CN116135980A - Comprehensive biological refining method using elaeagnus angustifolia fruits as raw materials and preparation method thereof - Google Patents
Comprehensive biological refining method using elaeagnus angustifolia fruits as raw materials and preparation method thereof Download PDFInfo
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- CN116135980A CN116135980A CN202111352790.6A CN202111352790A CN116135980A CN 116135980 A CN116135980 A CN 116135980A CN 202111352790 A CN202111352790 A CN 202111352790A CN 116135980 A CN116135980 A CN 116135980A
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- oil
- kernel
- elaeagnus angustifolia
- fruits
- powder
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- 244000307545 Elaeagnus angustifolia Species 0.000 title claims abstract description 84
- 235000017643 Elaeagnus angustifolia Nutrition 0.000 title claims abstract description 83
- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000002994 raw material Substances 0.000 title claims abstract description 23
- 238000007670 refining Methods 0.000 title claims abstract description 13
- 235000013399 edible fruits Nutrition 0.000 title claims description 55
- 238000002360 preparation method Methods 0.000 title description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 117
- 239000000843 powder Substances 0.000 claims abstract description 50
- 235000019198 oils Nutrition 0.000 claims abstract description 38
- 238000000855 fermentation Methods 0.000 claims abstract description 29
- 230000004151 fermentation Effects 0.000 claims abstract description 29
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 27
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000004593 Epoxy Substances 0.000 claims abstract description 22
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 22
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 21
- 102000004169 proteins and genes Human genes 0.000 claims abstract description 19
- 108090000623 proteins and genes Proteins 0.000 claims abstract description 19
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- 239000004382 Amylase Substances 0.000 claims abstract description 15
- 102000013142 Amylases Human genes 0.000 claims abstract description 15
- 108010065511 Amylases Proteins 0.000 claims abstract description 15
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- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims abstract description 12
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- 108010059892 Cellulase Proteins 0.000 claims abstract description 7
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims abstract description 7
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- 235000001456 Elaeagnus latifolia Nutrition 0.000 claims description 28
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- 238000001035 drying Methods 0.000 claims description 16
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- 235000014680 Saccharomyces cerevisiae Nutrition 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 12
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- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 7
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- 238000003763 carbonization Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 4
- 235000019476 oil-water mixture Nutrition 0.000 claims description 4
- 239000008247 solid mixture Substances 0.000 claims description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 4
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 3
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- 239000011592 zinc chloride Substances 0.000 claims description 2
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- 230000036983 biotransformation Effects 0.000 claims 1
- 239000003921 oil Substances 0.000 abstract description 30
- 238000006243 chemical reaction Methods 0.000 abstract description 22
- 235000000346 sugar Nutrition 0.000 abstract description 15
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- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 8
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- RFSUNEUAIZKAJO-ARQDHWQXSA-N Fructose Chemical compound OC[C@H]1O[C@](O)(CO)[C@@H](O)[C@@H]1O RFSUNEUAIZKAJO-ARQDHWQXSA-N 0.000 description 7
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- 235000014113 dietary fatty acids Nutrition 0.000 description 4
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- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 3
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- SCKXCAADGDQQCS-UHFFFAOYSA-N Performic acid Chemical compound OOC=O SCKXCAADGDQQCS-UHFFFAOYSA-N 0.000 description 2
- 230000003213 activating effect Effects 0.000 description 2
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- 239000008367 deionised water Substances 0.000 description 2
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- OYHQOLUKZRVURQ-NTGFUMLPSA-N (9Z,12Z)-9,10,12,13-tetratritiooctadeca-9,12-dienoic acid Chemical compound C(CCCCCCC\C(=C(/C\C(=C(/CCCCC)\[3H])\[3H])\[3H])\[3H])(=O)O OYHQOLUKZRVURQ-NTGFUMLPSA-N 0.000 description 1
- 240000003183 Manihot esculenta Species 0.000 description 1
- 235000016735 Manihot esculenta subsp esculenta Nutrition 0.000 description 1
- 241001052560 Thallis Species 0.000 description 1
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- 239000003463 adsorbent Substances 0.000 description 1
