CN103819514A - Cotton seed meal dephenolizing technology and method for preparing raffinose from cotton seed meal by technology - Google Patents
Cotton seed meal dephenolizing technology and method for preparing raffinose from cotton seed meal by technology Download PDFInfo
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Abstract
The invention relates to a cotton seed meal dephenolizing technology and a method for preparing raffinose from cotton seed meal by the technology. The cotton seed meal dephenolizing technology comprises the following steps: utilizing degreased cotton seed meal as a raw material, pulverizing, sieving, removing cotton flock and cotton hulls, adding ferrous sulfate, adding an ethanol water solution, adding a Na2CO3 conditioner, regulating the PH value to 7-9, agitating, uniformly mixing, and carrying out extrusion and detoxification treatment by a bulking machine so as to obtain extruded and detoxified cotton seed meal. The method for preparing the raffinose from the cotton seed meal by the cotton seed meal dephenolizing technology comprises the following steps: preparing the dephenolized cotton seed meal, and extracting by an alcoholic acid solution; fetching a filtrate, adding phase decoloring activated carbon, distilling under reduced pressure, recovering a solvent, concentrating the filtrate, and then filtering; concentrating and drying to obtain a crude raffinose product; utilizing absolute ethyl alcohol in drip washing, crystallizing after heating and dissolving, and obtaining the raffinose after drying. The cotton seed meal dephenolizing technology is economical and practical, is simple in operation and has great dephenolizing efficiency. The method provided by the invention is rapid, efficient, simple and convenient.
Description
Technical field
The present invention relates to a kind of cotton dregs dephenolize technology and utilize this technology from cotton dregs, to prepare the method for raffinose.
Background technology
Raffinose (raffinose) claim again raffinose, is made up of a part α-D-galactopyranose (1 → 6), a part α-D-Glucopyranose (1 → 2) and beta-D-fructofuranose, and molecular formula is C
18h
32o
16, relative molecular weight is 504, sugariness is sucrose 20% ~ 40%.Raffinose is the important component part of functional oligose soybean oligosaccharide, it is good bifidus bacillus multiplicaiton factor, to human body have the functions of intestines and stomach of improvement and, improve immunity of organisms and the disease-resistant different physiological roles such as liver of protecting, raffinose is extensively present in beet, cottonseed, honey, Caulis et Folium Brassicae capitatae, yeast, potato, grape, wheat class, corn and seeds of leguminous plant, Japan began one's study and from beet sirup, extracts raffinose as far back as 1977, started suitability for industrialized production in 1991.The larger market share has been occupied in current Japanese oligose market.What in plant, raffinose content was the highest is cottonseed, and cottonseed processing primary product is Oleum Gossypii semen and cottonseed meal, and raffinose mainly retains in cottonseed meal, is generally 5%～9%.In cottonseed meal, raffinose content is the more than 5 times of beet sirup, and in beet, raffinose content is 1.0～1.1%.From cottonseed meal, extract and prepare raffinose and there is vast potential for future development.
China is the first in the world Chan Mian big country, and look body of gland is contained but principal item is common cottonseed in ten thousand tons of cottonseed annual production 960 ~ 1100, and Glandless cotton plantation is few.Owing to containing the pigments such as poisonous gossypol in common cottonseed look body of gland, extracting before raffinose, should first be removed or gossypol be removed in purge process as far as possible, the existence of free gossypol becomes restriction and utilizes cotton dregs to prepare a key factor of raffinose.According to the literature, extract at present that raffinose is adopted water mostly and alcohols is made raffinose in solvent extraction low-phenol cottonseed from cottonseed meal, removing of free gossypol is more difficult.Zheng Jianxian proposes to add aniline in Glanded cottonseed alcohol leaching liquid, removes gossypol in leach liquor.From cotton dregs, extract raffinose and also can in purge process, remove gossypol, as described in patent CN200810089636.2, degreased cottonseed meal adopts methanol extraction, obtain the methanol extraction liquid containing phenol and raffinose, through 80～100 ℃ of distillation methanol removals and gossypol, concentrated, obtain raffinose coarse fodder.In addition, from cottonseed meal, extract raffinose extraction efficiency low.Russian Ivanovs in 1984 etc., take 85% ethanol as extraction agent, extract raffinose from cottonseed meal, and the rate of recovery is brought up to 56.45%, and yield is 3.3%, is in all report Glanded cottonseed, to extract raffinose up to now the report that yield is the highest.But these methods not yet realize industrialization.Its reason is that methyl alcohol or ethonal extraction are high to ingredient requirement, require methyl alcohol or alcohol solvent concentration expressed in percentage by volume more than 80% to reach the object of dephenolize in extracting raffinose, in addition, single solvent extraction mode efficiency is lower, solvent consumption is large, and the recovery of solvent and dephenolizing process limit its suitability for industrialized production process.
