CN105524713A - Industrialized method for removing rubber in rubber tree seed oil - Google Patents
Industrialized method for removing rubber in rubber tree seed oil Download PDFInfo
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- CN105524713A CN105524713A CN201610075658.8A CN201610075658A CN105524713A CN 105524713 A CN105524713 A CN 105524713A CN 201610075658 A CN201610075658 A CN 201610075658A CN 105524713 A CN105524713 A CN 105524713A
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- 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
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
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- 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
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- 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
- C11B3/10—Refining fats or fatty oils by adsorption
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- 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
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Abstract
The invention relates to an industrialized method for removing rubber in rubber tree seed oil and belongs to the technical field of plant oil processing. According to the method, firstly, activated carbon with the weight being 0.5-2.0 times of that of natural rubber is added according to the content of natural rubber in the rubber tree seed oil, and the mixture is heated to 90-120 DEG C and stirred for 14-16 minutes; activated clay with the mass being 3%-6% of that of the rubber tree seed oil is added, and the mixture is kept at the temperature of 90-120 DEG C and stirred for 14-16 min; then, a material is filtered, the activated carbon and the activated clay are filtered out, and the oil temperature during filtration is kept higher than 90 DEG C; finally, the absolute pressure in a sealed container is smaller than 500 Pa, the rubber tree seed oil is heated to 200-260 DEG C, thermal decomposition of natural rubber and distillation and volatilization of a decomposed product are performed, and rubber removal can be realized. By means of the method, the rubber removal effect is good, the rubber is thoroughly removed, no novel solvent is introduced, the production efficiency is high, and large-scale production can be realized.
Description
Technical field
The invention belongs to vegetables oil processing technique field, be specifically related to a kind of method of industrialized seeds of rubber tree oil removing rubber.
Background technology
Seeds of rubber tree oil is the vegetables oil extracted inside seeds of rubber tree, and seeds of rubber tree oil belongs to precious tropical woody oleiferous plants.Seeds of rubber tree fatty acid oil is based on Palmiticacid, stearic acid, oleic acid, linoleic acid plus linolenic acid, and degree of unsaturation (unsaturated fatty acids total), up to 83%, especially contains the linolenic acid of 20%.The research of domestic and international many research institutions shows, seeds of rubber tree oil is not only of high nutritive value, and has preventing cardiovascular disease, and promotes the health-care effect of Fadeaway of Atherosclerosis, is a kind of oil plant having practical value and health-care effect concurrently.
Natural rubber compositions (polyisoprene) containing trace in rubber seed kind benevolence, when extraction grease, also partly can dissolve in seeds of rubber tree oil and go.Research shows, the natural rubber inside seeds of rubber tree oil accounts for 0.1-0.4%, has any different because the kind of rubber tree is different with the method for liquefaction.Natural rubber is not the conventional ingredient in food oils, must remove.
The method that the seeds of rubber tree oil that current documents and materials, patent etc. have been announced removes rubber roughly can be divided into specific method and nonspecific method.Specific method can remove natural rubber targetedly, and removal effect is good, remove thoroughly.Specificity removes the method for the rubber in seeds of rubber tree oil, mainly solvent precipitation and membrane filter method.
Solvent precipitation is described by the patent No. ZL200910094034.0 method and apparatus of removing rubber " seeds of rubber tree oil ", take acetone as primary solvent, miscible in seeds of rubber tree oil, treat polyisoprene Precipitation, then distillation removes acetone solvent, obtains the seeds of rubber tree oil of removing rubber.But this method has two main drawbacks: the first, introduces organic solvent, has dissolvent residual; The second, deviate from trace ingredients that is nutritious in seeds of rubber tree oil and health-care effect when removing polyisoprene, such as phosphatide, sterol, vitamin-E etc. simultaneously.
Membrane filter method described by the patent " a kind of method (application number CN201410846892.7) of rubber seed oil high performance membrane filtering and removing rubber ", according to the difference of the molecular weight of natural rubber and triglyceride level, adopts ceramic membrane filtering natural rubber.The advantage of membrane filtration is a lot, the good product quality processed, but equipment is disposable to have high input, and filtration efficiency is on the low side, is not suitable for large scale continuous prod.