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- 235000019730 animal feed additive Nutrition 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P7/00—Preparation of oxygen-containing organic compounds
- C12P7/02—Preparation of oxygen-containing organic compounds containing a hydroxy group
- C12P7/04—Preparation of oxygen-containing organic compounds containing a hydroxy group acyclic
- C12P7/06—Ethanol, i.e. non-beverage
- C12P7/08—Ethanol, i.e. non-beverage produced as by-product or from waste or cellulosic material substrate
- C12P7/10—Ethanol, i.e. non-beverage produced as by-product or from waste or cellulosic material substrate substrate containing cellulosic material
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K10/00—Animal feeding-stuffs
- A23K10/10—Animal feeding-stuffs obtained by microbiological or biochemical processes
- A23K10/12—Animal feeding-stuffs obtained by microbiological or biochemical processes by fermentation of natural products, e.g. of vegetable material, animal waste material or biomass
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K10/00—Animal feeding-stuffs
- A23K10/10—Animal feeding-stuffs obtained by microbiological or biochemical processes
- A23K10/14—Pretreatment of feeding-stuffs with enzymes
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K10/00—Animal feeding-stuffs
- A23K10/30—Animal feeding-stuffs from material of plant origin, e.g. roots, seeds or hay; from material of fungal origin, e.g. mushrooms
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
- C01B32/318—Preparation characterised by the starting materials
- C01B32/324—Preparation characterised by the starting materials from waste materials, e.g. tyres or spent sulfite pulp liquor
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D301/00—Preparation of oxiranes
- C07D301/02—Synthesis of the oxirane ring
- C07D301/03—Synthesis of the oxirane ring by oxidation of unsaturated compounds, or of mixtures of unsaturated and saturated compounds
- C07D301/12—Synthesis of the oxirane ring by oxidation of unsaturated compounds, or of mixtures of unsaturated and saturated compounds with hydrogen peroxide or inorganic peroxides or peracids
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D303/00—Compounds containing three-membered rings having one oxygen atom as the only ring hetero atom
- C07D303/02—Compounds containing oxirane rings
- C07D303/38—Compounds containing oxirane rings with hydrocarbon radicals, substituted by carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals
- C07D303/40—Compounds containing oxirane rings with hydrocarbon radicals, substituted by carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals by ester radicals
- C07D303/42—Acyclic compounds having a chain of seven or more carbon atoms, e.g. epoxidised fats
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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
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/06—Production of fats or fatty oils from raw materials by pressing
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- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/02—Monosaccharides
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- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/14—Preparation of compounds containing saccharide radicals produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase, e.g. by cellulase, hemicellulase
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- C12P2201/00—Pretreatment of cellulosic or lignocellulosic material for subsequent enzymatic treatment or hydrolysis
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
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Abstract
The invention discloses a comprehensive biological refining method taking fructus elaeagnus angustifoliae as a raw material, which comprises the following steps: separating pulp and kernel of fructus Elaeagni Angustifoliae to obtain fructus Elaeagni Angustifoliae pulp powder and kernel; bioconversion is carried out on the elaeagnus angustifolia pulp powder to obtain ethanol and protein feed; squeezing fructus Elaeagni Angustifoliae kernel, and extracting to obtain kernel oil and kernel residue; epoxidation is carried out on the nut oil to obtain an epoxy plasticizer; carbonizing the kernel residues to obtain the active carbon. According to the invention, components such as fermentable sugar, starch, cellulose, lignin and the like in the elaeagnus angustifolia are fully utilized, the starch and the cellulose can be converted into monosaccharide by using amylase and cellulase with specific proportions, the ethanol yield is improved, the protein feed is obtained by using ammonium sulfate for growth in the thallus fermentation process, and the preferable dosage of formic acid, sulfuric acid and hydrogen peroxide can optimize the reaction rate and the reaction selectivity of epoxidation so as to obtain the epoxy plasticizer with higher epoxy value.
Description
Technical Field
The invention relates to the technical field of biochemical engineering, in particular to a comprehensive biological refining method taking non-grain crop oleaster fruits as raw materials, which is used for producing ethanol, protein feed, epoxy plasticizer and active carbon by conversion, wherein the obtained ethanol can be used as a green renewable energy source, the protein feed is used as an animal feed additive, the epoxy plasticizer is used as an environment-friendly green plasticizer, and the active carbon can be used as an adsorbent.