In recent years, cotton seed dephenolization equipment and technology is progressive gradually, thereby making to extract take cottonseed protein after dephenolize as raw material prepares raffinose and become possibility, provides a new thinking and larger selection space for raffinose extracts technology of preparing.
Summary of the invention
The object of the present invention is to provide a kind of economical and practical, simple to operate, dephenolize efficiency is high, can be used for extracting the cotton dregs dephenolize technology of preparing raffinose dephenolization cottonseed protein.
Another object of the present invention is on the basis of above-mentioned cotton dregs dephenolize technology, take dephenolize cotton dregs as raw material, a kind of efficient, easy, safety is provided, easily realize the extraction of suitability for industrialized production and prepare raffinose processing method, solve and from common cotton dregs, extract that the existing extraction efficiency of raffinose is low, extraction time is long, free gossypol removes difficult problem.
The invention discloses a kind of cotton dregs dephenolize technology, it is characterized in that mainly comprising following processing step:
Take defatted cotton dregs as raw material, pulverized 90～110 mesh sieves, remove velveteen and boll hull, the amount of substance is equivalent to the ferrous sulfate of 1～1.2 times of raw material Free Gossypol amount of substance, the aqueous ethanolic solution that the concentration expressed in percentage by volume that adds weight to be equivalent to weight of material 1/5～1/4 is 50%～60%, adds Na
2cO
3adjust material pH value to 7～9, stirring and evenly mixing, utilizes bulking machine to carry out extruding puffing detoxification treatment, its bulking process parameter: 135～140 ℃ of swelling temperatures, 150～170 revs/min of screw speeds, 3～5 millimeters of die throat diameters; Obtain expanded detoxification cotton dregs.
Described Na
2cO
3can use NaOH, ammoniacal liquor, liming one wherein to replace.
Utilize described cotton dregs dephenolize technology from cotton dregs, to prepare a method for raffinose, it is characterized in that mainly realizing by following processing step:
(1) cotton dregs dephenolize preparation: take defatted cotton dregs as raw material, pulverized 90～110 mesh sieves, remove velveteen and boll hull, the amount of substance is equivalent to the ferrous sulfate of 1～1.2 times of raw material Free Gossypol amount of substance, the aqueous ethanolic solution that the concentration expressed in percentage by volume that adds weight to be equivalent to weight of material 1/5～1/4 is 50%～60%, adds Na
2cO
3adjust material pH value to 7～9, stirring and evenly mixing, utilizes bulking machine to carry out extruding puffing detoxification treatment, its bulking process parameter: 135～140 ℃ of swelling temperatures; 150～170 revs/min of screw speeds; 3～5 millimeters of die throat diameters, obtain expanded detoxification cotton dregs;
(2) alkyd solution is extracted: take above-mentioned expanded detoxification cotton dregs as raw material, press solid-liquid ratio 1:10～1:15, adding concentration expressed in percentage by volume is 50%～70% alcoholic solution, aqueous acid adjust pH to 4～5, at 70～80 ℃ of temperature, lixiviate 15～30 minutes, extracting solution adopts filter to filter, filtrate being used for extracted raffinose, and filter residue is dried as cottonseed crude protein;
(3) get above-mentioned filtrate, adding and being equivalent to filtrate weight 0.8%～1% granularity is 10～40 object decoloration active carbons, 50～70 ℃ of underpressure distillation, reclaim solvent, filtrate be concentrated into original volume 1/5～1/4 after, concentrated solution is filtered;
(4) get filtrate, concentrate drying, obtain raffinose crude product, raffinose crude product utilizes dehydrated alcohol drip washing, then joining concentration expressed in percentage by volume in the ratio of solid-liquid ratio 1:10～1:12 is in 70%～80% aqueous ethanolic solution, heating for dissolving, 0～10 ℃ of crystallization 30～40 hours, obtain crystal, after oven dry, obtain raffinose finished product.