Nonspecific method is fat degumming while, nonspecificly removes natural rubber.Nonspecific method removes the poor effect of natural rubber, let alone thoroughly removes.Its reason is as follows:
1. " glue " of oils industry is also called " colloid ", and refer to and be dispersed in colloidalmaterial unstable in grease, long storage time can be deposited in container bottom, becomes oil foot.Colloid main chemical compositions is phosphatide, and it is a kind of amphiphatic material, both hydrophilic, oleophylic again.The principle of coming unstuck to be exactly grease add water under neutral (hydration degum) or acid (phosphoric acid or formic acid come unstuck) condition stirring, allows the water-swelling of phosphatide hydrophilic radical, becomes hydrated phospholipid micelle.After phosphatide aquation, become more hydrophilic, more oleophobic, in grease, again cannot keep the state of stable dispersion, so with regard to flocculation sediment out.
2., although natural rubber is also a kind of band sticking " colloid ", it is hydrocarbon polymer (polyisoprene) completely, is the molecule of strict oleophylic, containing any hydrophilic radical (oxygen-free and other atom).So no matter be hydration degum, or acidifying is come unstuck, natural rubber molecule all cannot be allowed to absorb water and to be precipitated out.
Why hydration degum or acidifying is called non-specific removing rubber if being come unstuck, be because phosphatide, in water-swelling, when flocculation sediment, also can carry some high molecular natural rubbers secretly out.But this carrying secretly is nonspecific, nonselective, is also halfway.According to documents and materials, following academic paper has related to the non-specific technology removing rubber of seeds of rubber tree oil:
1. " Study on Refining of rubber seed oil " (author king Xiao Li, Zhan Lin Chinese oil magazine, 2000,25 (4): 10-11) propose, and remove the tiny amount rubber in rubber seed oil with formic acid.
2. " producing and Study of Refining of rubber seed oil " (author Hu little Hong, Liu great Chuan, Zhang Xincai, Chinese oil magazine, 2005,30 (11): 65-67) think, rubber can be removed with phosphoric acid, and think that its principle is: " adding phosphoric acid can also make the rubber hydrocarbon double bond of high dispersing phase be oxidized, and becomes peroxidation rubber.Produce under heat effect and shrink, become aggregate, separate from oil." phosphoric acid thought about this paper makes the two hydrocarbon of rubber be oxidized to peroxidation rubber, those skilled in the art are these conclusions of disapprove.Because the phosphoric acid of generally acknowledging is not a kind of strong oxidizer, phosphoric acid can not be oxidized carbon-carbon double bond.
3. " rubber seed oil-producing technique with put into practice " (author Jia Wei, Chinese oil magazine, 2006,31 (2): 12-14) propose to adopt formic acid removing rubber, the method of removing rubber is: " formic acid removing rubber, the edible vegetable oil sloughing phosphatide is heated to 60 ~ 70 DEG C, and heavy 0.1% formic acid (food grade) of refueling reacts 20 ~ 25min; only put precipitation, add water washing 2 ~ 3 times.”
4. " rubber seed oil come unstuck decolouring technical study " (author Tian Hua, Huang Tao, Su Minghua, Wuhan University of Technology's journal, 2007,26 (2): 9-11) have employed 4 kinds of methods to come unstuck (author thinks that the implication of glue comprises rubber and colloid), these 4 kinds of methods respectively: 1. hydration degum; 2. phosphoric acid degumming; 3. freezing phosphoric acid degumming; 4. phosphoric acid+formic acid two-step approach is come unstuck.Author thinks method, and 4. effectiveness comparison is good, and to analyze that reason comes unstuck because of second step formic acid be special in rubber.
5. " Researching and practicing of rubber seed oil refining " (author Luo Xiaolan, red legend is prosperous, He Jian, Li Linkai, grain and oil processing magazine, 2009 (11): 46-49), author does not specifically distinguish removing rubber and comes unstuck matter (phosphatide), is also attempted 4 kinds of methods: 1. add phosphoric acid and calcium carbonate aquation; 2. formic acid aquation is added after first adding phosphoric acid; 3. phosphoric acid water is added separately; 4. the direct aquation of not doping.Finally have employed the Degumming method adding separately phosphoric acid water.Its working method and processing parameter as follows: add the food grade phosphoric acid that concentration is 85% when oil temperature being adjusted to 40 DEG C, add-on is that oil is heavy by 3 ‰, after being fully uniformly mixed, temperature is heightened to 80 DEG C, add the soft water of equality of temperature under fast stirring, amount of water is that oil is heavy by 8%, changes low rate mixing and heat up after adding water, about final temperature to 85 DEG C, continue to stir 30min after reaching final temperature, stop stirring, more than standing sedimentation 6h, release oil foot, sewage and sump oil, the oil after aquation carries out vacuum hydro-extraction.