Background
Along with the increasing of the dependence on energy sources at home and abroad and the increasing contradiction of exhaustion of fossil energy sources, the problems of environment generated in the processes of fossil energy source utilization and combustion, such as soil pollution, water pollution, air pollution and the like are increasingly highlighted, so that the development of the biological alternative energy source represented by fuel ethanol is widely promoted at home and abroad. The current production raw materials of biofuel ethanol mainly comprise grain crops, lignocellulose biomass and non-grain crops. The problem of 'competing with people for grain and competing with land' exists in the transformation of fuel ethanol of grain crops such as wheat, corn and the like, which is contrary to national conditions; the energy consumption of the process of converting the lignocellulose biomass into the ethanol is higher, the economic benefit is difficult to be improved, and the bottleneck limit is more because the lignocellulose biomass such as straw, agriculture and forestry waste and the like is complex and changeable in structure; the non-grain crops such as cassava and the like are used for converting fuel ethanol, so that the problems of 'competing for grain with people and competing for land with grain' are solved, and the problems of low fuel ethanol conversion efficiency and multiple bottleneck factors are solved, so that the non-grain crops are selected as raw materials for comprehensive refining at present.
The oleaster can utilize marginal land, has excellent characteristics of drought resistance, salt and alkali resistance and the like, can be planted in deserts and other lands, and can play roles in preventing wind, fixing sand and preventing water and soil loss. Oleaster is widely planted in northeast, north China, northwest and other areas in China for wind prevention and sand fixation, and becomes a rich natural resource. The oleaster fruit can be eaten, but the taste varies greatly with the species and the place of production, and is usually used as a feed for feeding livestock. If the elaeagnus angustifolia fruits are comprehensively utilized to obtain various products, the economic value of elaeagnus angustifolia planting can be further improved. Therefore, the invention provides a method for biologically refining the elaeagnus angustifolia fruits, which converts the elaeagnus angustifolia fruits into various products, realizes the comprehensive utilization of the elaeagnus angustifolia fruits and improves the economic benefit.
Disclosure of Invention
In order to overcome the technical problems, the invention aims to provide a comprehensive biorefinery method which takes fructus elaeagnus angustifoliae as a raw material to convert and produce ethanol, protein feed, epoxy plasticizer and active carbon. The method provided by the invention is developed based on the following analysis and recognition.
Oleaster fruit is rich in fermentable sugar content and contains a certain amount of starch and cellulose. These fermentable sugars and glycans can be used by microorganisms as a carbon source for fermentation conversion, for example, to ethanol by Saccharomyces cerevisiae fermentation. Ethanol can be used as an energy source after being mixed with gasoline as a green fuel. The fructus Elaeagni Angustifoliae has high content of antioxidant and trace elements, and the fermented solid residue can be used together with yeast as animal feed. In addition, the kernel oil in the oleaster pit is rich in unsaturated double bonds, and the epoxy plasticizer can be prepared through epoxidation, so that the epoxy plasticizer prepared from edible oil sources such as epoxidized soybean oil and the like is replaced. The oleaster pit is rich in lignin and is an excellent raw material for preparing activated carbon. Therefore, the elaeagnus angustifolia fruit conversion production of various products can be realized by the biorefinery technology, and the economic benefit of the process is remarkably improved.
The technical scheme adopted by the invention for achieving the purpose is as follows:
the invention provides a comprehensive biological refining method taking fructus elaeagnus angustifoliae as a raw material, which comprises the following steps:
step 1, separating pulp and pit of the elaeagnus angustifolia fruits to obtain elaeagnus angustifolia fruit pulp powder and elaeagnus angustifolia pit;
step 2, performing bioconversion on the elaeagnus angustifolia fruit flesh powder to obtain ethanol and protein feed;
step 3, squeezing and extracting oil from the oleaster pits to obtain kernel oil and pit residues;
step 4, epoxidation is carried out on the kernel oil to obtain an epoxy plasticizer;
and 5, carbonizing the kernel residues to obtain the activated carbon.
The comprehensive biological refining method using the elaeagnus angustifolia fruits as the raw material, wherein the pulp and the pit are separated in the step 1 through mechanical milling; optionally, the milling is performed at ambient temperature. The separation of pulp and pit can be achieved by simple mechanical crushing due to the different hardness of pulp and pit, and in order to avoid sugar loss during crushing, the preferred crushing process of the invention is carried out at normal temperature.
The comprehensive biorefinery method using the elaeagnus angustifolia fruits as the raw material, wherein the ethanol obtained by the bioconversion in the step 2 is obtained by the reaction under the catalysis of amylase and cellulase; the protein feed obtained by bioconversion is obtained by fermentation with Saccharomyces cerevisiae in an ammonium sulfate medium.