It is the drip washing of 75%-80% aqueous ethanolic solution replacement dehydrated alcohol that described raffinose crude product preferably utilizes the concentration expressed in percentage by volume that salt is saturated.
Alcoholic solution in described alcohol aqueous acid is preferably the one in methyl alcohol or ethanol, and aqueous acid is wherein preferably the one in hydrochloric acid or sulfuric acid.
Described filter is preferably diatomite plate and frame filter.
Compared with prior art, advantage of the present invention and innovation are:
Technique simple and fast of the present invention, can be continuously produced, and is suitable for commercial running and produces, and raffinose extraction efficiency is high, and raffinose total recovery is more than 70%, and gained raffinose product quality is higher, and purity is more than 98%, and free gossypol content is lower than detection limit 20mg/kg.
1, raw material processing aspect:
The present invention adopts the mode of adding ethanol in raw material, in puffing process, reach the effect of alcohol vapour explosion, a free gossypol part in material forms bound gossoypol in extrusion pressing puffing process, meanwhile free gossypol is in the process of being extruded by mould mouth with material, free gossypol and second alcohol and water mix vapor phase mutual effect, the content of free gossypol is minimized, after detoxification, free gossypol content is not more than 90 mg/kg, in extrusion pressing puffing process, add ethanol, reduce on the one hand free gossypol content, on the other hand, in extrusion pressing puffing process, the ethanol moment gasification of over-heat inside state, the very fast expansion of volume, the huge swelling pressure have not only been destroyed the external status of particle, and break the molecular structure of material particles inside, porosity and the perviousness of material greatly improve, raffinose is discharged, material directly carries out extraction, extraction efficiency greatly improves.By relatively finding, in extrusion pressing puffing process, add ethanol, all to have unusual effect aspect raising dephenolize efficiency or raising raffinose extraction yield, free gossypol content does not add the direct expanded material of ethanol to be reduced more than 10%, and raffinose yield has improved more than 30% than never Expanding cottonseed powder extraction raffinose, extraction time shortens over half, reaches same effect and can reduce solvent load more than 1/3.
2, extract solvent selection aspect:
Adopt 50% ~ 70% alcohol aqueous acid, sour water has increased the perviousness of material on the one hand, adopt the extracting solution of lower determining alcohol to increase the solubleness of raffinose, adopt on the other hand the alkyd extracting solution of pH 4 ~ 5, cottonseed protein is precipitated, in extracting solution, foreign matter content is extraction using alcohol 40% ~ 50%, is 50% ~ 60% of acid water extracting liquid, is conducive to follow-up raffinose purifies and separates.
3, raffinose purification aspect:
In decoloration process process of the present invention, the method that employing is treated different things alike, in extraction filtrate, directly add decoloration active carbon, to concentrate with decoloration process and merge into a step, the dephenolize of decolouring on the one hand, concentration and recovery solvent on the other hand, the rate of recovery of solvent is higher, it is low to reclaim the Impurities In Solvents content obtaining, save cost, improved production efficiency.
The invention provides a kind of economical and practical, simple to operate, the good cotton dregs dephenolize of dephenolize efficiency technology.In addition, this technology of utilizing providing is extracted the method for preparing raffinose from cotton dregs, utilize extruding puffing auxiliary extraction technology, it is a kind of extracting mode that is easy to realize suitability for industrialized production, greatly having improved and from cotton dregs, extracted the yield of preparing raffinose, is that a kind of quick, efficient, easy raffinose extracts preparation method.
Embodiment
Embodiment 1:
A kind of cotton dregs dephenolize technology, mainly comprises following processing step:
Take defatted cotton dregs as raw material, pulverized 90 mesh sieves, and removed velveteen and boll hull, the amount of substance is equivalent to the ferrous sulfate of 1 times of raw material Free Gossypol amount of substance, the aqueous ethanolic solution that the concentration expressed in percentage by volume that adds weight to be equivalent to weight of material 1/5 is 50%, adds Na
2cO
3adjust pH value to 7, stirring and evenly mixing, utilizes bulking machine to carry out extruding puffing detoxification treatment, its bulking process parameter: 135 ℃ of swelling temperatures, 150 revs/min of screw speeds, 3 millimeters of die throat diameters; Obtain expanded detoxification cotton dregs.