6. " rubber seed oil short distance/molecular distillation technical study " (author Li Linkai, Li Chen, Tao Yin, grain and oil are processed: electronic edition magazine, 2015 (9): 26-28) in, the idea of author is the same with " Researching and practicing of rubber seed oil refining ", and attempted 4 kinds of methods, last optimization adds separately the method that phosphoric acid water comes unstuck.
In sum, the oily method removing rubber of seeds of rubber tree can be divided into specific removal methods and nonspecific removal methods.Specific removal methods, removing rubber is effective, removes thoroughly, but exists and introduce chemical solvents or the low shortcoming of production efficiency.Nonspecific removing rubber method can merge with the Degumming method in oil and fat refining, does not increase extra step, is applicable to large-scale production, but there is removing rubber weak effect, remove not completely problem.Therefore how overcoming the deficiencies in the prior art is problems that current vegetables oil processing technique field needs solution badly.
Summary of the invention
The present invention is exactly that find a kind of removing rubber effective, remove thoroughly, do not introduce novel solvent, production efficiency is high, the method that can accomplish scale production for existing seeds of rubber tree oil removing rubber method Problems existing.
For achieving the above object, the technical solution used in the present invention is as follows:
A method for industrialized seeds of rubber tree oil removing rubber, comprises the steps:
Step (1), gac specific adsorption: according to the content of natural rubber in seeds of rubber tree oil, adding is natural rubber weight 0.5-2.0 gac doubly, is warmed up to 90-120 DEG C, stirs 14-16 minute;
Step (2), atlapulgite non-specific adsorption: in the material after step (1) stirring, add the atlapulgite that quality is the 3-6% of seeds of rubber tree oil quality, keep temperature 90-120 DEG C, stir 14-16 minute;
Step (3), non-specific filtering: by the material filtering after step (2) stirs, with filtering gac and atlapulgite, oil temperature during filtration remains on more than 90 DEG C;
Step (4), remaining natural rubber thermolysis: in sealed vessel, the absolute pressure in container is less than 500Pa, and seeds of rubber tree oil is heated to 200-260 DEG C, maintains more than 5min, carries out the volatile matter distillation of the thermolysis Sum decomposition product of natural rubber.
Wherein, degradation production is mainly the isoprene tetramer and the tripolymer of 20 carbon and 15 carbon.
In the present invention, simultaneously the volatile matter distillation of thermolysis Sum decomposition product is carrying out.
Further, the quality that preferably the middle gac of step (1) adds is 0.8-1.2 times of natural rubber quality in seeds of rubber tree oil.
Further, in order to reduce the oxidation of grease, preferably step (1) and middle stirring of step (2) are carried out in the sealed can that absolute pressure is less than 20kPa.
Further, the quality that preferably the middle atlapulgite of step (2) adds is the 4-5% of seeds of rubber tree oil quality.
Further, the filtration preferably described in step (3) adopts leaf filter or flame filter press.
Further, the sealed vessel preferably described in step (4) is sealed can or lock packing tower.
Further, the Heating temperature preferably described in step (4) is 220-240 DEG C.
Further, absolute pressure during heating preferably described in step (4) in container is less than 250Pa.
Further, more easily volatilize to allow natural rubber degradation production (the isoprene tetramer and tripolymer), preferably in step (4), pass into water vapor during the heating of seeds of rubber tree oil, the throughput of water vapor does not have specific requirement, as long as the air-flow produced can be easy to carry, thermal decomposition product goes out container.