The comprehensive biorefinery method using the elaeagnus angustifolia fruits as the raw material, wherein the bioconversion of the elaeagnus angustifolia fruit flesh powder in the step 2 is realized by the following steps:
step 2-1, adding amylase with the mass fraction of 1-3% and cellulase with the mass fraction of 0.5-2% into the elaeagnus angustifolia fruit pulp powder, and treating for 20-150 minutes under the conditions that the solid-liquid mass ratio is 1:10-1:20, the temperature is 15-90 ℃ and the stirring speed is 100-1000rpm to obtain a liquid-solid mixture;
2-2, adding ammonium sulfate with the mass fraction of 1-3% into the liquid-solid mixture, inoculating saccharomyces cerevisiae with the mass fraction of 1-5%, and fermenting for 12-72 hours at the temperature of 30-35 ℃ and the pH value of 4.5-6.0 to obtain mash;
and 2-3, carrying out liquid-solid separation on the mash, rectifying and dehydrating the obtained liquid phase to obtain absolute ethyl alcohol, and drying the obtained solid phase to obtain the protein feed.
The elaeagnus angustifolia pulp powder contains a large amount of fermentable sugar, mainly glucose and fructose, and the sugar can be directly utilized by Saccharomyces cerevisiae to be converted into ethanol. However, starch and cellulose in the fruit powder cannot be directly utilized by yeast and require prior saccharification to monosaccharides such as glucose. Therefore, starch and cellulose can be converted into monosaccharide by adding 1-3% of amylase and 0.5-2% of cellulase by mass fraction, and the yield of ethanol is improved. Meanwhile, in the thallus fermentation process, ammonium sulfate and part of carbon source are used for growth to obtain single-cell protein, and the single-cell protein and fermentation residues are dried together to obtain the protein feed.
In the above comprehensive biological refining method using fructus Elaeagni Angustifoliae as raw material, in the step 3, before squeezing and extracting oil from the fructus Elaeagni Angustifoliae kernel, drying is performed; optionally, the conditions of the drying treatment are: the drying temperature is 80-120 ℃ and the drying time is 1-10 hours. Preferably, the pressing and oil extraction are physical pressing and solvent extraction; the solvent is selected from one or more of n-hexane, cyclohexane, petroleum ether, chloroform, acetone, ethanol, methanol and diethyl ether. The grease extraction rate can be improved by combining physical pressing and solvent extraction.
The above comprehensive biorefinery method using fructus Elaeagni Angustifoliae fruit as raw material, wherein the epoxidation of the kernel oil in step 4 is achieved by the following steps:
step 4-1, mixing kernel oil and formic acid, dropwise adding 30% hydrogen peroxide under the stirring speed of 200-800rpm by taking sulfuric acid as a catalyst, and reacting for 1-6 hours at 20-80 ℃ to obtain an oil-water mixture;
and 4-2, performing oil-water separation on the oil-water mixture, and performing water washing, reduced pressure evaporation and drying on the obtained oil phase to obtain the epoxy plasticizer.
In the above comprehensive biological refining method using fructus Elaeagni Angustifoliae as raw material, in step 4-1, formic acid is 5-20% of oil weight, sulfuric acid is 0.1-0.6% of oil weight, and hydrogen peroxide is 30-120% of oil weight.
In the process, formic acid is used as an oxygen carrier to react with hydrogen peroxide under the catalysis of autocatalysis and trace sulfuric acid to generate peroxyformic acid, and the peroxyformic acid further performs epoxidation reaction with unsaturated double bonds in oil. The amounts of formic acid and sulfuric acid are particularly important to enhance the selectivity of the epoxidation. The high amounts of formic acid and sulfuric acid increase the rate of epoxidation but also accelerate ring opening side reactions of the epoxide groups. Thus, the preferred formic acid is used in an amount of 5 to 20% by weight of the oil and the preferred sulfuric acid is used in an amount of 0.1 to 0.6% by weight of the oil. Because the oil-water reaction is a two-phase reaction, in order to promote the reaction kinetics, the system needs to be assisted by good stirring to increase the reaction interface. The dosage and the reaction temperature of the hydrogen peroxide also obviously influence the reaction rate and the reaction selectivity, meanwhile, the reaction of the hydrogen peroxide and the formic acid is exothermic, and 30 percent of hydrogen peroxide is slowly added in a dropwise manner in order to avoid overhigh system temperature caused by severe reaction. By controlling the conditions, the fructus oleaster kernel oil can be well epoxidized, and a product with a higher epoxy value can be obtained.