Embodiment 2:
Compared with embodiment 1, the difference of the present embodiment is:
Take defatted cotton dregs as raw material, pulverized 100 mesh sieves, remove velveteen and boll hull, the amount of substance is equivalent to the ferrous sulfate of 1.1 times of raw material Free Gossypol amount of substances, the aqueous ethanolic solution that the concentration expressed in percentage by volume that adds weight to be equivalent to weight of material 1/4 is 60%, add NaOH and adjust pH value to 7.5, stirring and evenly mixing, utilizes bulking machine to carry out extruding puffing detoxification treatment, its bulking process parameter: 138 ℃ of swelling temperatures, 170 revs/min of screw speeds, 3.5 millimeters of die throat diameters; Obtain expanded detoxification cotton dregs.
Embodiment 3:
Compared with embodiment 1, the difference of the present embodiment is:
Take defatted cotton dregs as raw material, pulverized 105 mesh sieves, remove velveteen and boll hull, the amount of substance is equivalent to the ferrous sulfate of 1.2 times of raw material Free Gossypol amount of substances, the aqueous ethanolic solution that the concentration expressed in percentage by volume that adds weight to be equivalent to weight of material 1/4 is 53%, add ammoniacal liquor and adjust pH value to 8, stirring and evenly mixing, utilizes bulking machine to carry out extruding puffing detoxification treatment, its bulking process parameter: 139 ℃ of swelling temperatures, 155 revs/min of screw speeds, 4 millimeters of die throat diameters; Obtain expanded detoxification cotton dregs.
Embodiment 4:
Compared with embodiment 1, the difference of the present embodiment is:
Take defatted cotton dregs as raw material, pulverized 110 mesh sieves, remove velveteen and boll hull, the amount of substance is equivalent to the ferrous sulfate of 1.15 times of raw material Free Gossypol amount of substances, the aqueous ethanolic solution that the concentration expressed in percentage by volume that adds weight to be equivalent to weight of material 1/5 is 58%, add liming and adjust pH value to 9, stirring and evenly mixing, utilizes bulking machine to carry out extruding puffing detoxification treatment, its bulking process parameter: 140 ℃ of swelling temperatures, 160 revs/min of screw speeds, 4.5 millimeters of die throat diameters; Obtain expanded detoxification cotton dregs.
Embodiment 5:
Compared with embodiment 1, the difference of the present embodiment is:
Take defatted cotton dregs as raw material, pulverized 100 mesh sieves, remove velveteen and boll hull, the amount of substance is equivalent to the ferrous sulfate of 1.2 times of raw material Free Gossypol amount of substances, the aqueous ethanolic solution that the concentration expressed in percentage by volume that adds weight to be equivalent to weight of material 1/5 is 52%, add liming and adjust pH value to 8.6, stirring and evenly mixing, utilizes bulking machine to carry out extruding puffing detoxification treatment, its bulking process parameter: 140 ℃ of swelling temperatures, 165 revs/min of screw speeds, 5 millimeters of die throat diameters; Obtain expanded detoxification cotton dregs.
embodiment 6:
The purchasing of raw materials is in Shihezi Hui Chang grease company limited (crude protein 40 ~ 44%, robust fibre 14 ~ 16%, crude fat 2% ~ 3%, moisture 10% ~ 12%, raffinose 5.0 ~ 5.1%, free gossypol 750 mg/kg ~ 800 mg/kg).