Science and technology principle of the present invention
The present invention employs the principle that three kinds remove natural rubber simultaneously:
1. one of principle: gac is to the specific adsorption of natural rubber
The chemical composition of natural rubber is polyisoprene, is pure hydrocarbon polymer, has strict hydrophobicity.Gac is a kind of carbon simple substance, and its structure is the small graphite crystal of porosity and looseness.The sheet structure that graphite crystal is made up of cellular hydrogenation of six carbocyclic, is carbon-carbon double bond and combines (carbon-carbon double bond comprises a σ singly-bound and conjugatedπbond) between each carbon atom.Gac has very large surface-area, has very strong adsorptive power.But gac has certain selectivity to adsorbent, its selectivity is greater than adsorptivity to hydrophilic substance to the adsorptivity of hydrophobic substance; Not carbon-carbon double bonds is greater than to the adsorptive power containing the many material of carbon-carbon double bond (comprising a σ singly-bound and a π key), or the poor material of carbon-carbon double bond.
Natural rubber is strictly hydrophobic material, not containing Sauerstoffatom and other hydrophilic radical, and its each monomer (5 carbon repeating unit) is all containing a carbon-carbon double bond (comprising a σ singly-bound and a π key), and therefore gac is very strong for the adsorptive power of natural rubber.Seeds of rubber tree main body of oil is triglyceride level, and all containing 3 ester bonds in each triglyceride level molecule, ester bond belongs to hydrophilic radical.So gac is weaker than the adsorptive power to natural rubber for the adsorptive power of triglyceride level, can optionally natural rubber be adsorbed from triglyceride level, this belongs to specific adsorption.
2. principle two, atlapulgite is to the non-specific filtering of natural rubber.
Atlapulgite belongs to the silicate after activation, and composition comprises calsil, britesorb, aluminium silicate salt, silicic acid molysite etc.Atlapulgite also has very strong adsorptive power, but atlapulgite self is hydroaropic substance, is eager to excel, does not possess the ability of specific adsorption natural rubber to the absorption of hydroaropic substance in grease.
Atlapulgite removes by filtering formation filter cake removing of natural rubber.Natural rubber belongs to natural macromolecular material.The molecular weight of natural rubber is 3-300 ten thousand dalton, and the diameter of molecule is within the scope of 5-50nm, and molecular mass about 900 dalton of grease (triglyceride level), molecular diameter is less than 1nm.Atlapulgite filters after adding grease, forms filter cake.Filter cake is exactly the mesh-like structure be made up of atlapulgite fine particle, molecule less (molecular weight is low, and diameter is little), easilier passes from filter cake network of micropores; Molecule larger (molecular weight is high, and diameter is large), is is more easily intercepted and captured by filter cake network of micropores.The principle of Here it is the non-specific filtering natural rubber of atlapulgite.
Add atlapulgite, except non-specific filtering natural rubber, also have the effect of auxiliary activity charcoal filtering separation from seeds of rubber tree oil.Because gac can specific adsorption natural rubber, after therefore adding seeds of rubber tree oil, a large amount of natural rubber molecules can be adsorbed in the surface of micro activated carbon particle, forms adhesion layer, becomes very thickness.If adopt traditional filter type (comprising plate and frame to filter and vane type filtration), be easy to harden, blocking filter opening, makes filtration difficulty.If but after adding atlapulgite, because the quantity of atlapulgite is far more than the quantity of gac, the atlapulgite of non-thickness can wrap up the gac of thickness, forms filter cake, plays filtrating aid function.
3. principle three, the thermolysis of natural rubber and vacuum removal.
The thermostability of natural rubber (polyisoprene) is poorer than grease (triglyceride level), and after being heated to decomposition temperature, natural rubber (polyisoprene) polymer carbochain can produce phenomenon of rupture, and molecular weight diminishes.If temperature raises further, then the fracture of polyisoprene carbochain is more violent, becomes the oligomer of polyisoprene from high molecular polymer, and even forms isoprene monomer.Although high temperature contributes to the decomposition of natural rubber, equally also can affect the quality of grease, therefore temperature can not be too high.According to chemical equilibrium theory, if remove reaction product from reaction system, then the forward being conducive to chemical reaction carries out.Due to isoprene oligomer (tetramer or tripolymer) in high vacuum conditions, can evaporate from seeds of rubber tree oil, so can under high vacuum environment and relatively low temperature (grease keeps stable at such a temperature), realize the decomposition of natural rubber, and remove degradation production.In reaction system, pass into xeothermic water vapor, water vapor can be assisted and be carried isoprene oligomer (tetramer or tripolymer) reaction product, improves the volatilization efficiency of isoprene oligomer.The thermolysis of natural rubber that Here it is and the principle of vacuum removal.