The above comprehensive biorefinery method using fructus Elaeagni Angustifoliae fruit as raw material, wherein the carbonization of the kernel residue in step 5 is realized by the following steps:
step 5-1, crushing the kernel residues to 60-150 meshes to obtain kernel residue powder;
step 5-2, mixing the kernel residue powder with an activator according to a mass ratio of 1:0.2-1:2, and then treating for 20-120 minutes under the conditions that the temperature is 20-80 ℃ and the stirring speed is 100-300rpm to obtain dry powder;
and 5-3, carbonizing the dry powder in a nitrogen atmosphere for 30-120 minutes at the temperature rising rate of 5-30 ℃/min and the carbonization temperature of 500-900 ℃, cooling, washing with water, and drying to obtain the activated carbon.
The comprehensive biological refining method using fructus elaeagnus angustifoliae as the raw material is characterized in that the activating agent is selected from one of phosphoric acid, zinc chloride and potassium hydroxide.
The oleaster pit residue is rich in lignin, and can be used for preparing active carbon. The porosity and the adsorption capacity of the obtained activated carbon product can be improved after activation and carbonization.
The oleaster fruit serving as a non-grain crop is rich in soluble monosaccharide with good content, sugar available for microbial fermentation can be obtained without additional chemical pretreatment, and the kernel contains unsaturated fatty acid, is suitable for epoxidation, and the kernel is rich in lignin, so that the oleaster fruit is a good raw material for preparing activated carbon. In addition, the oleaster can grow in a wide area, is resistant to salt and alkali, drought, barren and the like, and can fully utilize marginal land to play the roles of wind prevention, sand fixation and water and soil loss prevention. The biological refining of the elaeagnus angustifolia fruits can fully utilize the components, can provide new energy of fuel ethanol to relieve energy crisis and environmental pollution, can promote mass planting of elaeagnus angustifolia plants to promote water and soil conservation, fully utilizes marginal land, and has remarkable environmental and economic benefits.
The beneficial effects of the invention are as follows: the method provided by the invention can convert the fructus oleaster fruits into ethanol, protein feed, epoxy plasticizer and active carbon, thereby avoiding the complicated pretreatment process, fully utilizing the components such as fermentable sugar, starch, cellulose, lignin and the like which are rich in the fructus oleaster fruits, converting the starch and cellulose into monosaccharide by using amylase and cellulase with specific proportion, improving the yield of the ethanol, simultaneously utilizing ammonium sulfate and partial carbon source to grow in the thallus fermentation process to obtain the protein feed, and optimizing the reaction rate and the reaction selectivity of epoxidation by using the preferential dosage of formic acid, sulfuric acid and hydrogen peroxide so as to obtain the epoxy plasticizer with higher epoxy value.
Drawings
The invention will be further described with reference to the drawings and examples.
FIG. 1 is a flow chart of the comprehensive biorefinery of fructus Elaeagni Angustifoliae.
Detailed Description
The present invention will be further illustrated by the following examples, which are not intended to limit the scope of the invention.
Example 1: analysis of fermentable sugar components of elaeagnus angustifolia fruit powder and optimization of dissolution conditions
The fructus Elaeagni Angustifoliae is produced from Ningxia. Removing the pit after mechanical crushing, and obtaining the elaeagnus angustifolia fruit flesh powder after further mechanical crushing of the pulp. The mass content of the main components in the fruit powder is measured as follows: the water content was 18.0%, the glucose content was 21.56%, the fructose content was 20.13%, the starch content was 7.70%, the cellulose content was 3.30%, and the protein content was 0.70%. In addition, the content of each element in the elaeagnus angustifolia fruit flesh powder (XRF analysis and detection) is shown in table 1 below. Wherein, mg, P, S, cl, K, ca is inorganic salt element necessary for producing ethanol by yeast fermentation.
Analysis of each element and content of the fructus Elaeagni Angustifoliae fruit powder used in Table 1
The fructus Elaeagni Angustifoliae pulp powder was dissolved at a concentration of 100g/L at 30℃and stirring rates of 0rpm, 100rpm and 200rpm for 90 minutes, and it was found that the fructus Elaeagni Angustifoliae pulp powder had the maximum concentration of soluble sugar in an aqueous solution at a stirring rate of 100rpm, wherein the concentrations of glucose and fructose were 29.67g/L and 33.82g/L, respectively.