(1) cotton dregs dephenolize preparation: take defatted cotton dregs as raw material, pulverized 100 mesh sieves, remove velveteen and boll hull, the amount of substance is equivalent to the ferrous sulfate of 1 times of raw material Free Gossypol amount of substance, the aqueous ethanolic solution that the concentration expressed in percentage by volume that adds weight to be equivalent to weight of material 1/5 is 50%, adds Na
2cO
3adjust pH value to 8, stirring and evenly mixing, utilizes bulking machine to carry out extruding puffing detoxification treatment, its bulking process parameter: 140 ℃ of swelling temperatures; 150 revs/min of screw speeds; 3 millimeters of die throat diameters, obtain expanded detoxification cotton dregs;
(2) alkyd solution is extracted: take above-mentioned expanded detoxification cotton dregs as raw material, press solid-liquid ratio 1:10, adding concentration expressed in percentage by volume is 50% alcoholic solution, aqueous acid adjust pH to 4, at 70 ℃ of temperature, lixiviate 20 minutes, extracting solution adopts diatomite plate and frame filter to filter, filtrate being used for extracted raffinose, and filter residue is dried as cottonseed crude protein;
(3) get above-mentioned filtrate, add and be equivalent to the gac that filtrate weight 1% granularity is 20 orders decolourings, 50 ℃ of underpressure distillation, reclaim solvent, filtrate be concentrated into original volume 1/5 after, concentrated solution is carried out to diatomite filtration;
(4) get filtrate, concentrate drying, obtains raffinose crude product, raffinose crude product utilizes dehydrated alcohol drip washing, and then joining concentration expressed in percentage by volume in the ratio of solid-liquid ratio 1:10 is in 70% aqueous ethanolic solution, 80 ℃ of heating for dissolving, 0 ℃ of crystallization 30 hours, obtains crystal, obtains raffinose finished product after oven dry.
Experiment is divided into 2 groups, control group and experimental group, and control group is to pulverize cottonseed meal as raw material, concentration expressed in percentage by volume 80% aqueous ethanolic solution lixiviate (solid-liquid ratio 1:10,70 ℃ of extraction temperatures, 30 minutes extraction times, extraction time 2 times).
Calculate as follows raffinose yield: raffinose yield (%)=(raffinose crystal weight (g) × purity of raffinose ÷ cottonseed meal weight (g)) × 100
Experimental result shows that experimental group raffinose yield is that 3.7%(is with respect to dregs of rice weight), improve 37% compared with control group raffinose yield (2.7%), raffinose finished product purity 98.2%, free gossypol does not detect, product reaches the requirement of raffinose product standard, illustrate that technique extraction efficiency of the present invention is high, extraction time is short, easy and simple to handle, can be used for the extraction preparation of raffinose in defatted cotton dregs.
Embodiment 7:
Compared with embodiment 1, the difference of the present embodiment is:
(1) cotton dregs dephenolize preparation: take defatted cotton dregs as raw material, pulverized 90 mesh sieves, and removed velveteen and boll hull, the amount of substance is equivalent to the ferrous sulfate of 1 times of raw material Free Gossypol amount of substance, the aqueous ethanolic solution that the concentration expressed in percentage by volume that adds weight to be equivalent to weight of material 1/4 is 50%, adds Na
2cO
3adjust material pH value to 7, stirring and evenly mixing, utilizes bulking machine to carry out extruding puffing detoxification treatment, its bulking process parameter: 140 ℃ of swelling temperatures; 150 revs/min of screw speeds; 3 millimeters of die throat diameters, obtain expanded detoxification cotton dregs;
(2) alkyd solution is extracted: take above-mentioned expanded detoxification cotton dregs as raw material, press solid-liquid ratio 1:12, adding concentration expressed in percentage by volume is 50% alcoholic solution, aqueous acid adjust pH to 4, at 70 ℃ of temperature, lixiviate 15 minutes, extracting solution adopts filter to filter, filtrate being used for extracted raffinose, and filter residue is dried as cottonseed crude protein;
(3) get above-mentioned filtrate, add and be equivalent to the gac that filtrate weight 0.8% granularity is 10 orders decolourings, 50 ℃ of underpressure distillation, reclaim solvent, filtrate be concentrated into original volume 1/5 after, concentrated solution is filtered;
(4) get filtrate, concentrate drying, obtains raffinose crude product, raffinose crude product utilizes dehydrated alcohol drip washing, and then joining concentration expressed in percentage by volume in the ratio of solid-liquid ratio 1:10 is in 70% aqueous ethanolic solution, heating for dissolving, 3 ℃ of crystallizations 40 hours, obtain crystal, obtain raffinose finished product after oven dry.
Alcoholic solution in described alcohol aqueous acid is the one in methyl alcohol or ethanol, and aqueous acid is wherein the one in hydrochloric acid or sulfuric acid.