Experimentally survey (measuring method is the company standard mensuration of natural rubber content " in the Q/XSBNHK0010-2015 seeds of rubber tree oil "), in the present invention, gac can the natural rubber of specific adsorption more than 80%, and atlapulgite can the natural rubber of filtering residue about 20%.The residual natural rubber less than 1%, through thermolysis and vacuum removal, thoroughly can remove the natural rubber in seeds of rubber tree oil.
Compared with prior art, its beneficial effect is in the present invention:
Removing rubber of the present invention is effective, and remove thoroughly, do not introduce novel solvent, production efficiency is high, can realize the method for mass-producing.Relative to the method for other removing rubber, present method is more suitable for large scale continuous prod, proves through production practice, and the decreasing ratio of its rubber is significantly higher than other method; Present invention process flow process is simple, does not need to use organic chemical reagent to do removing rubber agent, and security is high; Scouring processes of the present invention can keep holding the nutritive ingredient in seeds of rubber tree oil to a great extent.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.
It will be understood to those of skill in the art that the following example only for illustration of the present invention, and should not be considered as limiting scope of the present invention.Unreceipted concrete technology or condition person in embodiment, according to the technology described by the document in this area or condition or carry out according to product description.Agents useful for same or the unreceipted production firm person of instrument, being can by buying the conventional products obtained.
Embodiment 1
1) low temperature pressing seeds of rubber tree oil crude oil, the content of surveying wherein natural rubber is 0.25%.Add the gac (i.e. oil heavy 0.25%) of natural rubber weight 1 times, be warmed up to 120 DEG C, stir 15 minutes.This operates in sealed can and carries out under condition of negative pressure, and the absolute pressure of tank inside is less than 15kPa.
2) add the atlapulgite that oil weighs 3.5%, keep temperature 120 DEG C, stir 15 minutes.This operates in sealed can and carries out under condition of negative pressure, and the absolute pressure of tank inside is less than 15kPa.
3) adopt plate and frame filter, filtering gac and atlapulgite, during filtration, oil temperature remains on more than 90 DEG C.
4) in sealed vessel, seeds of rubber tree oil is heated to 200 DEG C, keep 5min, the absolute pressure in container is less than 250Pa, carries out the thermolysis of natural rubber, in seeds of rubber tree oil, pass into water vapor, to promote the volatilization of rubber degradation production.Remove the oil of the seeds of rubber tree after rubber viscosity little, not wire drawing, is heated to 280 DEG C of oil colours not blackening, separates out without carbon fiber.Survey natural rubber content in the crude oil after coming unstuck not detect.
Embodiment 2
1) low temperature pressing seeds of rubber tree oil crude oil, surveying wherein natural rubber content is 0.25%.Add the gac (i.e. oil heavy 0.3%) of natural rubber weight 1.2 times, be warmed up to 110 DEG C, stir 14 minutes.This operates in sealed can and carries out under condition of negative pressure, and the absolute pressure of tank inside is less than 20kPa.
2) add the atlapulgite that oil weighs 3%, keep temperature 90 DEG C, stir 14 minutes.This operates in sealed can and carries out under condition of negative pressure, and the absolute pressure of tank inside is less than 20kPa.
3) adopt plate and frame filter, filtering gac and atlapulgite, during filtration, oil temperature remains on more than 90 DEG C.
4) in sealed vessel, seeds of rubber tree oil is heated to 200 DEG C, keep 10min, the absolute pressure in container is less than 250Pa, carries out the thermolysis of natural rubber, in seeds of rubber tree oil, pass into water vapor, to promote the volatilization of rubber degradation production.Remove the oil of the seeds of rubber tree after rubber viscosity little, not wire drawing, is heated to 280 DEG C of oil colours not blackening, separates out without carbon fiber.Survey natural rubber content in the crude oil after coming unstuck not detect.
Embodiment 3
1) seeds of rubber tree oil crude oil is squeezed in hot pressing, and surveying wherein natural rubber content is 0.15%.Add the gac (i.e. oil heavy 0.3%) of natural rubber weight 2 times, be warmed up to 120 DEG C, stir 16 minutes.This operates in sealed can and carries out under condition of negative pressure, and the absolute pressure of tank inside is less than 15kPa.