The oleaster pulp powder was treated at a concentration of 100g/L for 30-90 minutes at different temperatures (20 ℃,30 ℃, 37 ℃, 50 ℃) with a stirring rate of 100rpm, and the temperature was found to have no significant effect on the dissolution of fermentable sugars.
Example 2: effect of amylase addition on fermentable sugar digestion
The effect of adding and not adding amylase is compared under the condition of 100g/L of the elaeagnus angustifolia pulp powder concentration, and the result shows that the amylase with the mass fraction of 1.8% based on the pulp powder can improve the concentration of glucose dissolution rate by 24% and the fructose dissolution rate by 18%.
Example 3: ethanol production by directly dissolving out fermentable sugar from elaeagnus angustifolia pulp powder and fermenting
The fructus oleaster pulp powder and the nutrient substances are prepared into a fermentation culture medium according to the following compositions: oleaster powder 100g/L, (NH) 4 ) 2 SO 4 2.0g/L、K 2 HPO 4 5.0g/L, yeast extract 5.0g/L, mgSO 4 1.0g/L、CaCl 2 0.2g/L. The saccharomyces cerevisiae is inoculated according to 10 percent of inoculation amount, glucose dissolved out from the elaeagnus angustifolia fruit pulp powder after 24 hours of fermentation can be completely utilized, the utilization rate of fructose is 87.47 percent, the concentration of ethanol is 19.36g/L, and the yield of ethanol is 194g/kg elaeagnus angustifolia fruit pulp powder. The method shows that the fermentable sugar dissolved out by the elaeagnus angustifolia fruit pulp powder can be well converted into ethanol by the saccharomyces cerevisiae.
Example 4: ethanol is produced by fermenting the soluble sugar dissolved out after amylase saccharification is added into elaeagnus angustifolia pulp powder
Adding amylase with the mass fraction of 1.8% into 100g/L elaeagnus angustifolia fruit pulp powder for enzymolysis saccharification to obtain 31.18g/L glucose and 29.82g/L fructose. Further fermentation was performed according to the medium formulation of example 3, and after 24 hours of fermentation both glucose and fructose were fully utilized, with a maximum ethanol concentration of 25.19g/L and an ethanol yield of 252g/kg oleaster pulp powder. The result shows that the ethanol yield can be effectively improved after amylase is added to saccharify starch in the elaeagnus angustifolia fruit powder.
Example 5: thick mash fermentation of elaeagnus angustifolia fruit pulp powder
The fermentation medium composition was as in example 3, but when the concentration of the elaeagnus angustifolia fruit powder was adjusted to 200g/L, 300g/L, 400g/L and 500g/L, saccharification was carried out by adding amylase in an amount of 1.8% by mass. Fermentation was performed in shake flasks. As can be seen, as the concentration of the elaeagnus angustifolia fruit pulp powder increased, the ethanol concentration in the fermentation broth increased, and the ethanol concentrations in the fermentation broth were 20.59g/L, 30.60g/L, 39.30g/L and 47.21g/L, respectively, with 200g/L, 300g/L, 400g/L, 500g/L elaeagnus angustifolia fruit pulp powder, and the sugar alcohol conversions were 73.42%, 67.09%, 68.95% and 68.23%, respectively. The method shows that in the thick mash fermentation process, the concentration of the elaeagnus angustifolia fruit pulp powder can be increased, but the ethanol yield is reduced.
Further, the pulp powder was fed to a 1L fermenter at an initial pulp powder concentration of 200g/L for every 24 hours, and the results are shown in Table 2 below:
table 2 experiment results of ethanol production by batch fermentation of fructus Elaeagni Angustifoliae fruit powder
It can be seen that fermentation is performed in the fermenter, and the ethanol concentration is significantly increased compared with the shaking flask fermentation due to good stirring, and the sugar alcohol conversion rate is significantly increased. The ethanol concentration in the fermentation liquid can be effectively improved by the fed-batch fermentation, but the sugar alcohol conversion rate is reduced. This is due to the increased solids content in the fermentation system, reduced free moisture, and unfavorable mass transfer.