Embodiment 8:
Compared with embodiment 1, the difference of the present embodiment is:
(1) cotton dregs dephenolize preparation: take defatted cotton dregs as raw material, pulverized 105 mesh sieves, remove velveteen and boll hull, the amount of substance is equivalent to the ferrous sulfate of 1.1 times of raw material Free Gossypol amount of substances, the aqueous ethanolic solution that the concentration expressed in percentage by volume that adds weight to be equivalent to weight of material 0.22 is 55%, adds Na
2cO
3adjust material pH value to 9, stirring and evenly mixing, utilizes bulking machine to carry out extruding puffing detoxification treatment, its bulking process parameter: 138 ℃ of swelling temperatures; 155 revs/min of screw speeds; 4 millimeters of die throat diameters, obtain expanded detoxification cotton dregs;
(2) alkyd solution is extracted: take above-mentioned expanded detoxification cotton dregs as raw material, press solid-liquid ratio 1:13, adding concentration expressed in percentage by volume is 55% alcoholic solution, aqueous acid adjust pH to 4.3, at 73 ℃ of temperature, lixiviate 18 minutes, extracting solution adopts filter to filter, filtrate being used for extracted raffinose, and filter residue is dried as cottonseed crude protein;
(3) get above-mentioned filtrate, adding and being equivalent to filtrate weight 0.9% granularity is 30 object decoloration active carbons, 55 ℃ of underpressure distillation, reclaim solvent, filtrate be concentrated into original volume 1/4 after, concentrated solution is filtered;
(4) get filtrate, concentrate drying, obtains raffinose crude product, raffinose crude product utilizes dehydrated alcohol drip washing, and then joining concentration expressed in percentage by volume in the ratio of solid-liquid ratio 1:11 is in 72% aqueous ethanolic solution, heating for dissolving, 5 ℃ of crystallizations 32 hours, obtain crystal, obtain raffinose finished product after oven dry.
Embodiment 9:
Compared with embodiment 1, the difference of the present embodiment is:
(1) cotton dregs dephenolize preparation: take defatted cotton dregs as raw material, pulverized 110 mesh sieves, remove velveteen and boll hull, the amount of substance is equivalent to the ferrous sulfate of 1.2 times of raw material Free Gossypol amount of substances, the aqueous ethanolic solution that the concentration expressed in percentage by volume that adds weight to be equivalent to weight of material 1/4 is 58%, adds Na
2cO
3adjust pH value to 7.8, stirring and evenly mixing, utilizes bulking machine to carry out extruding puffing detoxification treatment, its bulking process parameter: 135 ℃ of swelling temperatures; 160 revs/min of screw speeds; 5 millimeters of die throat diameters, obtain expanded detoxification cotton dregs;
(2) alkyd solution is extracted: take above-mentioned expanded detoxification cotton dregs as raw material, press solid-liquid ratio 1:15, adding concentration expressed in percentage by volume is 60% alcoholic solution, aqueous acid adjust pH to 5, at 75 ℃ of temperature, lixiviate 25 minutes, extracting solution adopts filter to filter, filtrate being used for extracted raffinose, and filter residue is dried as cottonseed crude protein;
(3) get above-mentioned filtrate, adding and being equivalent to filtrate weight 1% granularity is 35 object decoloration active carbons, 60 ℃ of underpressure distillation, reclaim solvent, filtrate be concentrated into original volume 1/4 after, concentrated solution is filtered;
(4) get filtrate, concentrate drying, obtains raffinose crude product, raffinose crude product utilizes dehydrated alcohol drip washing, and then joining concentration expressed in percentage by volume in the ratio of solid-liquid ratio 1:12 is in 75% aqueous ethanolic solution, heating for dissolving, 8 ℃ of crystallizations 35 hours, obtain crystal, obtain raffinose finished product after oven dry.