2) add the atlapulgite that oil weighs 5%, keep temperature 120 DEG C, stir 16 minutes.This operates in sealed can and carries out under condition of negative pressure, and the absolute pressure of tank inside is less than 15kPa.
3) adopt plate and frame filter, filtering gac and atlapulgite, during filtration, oil temperature remains on more than 90 DEG C.
4) in sealed vessel, seeds of rubber tree oil is heated to 230 DEG C, keep 12min, the absolute pressure in container is less than 250Pa, carries out the thermolysis of natural rubber, in seeds of rubber tree oil, pass into water vapor, to promote the volatilization of rubber degradation production.Remove the oil of the seeds of rubber tree after rubber viscosity little, not wire drawing, is heated to 280 DEG C of oil colours not blackening, separates out without carbon fiber.Survey natural rubber content in the crude oil after coming unstuck not detect.
Embodiment 4
1) seeds of rubber tree oil crude oil is squeezed in hot pressing, and surveying wherein natural rubber content is 0.15%.Add the gac (i.e. oil heavy 0.2%) of natural rubber weight 0.8 times, be warmed up to 100 DEG C, stir 15 minutes.This operates in sealed can and carries out under condition of negative pressure, and the absolute pressure of tank inside is less than 20kPa.
2) add the atlapulgite that oil weighs 4.5%, keep temperature 100 DEG C, stir 15 minutes.This operates in sealed can and carries out under condition of negative pressure, and the absolute pressure of tank inside is less than 20kPa.
3) adopt plate and frame filter, filtering gac and atlapulgite, during filtration, oil temperature remains on more than 90 DEG C.
4) in sealed vessel, seeds of rubber tree oil is heated to 230 DEG C, keep 8min, the absolute pressure in container is less than 250Pa, carries out the thermolysis of natural rubber, in seeds of rubber tree oil, pass into water vapor, to promote the volatilization of rubber degradation production.Remove the oil of the seeds of rubber tree after rubber viscosity little, not wire drawing, is heated to 280 DEG C of oil colours not blackening, separates out without carbon fiber.Survey natural rubber content in the crude oil after coming unstuck not detect.
Embodiment 5
1) leach seeds of rubber tree oil crude oil, surveying wherein natural rubber content is 0.4%.Add the gac (i.e. oil heavy 0.2%) of natural rubber weight 0.5 times, be warmed up to 120 DEG C, stir 15 minutes.This operates in sealed can and carries out under condition of negative pressure, and the absolute pressure of tank inside is less than 15kPa.
2) add the atlapulgite that oil weighs 4%, keep temperature 120 DEG C, stir 15 minutes.This operates in sealed can and carries out under condition of negative pressure, and the absolute pressure of tank inside is less than 15kPa.
3) adopt plate and frame filter, filtering gac and atlapulgite, during filtration, oil temperature remains on more than 90 DEG C.
4) in sealed vessel, seeds of rubber tree oil is heated to 260 DEG C, keep 10min, the absolute pressure in container is less than 250Pa, carries out the thermolysis of natural rubber, in seeds of rubber tree oil, pass into water vapor, to promote the volatilization of rubber degradation production.Remove the oil of the seeds of rubber tree after rubber viscosity little, not wire drawing, is heated to 280 DEG C of oil colours not blackening, separates out without carbon fiber.Survey natural rubber content in the crude oil after coming unstuck not detect.
Embodiment 6
1) leach seeds of rubber tree oil crude oil, surveying wherein natural rubber content is 0.4%.Add the gac (i.e. oil heavy 0.6%) of natural rubber weight 1.5 times, be warmed up to 90 DEG C, stir 15 minutes.This operates in sealed can and carries out under condition of negative pressure, and the absolute pressure of tank inside is less than 20kPa.
2) add the atlapulgite that oil weighs 4%, keep temperature 100 DEG C, stir 15 minutes.This operates in sealed can and carries out under condition of negative pressure, and the absolute pressure of tank inside is less than 20kPa.
3) adopt plate and frame filter, filtering gac and atlapulgite, during filtration, oil temperature remains on more than 90 DEG C.