Example 6: fermentation residues and thalli as protein feed
100g/L elaeagnus angustifolia fruit pulp powder is subjected to amylase enzymolysis and Saccharomyces cerevisiae fermentation, fermented mash is filtered, and the residual solid is subjected to freeze drying. The solids, analyzed, contained 15% cellulose, 40% protein, 10% soluble polysaccharide, and 5% inorganic salt. The proteins in the remaining solids are mainly derived from the fermentation broths. The amino acid composition of a particular protein was analyzed and the results are shown in table 3 below:
TABLE 3 composition of amino acids of mycoprotein of Saccharomyces cerevisiae cultured with elaeagnus angustifolia pulp powder
As can be seen, the mycoprotein has rich amino acid species and meets the requirement of amino acid as protein for animal feed.
Example 7: analysis of components of oleaster pit extract and nutlet oil
The oleaster pit obtained in example 1 was dried at 105℃for 6 hours, and after pulverization, extracted with cyclohexane to obtain a nut oil and pit residue, wherein the oil yield was 10g of oil per 100g of dry pit. The fatty acid composition of the obtained oil was measured after the oil was converted into fatty acid methyl ester by lipase-catalyzed methanolysis, and the results are shown in the following table 4:
table 4 fatty acid composition of oleaster seed oil
| Fatty acid | C16:0 | C16:1 | C18:0 | C18:1 | C18:2 | C18:3 | C19:0 | C19:1 | Others |
| Content (%) | 3.79 | 0.16 | 2.06 | 24.85 | 50.50 | 15.36 | 0.28 | 0.54 | 0.88 |
The fatty acid of the elaeagnus angustifolia seed oil is mainly linoleic acid, the content of the elaeagnus angustifolia seed oil is up to 50.5%, the content of the elaeagnus angustifolia seed oil is 24.85%, the content of the elaeagnus angustifolia seed oil is 15.36%, and the content of the three unsaturated fatty acids is up to 90.7% and is higher than the content of the unsaturated fatty acids of soybean oil, so that the elaeagnus angustifolia seed oil can be used as an excellent raw material for preparing the epoxy oil plasticizer.
Example 8: epoxy oil plasticizer prepared from fructus Elaeagni Angustifoliae kernel oil
50g of the oleaster seed oil obtained in example 7 was mixed with 15% formic acid based on the weight of the oil, sulfuric acid 0.3% based on the weight of the oil was added as a catalyst, and a 30% hydrogen peroxide solution 80% based on the weight of the oil was dropped with a stirring rate of 600rpm, and reacted at 60℃for 6 hours. After the reaction is finished, centrifugally separating an oil layer, and washing by adopting deionized water until the washing liquid is neutral. After centrifugation and evaporation under reduced pressure at 60℃the epoxy value was determined to be 6.4%. The epoxy value meets the industry standard of the epoxidized soybean oil (HGT 4386-2012 chemical industry standard, plasticizer-epoxidized soybean oil) and is higher than the highest epoxy value (6.2%) which can be achieved by the epoxidized soybean oil. This is mainly due to the higher unsaturated fatty acid content of the elaeagnus angustifolia seed oil. The prepared fructus oleaster kernel oil is a good raw material for preparing the epoxy plasticizer.
Example 9: preparation of active carbon from kernel residue
Drying the kernel residue obtained in example 7, pulverizing to below 80 mesh, mixing with 20% potassium hydroxide solution at a mass ratio of 1:2, activating at 110deg.C for 60 min, heating to 700deg.C at a heating rate of 20deg.C/min in nitrogen atmosphere, carbonizing at 700deg.C for 30 min, cooling, washing with deionized water, and drying at 105deg.C to obtain active carbon powder. The activated carbon powder was found to have a particle size of 1250m 2 The specific surface area per gram was 135mg/g for methylene blue adsorption. The prepared activated carbon powder has higher specific surface area and good adsorption performance.
The above description is only of the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any person skilled in the art can make many possible variations and modifications to the technical solution of the present invention or modifications to equivalent embodiments using the technical means and technical contents disclosed above without departing from the scope of the technical solution of the present invention. Therefore, all equivalent changes according to the shape, structure and principle of the present invention should be covered in the protection scope of the present invention.
