present invention process, the measurement data of Ω -6 grease is as shown in table 2.
Table 2 deviates from Ω -3 of plasticizer treats, the measurement index of Ω -6 grease
It can be seen from table 1, table 2 in case study on implementation, three kinds of different greases are taken off by technique of the invention
After modeling processing, the content of acid value, peroxide value in grease is greatly lowered, meanwhile, DBP, DEHP contain in treated grease
Measure all zero.Thus it can illustrate that technique of the invention can guarantee that 100% de- modeling is handled for the de- modeling processing of grease.Due to
Present invention process is distilled using low temperature molecular, is protected by the way that about 180 DEG C after de- modeling processing of high-temperature material is sent into quality
Be rapidly cooled to after card heat exchanger 25 DEG C hereinafter, can significantly low-peroxide value and acid value, and remain day whole in material
So battalion oxygen composition (natural ingredient VE, sterol substance), and alpha linolenic acid, gamma-linolenic acid content are not damaged.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalent structure or equivalent flow shift made by bright specification and accompanying drawing content is applied directly or indirectly in other relevant skills
Art field is included in scope of patent protection of the invention.
Claims (7)
1. the preparation method of a kind of zero plasticiser Ω -3 of low-peroxide value, Ω -6 series grease, it is characterised in that including following step
It is rapid:
(1) equipment is opened, Ω -3, Ω -6 series grease are pumped into flowmeter by charging metering, after metering pump precisely measures
By Ω -3, Ω -6 series grease is sequentially sent to energy-saving heat exchanger, pre-treatment evaporator；
(2) through pre-treatment evaporator treated Ω -3, Ω -6 series grease is sent into the distillation of primary distillation device, quilt by intermediate pump 1
Ω -3 after distillating some of the contaminants, Ω -6 series grease are sent into rectifier by intermediate pump 2；
(3) high-temperature material in rectifier sends energy-saving heat exchanger back to by discharging pump 3, and the effect of a preheating is played to charging；
(4) 25 DEG C or less will be rapidly cooled to after quality assurance heat exchanger by the high-temperature grease after energy-saving heat exchanger；
(5) grease after cooling down passes through fine filter finally to guarantee that mechanicalness impurity is not exceeded.
2. the preparation method of zero plasticiser Ω -3 of a kind of low-peroxide value according to claim 1, Ω -6 series grease,
It is characterized in that, the machine parameter of the step (1) includes pre-treatment evaporator optimum temperature section: 150 DEG C~180 DEG C；It is primary
The optimum temperature section of distiller, rectifier: 170 DEG C~180 DEG C；Vacuum degree≤10.0pa of primary distillation device, rectifier
Vacuum degree≤5.0pa；The best section of mass flow: 90~160L/H；Material outlet optimum temperature≤25 DEG C；Cooling circulating water
Temperature≤25 DEG C, pre-treatment evaporator can handle moisture and some light component volatility in material in the step (1)
Gas, and preheated for the material that will be distilled.
3. the preparation method of zero plasticiser Ω -3 of a kind of low-peroxide value according to claim 1, Ω -6 series grease,
Be characterized in that, the primary distillation device in the step (2) it is retortable go out about 70% plasticiser and the pollutants such as dissolvent residual by
Discharging pump 1 distillates.
4. the preparation method of zero plasticiser Ω -3 of a kind of low-peroxide value according to claim 1, Ω -6 series grease,
It is characterized in that, the rectifier in the step (2) distills out the pollution of the plasticiser and dissolvent residual of residue about 30% in oil plant
Object is distillated by discharging pump 2.
5. the preparation method of zero plasticiser Ω -3 of a kind of low-peroxide value according to claim 1, Ω -6 series grease,
It is characterized in that, step (3) the high temperature material is sent into energy-saving heat exchanger by discharging pump 3 after 100% removing pollutant, can rise
To recovering energy, energy-efficient purpose.
6. the preparation method of zero plasticiser Ω -3 of a kind of low-peroxide value according to claim 1, Ω -6 series grease,
It is characterized in that, about 180 DEG C of high-temperature material in the step (4) is sent into quality assurance heat exchanger, it is rapidly cooled to
25 DEG C hereinafter, can effectively reduce the acid value and peroxide value and realization natural ingredient VE, sterol substance, α of grease
The reservation of the battalion such as linolenic acid and acid and gamma-linolenic oxygen composition.
7. the preparation method of zero plasticiser Ω -3 of a kind of low-peroxide value according to claim 1, Ω -6 series grease,
It is characterized in that, the oil plant in the step (5) need to finally pass through fine filter, to guarantee that mechanicalness impurity is not exceeded in oil plant.
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| CN113201397A (en) * | 2021-04-08 | 2021-08-03 | 四川国为制药有限公司 | Method for reducing plasticizer content in fish oil product |
| CN113528238A (en) * | 2021-08-31 | 2021-10-22 | 武汉绿林茶籽油有限公司 | Method for reducing plasticizer content in tea seed oil |
| CN113774094A (en) * | 2021-09-23 | 2021-12-10 | 江南大学 | Enzymatic synthesis method of medium-long chain triglyceride |
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