Embodiment 10:
Compared with embodiment 1, the difference of the present embodiment is:
(1) cotton dregs dephenolize preparation: take defatted cotton dregs as raw material, pulverized 110 mesh sieves, remove velveteen and boll hull, the amount of substance is equivalent to the ferrous sulfate of 1 times of raw material Free Gossypol amount of substance, the aqueous ethanolic solution that the concentration expressed in percentage by volume that adds weight to be equivalent to weight of material 1/5 is 60%, adds Na
2cO
3adjust pH value to 9, stirring and evenly mixing, utilizes bulking machine to carry out extruding puffing detoxification treatment, its bulking process parameter: 136 ℃ of swelling temperatures; 165 revs/min of screw speeds; 5 millimeters of die throat diameters, obtain expanded detoxification cotton dregs;
(2) alkyd solution is extracted: take above-mentioned expanded detoxification cotton dregs as raw material, press solid-liquid ratio 1:13, adding concentration expressed in percentage by volume is 65% alcoholic solution, aqueous acid adjust pH to 4.5, at 78 ℃ of temperature, lixiviate 28 minutes, extracting solution adopts filter to filter, filtrate being used for extracted raffinose, and filter residue is dried as cottonseed crude protein;
(3) get above-mentioned filtrate, adding and being equivalent to filtrate weight 0.9% granularity is 40 object decoloration active carbons, 65 ℃ of underpressure distillation, reclaim solvent, filtrate be concentrated into original volume 1/5 after, concentrated solution is filtered;
(4) get filtrate, concentrate drying, obtains raffinose crude product, raffinose crude product utilizes dehydrated alcohol drip washing, and then joining concentration expressed in percentage by volume in the ratio of solid-liquid ratio 1:10 is in 78% aqueous ethanolic solution, heating for dissolving, 6 ℃ of crystallizations 38 hours, obtain crystal, obtain raffinose finished product after oven dry.
Embodiment 11:
Compared with embodiment 1, the difference of the present embodiment is:
(1) cotton dregs dephenolize preparation: take defatted cotton dregs as raw material, pulverized 90 mesh sieves, remove velveteen and boll hull, the amount of substance is equivalent to the ferrous sulfate of 1.1 times of raw material Free Gossypol amount of substances, the aqueous ethanolic solution that the concentration expressed in percentage by volume that adds weight to be equivalent to weight of material 0.24 is 58%, adds liming and adjusts pH value to 9, stirring and evenly mixing, utilize bulking machine to carry out extruding puffing detoxification treatment, its bulking process parameter: 140 ℃ of swelling temperatures; 170 revs/min of screw speeds; 5 millimeters of die throat diameters, obtain expanded detoxification cotton dregs;
(2) alkyd solution is extracted: take above-mentioned expanded detoxification cotton dregs as raw material, press solid-liquid ratio 1:15, adding concentration expressed in percentage by volume is 70% alcoholic solution, aqueous acid adjust pH to 4, at 80 ℃ of temperature, lixiviate 30 minutes, extracting solution adopts filter to filter, filtrate being used for extracted raffinose, and filter residue is dried as cottonseed crude protein;
(3) get above-mentioned filtrate, adding and being equivalent to filtrate weight 1% granularity is 30 object decoloration active carbons, 70 ℃ of underpressure distillation, reclaim solvent, filtrate be concentrated into original volume 1/5 after, concentrated solution is filtered;
(4) get filtrate, concentrate drying, obtains raffinose crude product, raffinose crude product utilizes dehydrated alcohol drip washing, and then joining concentration expressed in percentage by volume in the ratio of solid-liquid ratio 1:12 is in 80% aqueous ethanolic solution, heating for dissolving, 10 ℃ of crystallizations 30 hours, obtain crystal, obtain raffinose finished product after oven dry.
