CN1050740A - The production method of refined mink fat - Google Patents

Abstract

The present invention extracts from mink fat and the method for refining ermine oil.Mink fat is through the decompression water extraction, and neutralization, reduced steam distill deodorization, and the refining ermine oil that operations such as high speed centrifugation and vacuum hydro-extraction make is preserved down at-5 ℃ and never degenerated substantially more than 1 year, satisfies the requirement of superior cosmetics, medical supplies.

Description

The production method of refined mink fat

The invention belongs to greasy extraction in the animal tallow.

The greasy composition of animal mink with and proportion, iodine number, saponification value, physico-chemical properties such as alkali compound amount, zero pour are not close with body fat, have again perviousness by force, very easily emulsification and do not have adhesivity, can fetter the characteristics such as effect of perfume molecules, thereby be the desirable feedstock of the external-applied ointment etc. of cosmetics, medicine.Because its character and characteristics, developing and enlarge in the potential use of aspects such as the very low temperature of the protection of the washing of fur and natural fiber, high leather goods, machinery is lubricated, thereby it also is a kind of important fine chemical material.The extracting method of mink oil is more, and primary is with the crude fat of mink direct heating melting, and gained ermine oil has heavier raw meat and disturbs flavor and very easily become sour and can't utilize.The external in recent years solvent-extraction process that successively proposes, boil and follow the example of and water-bath smelting process etc. all has certain advantage.J.V.Harispe mixes with the mink of rubbing is fatty with chloroform methanol, and stir down at 20 ℃ and extract, and after washing and under reduced pressure concentrated, yield reaches 90～95%(Fr.1405887 1964), this method need consume a large amount of organic solvents.The mink fat that D.H.Dupre proposes to rub is 60～70 ℃ of meltings, yet mink fat must be fresh and handle (Fr.Derrotde 2.213052 1974) in three hours after killing ermine.The method of propositions such as O.Fertek is will be under protection of inert gas; add scavenging agent, non-emulsifying agent, anti-albumen agent and the agent of restricting water supply mink fat is carried out the water-bath melting, can quicken melting and can reach the purpose (Czech 153 133 1971) that prevents ermine oil oxidation and deodorization.This method is that the extraction of ermine oil and treating process are merged, its operation is comparatively complicated, and various " auxiliary materials " that add are more, the refining ermine oil measure that obtains exists in the sealed vessel can only be preserved more than six months, obviously, it is not difficult to extract ermine oil from mink fat, and extract and refining obtain makeup and the required high-quality oil product of medical external ointment be do not allow very much readily accessible.Document (Ri Xingli chemistry Industry Co., Ltd compile " about mink oil ") thinks that also removing raw meat beastly in the ermine oil disturbs flavor and be difficult to arrive with common way.O.Fertek also mentions and can be blown into rare gas element to get rid of volatile stink in refining except the extraction and purified method that propose in above-mentioned document, can also further take away with mechanical way.In order to deviate from stink, the document that has proposes to make the modification of ermine oil, as the ermine oleyl alcohol is separated, transesterify and make modification such as inner transesterify, its ethanol ester can obtain not having the mobile oil of clarification (Ri Xingli chemistry Industry Co., Ltd's " about mink oil ") of unhappy smell through vacuum distilling; O.Fertel etc. mention in another patent and the mink grease is carried out nature separate ester under-5～0 ℃, make to release the fatty acid content that solves and reach 6%, and be that base-material is made makeup, medicine or washing composition better effects if (Czech 17,312 1978) with this mink oil.O.Fertek advocates that also adding stablizer at mink oil can strengthen its stability: add oxidation inhibitor such as tocopherol, lecithin, More sore resin, loban, alkylphenol, gallic acid ester etc. and can stop oxidation; Add easy oxydised component in intercalating agent (salt of polyprotonic acid or alcohol acid) the restriction oil; The ester, Sorbic Acid or the dehydro-acetic acid that add hydroxy-benzoic acid are to stop the breeding of microorganism.J.H.Fuss heats the grease that obtains with SI with thick mink oil and can preserve (Ger Offon 2.504961 1976) more than 2 years in addition.

The objective of the invention is on the basis of prior art, to work out one from mink fat extraction ermine oil, and can make with extra care and obtain the method for the refining ermine oil of high quality.

The present invention adopts the decompression water at low temperature to extract, and lipid acid is removed in neutralization, decompression or the distillation deodorizing of logical nitrogen reduced steam and dehydration method and make refined mink fat.At first the mink fat that rubs and water (1: 0.5～10) are placed in the extractor decompression heating to extract, vacuum tightness is 440～640mmHg, and 40～90 ℃ of temperature are advisable with 50～70 ℃, and extraction time is 2～10hr.Filter then, standing demix, oil reservoir is thick ermine oil.It is that 5～40% alkali lye carries out neutralization reaction that thick ermine oil drips concentration down at 30～80 ℃.Temperature of reaction commonly used is 50 ± 5 ℃, and the caustic solution of alkali lye commonly used 10%, its consumption are to calculate according to thick ermine oleic acid value to get, and promptly thick ermine weight of oil is taken advantage of 1.00～1.05 times of its acid number.The neutralization reaction standing demix that finishes, oil reservoir is neutral until washing water for several times with 50～70 ℃ of water washings.It is that oil is carried out the reduced steam distillation that oil after washing carries out the purified method, and vacuum tightness is 300～750mmHg.Also can before steam distillation, in the system that treats treated oil is housed, take to vacuumize-the inflated with nitrogen repeated treatments is for several times.And then carry out reduced steam and distill.Distillation time is 4～10 hours.Distill last thing and carry out standing demix, oil reservoir heats up, and high speed centrifugation (4000～6000 rev/mins) separates 80～90 ℃ the time, oil after the separation is again under 440～640mmHg vacuum, in 50～70 ℃ of dehydrations, pack in the airtight container of inflated with nitrogen and store more than 1 year down at-5 ℃ through the refining ermine oil that thoroughly dehydrates.This refining ermine oil can satisfy the requirement of superior cosmetics and medical cream fully.