Claims (10)
1. The comprehensive biological refining method using the elaeagnus angustifolia fruits as raw materials is characterized by comprising the following steps of:
step 1, separating pulp and pit of the elaeagnus angustifolia fruits to obtain elaeagnus angustifolia fruit pulp powder and elaeagnus angustifolia pit;
step 2, performing bioconversion on the elaeagnus angustifolia fruit flesh powder to obtain ethanol and protein feed;
step 3, squeezing and extracting oil from the oleaster pits to obtain kernel oil and pit residues;
step 4, epoxidation is carried out on the kernel oil to obtain an epoxy plasticizer;
and 5, carbonizing the kernel residues to obtain the activated carbon.
2. The integrated biorefinery with elaeagnus angustifolia fruits as claimed in claim 1, wherein the separation of pulp and pit in step 1 is achieved by mechanical milling;
optionally, the milling is performed at ambient temperature.
3. The comprehensive biorefinery process with oleaster fruits as raw materials of claim 1, wherein the biotransformation in step 2 is carried out under the catalysis of amylase and cellulase to obtain ethanol;
the protein feed obtained by bioconversion is obtained by fermentation with Saccharomyces cerevisiae in an ammonium sulfate medium.
4. The comprehensive biorefinery method of claim 3 wherein said bioconversion of said fructus Elaeagni Angustifoliae pulp powder in step 2 is accomplished by:
step 2-1, adding amylase with the mass fraction of 1-3% and cellulase with the mass fraction of 0.5-2% into the elaeagnus angustifolia fruit pulp powder, and treating for 20-150 minutes under the conditions that the solid-liquid mass ratio is 1:10-1:20, the temperature is 15-90 ℃ and the stirring speed is 100-1000rpm to obtain a liquid-solid mixture;
2-2, adding ammonium sulfate with the mass fraction of 1-3% into the liquid-solid mixture, inoculating saccharomyces cerevisiae with the mass fraction of 1-5%, and fermenting for 12-72 hours at the temperature of 30-35 ℃ and the pH value of 4.5-6.0 to obtain mash;
and 2-3, carrying out liquid-solid separation on the mash, rectifying and dehydrating the obtained liquid phase to obtain absolute ethyl alcohol, and drying the obtained solid phase to obtain the protein feed.
5. The method for comprehensive biorefinery with oleaster fruit as raw material according to claim 1, wherein in the step 3, before squeezing and extracting oil from the oleaster fruit pit, drying treatment is performed;
optionally, the conditions of the drying treatment are: the drying temperature is 80-120 ℃ and the drying time is 1-10 hours.
6. The method according to claim 5, wherein in step 3, the squeezing and oil extraction are physical squeezing and solvent extraction;
optionally, the solvent is selected from one or more of n-hexane, cyclohexane, petroleum ether, chloroform, acetone, ethanol, methanol, diethyl ether.
7. The method for comprehensive biorefinery with elaeagnus angustifolia fruits as claimed in claim 1, wherein the epoxidation of the nutlet oil in step 4 is achieved by:
step 4-1, mixing kernel oil and formic acid, dropwise adding 30% hydrogen peroxide under the stirring speed of 200-800rpm by taking sulfuric acid as a catalyst, and reacting for 1-6 hours at 20-80 ℃ to obtain an oil-water mixture;
and 4-2, performing oil-water separation on the oil-water mixture, and performing water washing, reduced pressure evaporation and drying on the obtained oil phase to obtain the epoxy plasticizer.
8. The method according to claim 7, wherein in the step 4-1, formic acid is used in an amount of 5-20% by weight of the fat, sulfuric acid is used in an amount of 0.1-0.6% by weight of the fat, and hydrogen peroxide is used in an amount of 30-120% by weight of the fat.
9. The comprehensive biorefinery with elaeagnus angustifolia fruits as claimed in claim 1, wherein the carbonizing of the kernel residues in step 5 is achieved by:
step 5-1, crushing the kernel residues to 60-150 meshes to obtain kernel residue powder;
step 5-2, mixing the kernel residue powder with an activator according to a mass ratio of 1:0.2-1:2, and then treating for 20-120 minutes under the conditions that the temperature is 20-80 ℃ and the stirring speed is 100-300rpm to obtain dry powder;
and 5-3, carbonizing the dry powder in a nitrogen atmosphere for 30-120 minutes at the temperature rising rate of 5-30 ℃/min and the carbonization temperature of 500-900 ℃, cooling, washing with water, and drying to obtain the activated carbon.
10. The integrated biorefinery with elaeagnus angustifolia fruits as claimed in claim 9, wherein the activator is one selected from phosphoric acid, zinc chloride and potassium hydroxide.
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