4) in sealed vessel, seeds of rubber tree oil is heated to 260 DEG C, keep 10min, the absolute pressure in container is less than 250Pa, carries out the thermolysis of natural rubber, in seeds of rubber tree oil, pass into open steam, to promote the volatilization of rubber degradation production.Remove the oil of the seeds of rubber tree after rubber viscosity little, not wire drawing, is heated to 280 DEG C of oil colours not blackening, separates out without carbon fiber.Survey natural rubber content in the crude oil after coming unstuck not detect.
Performance Detection
The present invention, compared with other removing rubber method, has the advantage that degumming rate is high, reduce production cost.Seeds of rubber tree degumming of oil (result is as table 1) is carried out through following three kinds of methods, in actual production that formic acid comes unstuck and acetone comes unstuck, degumming rate only has 50% ~ 60%, degumming rate of the present invention can reach 99.99%, and utilizing the company standard mensuration of natural rubber content " in the Q/XSBNHK0010-2015 seeds of rubber tree oil " to detect the seeds of rubber tree oil after coming unstuck, result does not detect (< 0.01%).
Table 1
Relative to the method for other removing rubber, present method is more suitable for large scale continuous prod, proves through production practice, and the decreasing ratio of its rubber is significantly higher than other method; Present invention process flow process is simple, does not need to use organic chemical reagent to do removing rubber agent, and security is high; Scouring processes of the present invention can keep holding the nutritive ingredient in seeds of rubber tree oil to a great extent.
More than show and describe ultimate principle of the present invention, principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (9)
1. a method for industrialized seeds of rubber tree oil removing rubber, is characterized in that, comprise the steps:
Step (1), gac specific adsorption: according to the content of natural rubber in seeds of rubber tree oil, adding is natural rubber weight 0.5-2.0 gac doubly, is warmed up to 90-120 DEG C, stirs 14-16 minute;
Step (2), atlapulgite non-specific adsorption: in the material after step (1) stirring, add the atlapulgite that quality is the 3-6% of seeds of rubber tree oil quality, keep temperature 90-120 DEG C, stir 14-16 minute;
Step (3), non-specific filtering: by the material filtering after step (2) stirs, with filtering gac and atlapulgite, oil temperature during filtration remains on more than 90 DEG C;
Step (4), remaining natural rubber thermolysis: in sealed vessel, the absolute pressure in container is less than 500Pa, and seeds of rubber tree oil is heated to 200-260 DEG C, maintains more than 5min, carries out the volatile matter distillation of the thermolysis Sum decomposition product of natural rubber.
2. the method for industrialized seeds of rubber tree oil removing rubber according to claim 1, it is characterized in that, the quality that in step (1), gac adds is 0.8-1.2 times of natural rubber quality in seeds of rubber tree oil.
3. the method for industrialized seeds of rubber tree oil removing rubber according to claim 1, is characterized in that, step (1) and middle stirring of step (2) are carried out in the sealed can that absolute pressure is less than 20kPa.
4. the method for industrialized seeds of rubber tree oil removing rubber according to claim 1, it is characterized in that, the quality that in step (2), atlapulgite adds is the 4-5% of seeds of rubber tree oil quality.
5. the method for industrialized seeds of rubber tree oil removing rubber according to claim 1, it is characterized in that, the filtration described in step (3) adopts leaf filter or flame filter press.
6. the method for industrialized seeds of rubber tree oil removing rubber according to claim 1, it is characterized in that, the sealed vessel described in step (4) is sealed can or lock packing tower.
7. the method for industrialized seeds of rubber tree oil removing rubber according to claim 1, it is characterized in that, the Heating temperature described in step (4) is 220-240 DEG C.
8. the method for industrialized seeds of rubber tree oil removing rubber according to claim 1, is characterized in that, absolute pressure during heating described in step (4) in container is less than 250Pa.
9. the method for industrialized seeds of rubber tree oil removing rubber according to claim 1, it is characterized in that, in step (4), pass into water vapor during the heating of seeds of rubber tree oil, the air-flow produced is used for carrying thermal decomposition product.
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| CN110433195A (en) * | 2018-05-05 | 2019-11-12 | 西双版纳华坤生物科技有限责任公司 | A kind of application of substance on relieving alcoholism and protecting liver |
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