The present invention considers that the raw meat in the mink oil is disturbed flavor and peculiar smell is wherein to have certain volatile low-molecular-weight compound to exist, adopt the method for decompression that they are evaporated from ermine oil, water extraction has just adopted this measure, particularly adopts this measure to make the not too big organic compound of those not volatile molecules also be brought out and remove by water vapor in steam distillation.Decompression can also reduce the oxidation of air to ermine oil, and logical nitrogen also can reach this purpose.The soap stock that produces in neutralization reaction (sodium soap) can adsorb various pigments, mucus and other impurity, plays the part decolorization.Water in the ermine oil is to produce the major reason become sour easily make microorganism existence down and accelerate breeding because water exists, thereby the present invention to take thoroughly dehydration be to guarantee the refining stable important measures of ermine oil quality.

Example 1.

Mink crude fat and water added in the vacuum tank by 1: 1 amount mixing reduce pressure, make progressively that vacuum tightness reaches 600mmHg in the jar, heats up 55～65 ℃, keep this condition to extract 4～8 hours, blowing filters then, and filtrate was left standstill 20～24 hours, and the branch oil-yielding stratum is weighed.Its result such as following table:

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Project

Crude fat add-on (kilogram) 350 300 300 260

Get oil mass (kilogram) 94.5 94.5 114.6 83.2

Oil yield (%) 27.0 31.5 38.3 32.0

Example 2.

Get 295 kilograms of water of thick ermine oil and pack in the enamel still, start stirring and heat up 50～60 ℃, slowly splash into totally 38 kilograms of 10% sodium hydroxide solutions with a great deal of.And then stir half an hour.The insulation layering, oil reservoir is neutrality with 50 ℃ of warm water agitator treatings twice, last washing water, and oil reservoir weighs 261 kilograms.Oil reservoir is inserted in the still kettle, open vacuum pump and make the vacuum tightness of system remain on 520～640mmHg, heat up then and carry out steam distillation, steamed in 6 hours 29 kilograms of water of condensation, the material standing demix gets oily 255 kilograms in the still, divides water with the oil 85 ℃ of supercentrifuges with 5720 rev/mins that heat up, then with oil in 600mmHg and≤60 ℃ of following vacuum hydro-extractions, must make with extra care 228.3 kilograms of ermine oil, true weight yield 77.4%.

Example 3.

Get 477 kilograms of thick ermine oil and suitable water gaging and carry out neutralization reaction in enamel still, its reactions steps and condition add 57 kilograms of 10% sodium hydroxide solutions with example 2.Oil reservoir is with 50～53 ℃ of warm water washed twice.Steam distillation carries out under 500～520mmHg, gets 13.3 kilograms of water of condensation.Oil reservoir must be made with extra care ermine oil 298.3, true weight yield 62.5% after high speed centrifugation separation and vacuum hydro-extraction.Its physicochemical property test result such as following table.

The test event data

Refractive index (20 ℃) 1.4700

Cloud point (℃) 17

Proportion (D) 0.9310

Iodine number (g/100g) 91.30

Acid number (KOH mg/g) 0.78

Saponification value (KOH mg/g) 195.20

Unsaponifiables (%) 1.76

Claims (5)

1, utilize mink fat to produce the method for refining ermine oil, the invention is characterized in that reparation technology comprises through water extraction, technology such as refining:

(1) water extraction, mink fat under reduced pressure extract down in 40～90 ℃ with water.

(2) neutralization and washing, the alkali lye that thick oil is mixed adding 5～40% down in wiping carries out neutralization reaction under 30～80 ℃, wash then.

(3) refining: washing back oil carries out oily water separation and oil dehydration then through the steam distillation deodorization.

2, as method as described in the claim 1., can under reduced pressure carry out when it is characterized in that with water extraction, its condition is: vacuum tightness is 440～640mmHg; Extracting temperature is advisable with 50～70 ℃.

3, as claim 1,2 described methods is characterized in that its concentration of the used alkali lye of neutralization reaction is 10% caustic solution, and the caustic alkali consumption is 1.00～1.05 times of thick ermine oleic acid thick ermine oil quality on duty.Neutral temperature is advisable with 50 ℃, and the water temperature during washing is advisable with 50～70 ℃.

4, as the described method of claim 1～3, the steam distillation in it is characterized in that making with extra care under reduced pressure carries out, and vacuum tightness is advisable with 300～750mmHg.Preferably before steam distillation system with vacuumize-the inflated with nitrogen repeated treatments for several times.

5, as the described method of claim 1～4, it is characterized in that carrying out oily water separation behind the steam distillation, to carry out high speed centrifugation after oil reservoir heats up and separate (4000～6000 rev/mins), separation temperature is advisable with 80～90 ℃.Oil reservoir after the separation carries out decompression dehydration again, and condition is: vacuum tightness is 440～640mmHg; Temperature is 50～70 ℃.