Embodiment 12:
Compared with embodiment 1, the difference of the present embodiment is:
(1) cotton dregs dephenolize preparation: take defatted cotton dregs as raw material, pulverized 100 mesh sieves, remove velveteen and boll hull, the amount of substance is equivalent to the ferrous sulfate of 1.2 times of raw material Free Gossypol amount of substances, adding weight is the aqueous ethanolic solution that the concentration expressed in percentage by volume of weight of material 1/4 is 60%, adds ammoniacal liquor and adjusts pH value to 8.5, stirring and evenly mixing, utilize bulking machine to carry out extruding puffing detoxification treatment, its bulking process parameter: 136 ℃ of swelling temperatures; 165 revs/min of screw speeds; 4 millimeters of die throat diameters, obtain expanded detoxification cotton dregs;
(2) alkyd solution is extracted: take above-mentioned expanded detoxification cotton dregs as raw material, press solid-liquid ratio 1:13, adding concentration expressed in percentage by volume is 60% alcoholic solution, aqueous acid adjust pH to 4, at 75 ℃ of temperature, lixiviate 24 minutes, extracting solution adopts diatomite plate and frame filter to filter, filtrate being used for extracted raffinose, and filter residue is dried as cottonseed crude protein;
(3) get above-mentioned filtrate, adding and being equivalent to filtrate weight 1% granularity is 20 object decoloration active carbons, 60 ℃ of underpressure distillation, reclaim solvent, filtrate be concentrated into original volume 1/5 after, concentrated solution is filtered;
(4) get filtrate, concentrate drying, obtains raffinose crude product, raffinose crude product utilizes dehydrated alcohol drip washing, and then joining concentration expressed in percentage by volume in the ratio of solid-liquid ratio 1:10 is in 75% aqueous ethanolic solution, heating for dissolving, 5 ℃ of crystallizations 35 hours, obtain crystal, obtain raffinose finished product after oven dry.
Embodiment 13: compared with embodiment 1, the difference of the present embodiment is: described raffinose crude product utilizes the aqueous ethanolic solution that concentration expressed in percentage by volume that salt is saturated is 75%-80% to replace dehydrated alcohol.
Claims (9)
1. a cotton dregs dephenolize technology, is characterized in that mainly comprising following processing step:
Take defatted cotton dregs as raw material, pulverized 90～110 mesh sieves, remove velveteen and boll hull, the amount of substance is equivalent to the ferrous sulfate of 1～1.2 times of raw material Free Gossypol amount of substance, the aqueous ethanolic solution that the concentration expressed in percentage by volume that adds weight to be equivalent to weight of material 1/5～1/4 is 50%～60%, adds Na
2cO
3adjust material pH value to 7～9, stirring and evenly mixing, utilizes bulking machine to carry out extruding puffing detoxification treatment, its bulking process parameter: 135～140 ℃ of swelling temperatures, 150～170 revs/min of screw speeds, 3～5 millimeters of die throat diameters; Obtain expanded detoxification cotton dregs.
2. cotton dregs dephenolize technology as claimed in claim 1, is characterized in that described Na
2cO
3can use NaOH, ammoniacal liquor, liming one wherein to replace.
3. utilize the cotton dregs dephenolize technology described in claim 1 from cotton dregs, to prepare a method for raffinose, it is characterized in that mainly realizing by following processing step:
(1) dephenolize cotton dregs preparation: take defatted cotton dregs as raw material, pulverized 90～110 mesh sieves, remove velveteen and boll hull, the amount of substance is equivalent to the ferrous sulfate of 1～1.2 times of raw material Free Gossypol amount of substance, the aqueous ethanolic solution that the concentration expressed in percentage by volume that adds weight to be equivalent to weight of material 1/5～1/4 is 50%～60%, adds Na
2cO
3adjust material pH value to 7～9, stirring and evenly mixing, utilizes bulking machine to carry out extruding puffing detoxification treatment, its bulking process parameter: 135～140 ℃ of swelling temperatures; 150～170 revs/min of screw speeds; 3～5 millimeters of die throat diameters, obtain expanded detoxification cotton dregs;
(2) alkyd solution is extracted: take above-mentioned expanded detoxification cotton dregs as raw material, press solid-liquid ratio 1:10～1:15, adding concentration expressed in percentage by volume is 50%～70% alcoholic solution, aqueous acid adjust pH to 4～5, at 70～80 ℃ of temperature, lixiviate 15～30 minutes, extracting solution adopts filter to filter, filtrate being used for extracted raffinose, and filter residue is dried as cottonseed crude protein;
(3) get above-mentioned filtrate, adding and being equivalent to filtrate weight 0.8%～1% granularity is 10～40 object decoloration active carbons, 50～70 ℃ of underpressure distillation, reclaim solvent, filtrate be concentrated into original volume 1/5～1/4 after, concentrated solution is filtered;
(4) get filtrate, concentrate drying, obtain raffinose crude product, raffinose crude product utilizes dehydrated alcohol drip washing, then joining concentration expressed in percentage by volume in the ratio of solid-liquid ratio 1:10～1:12 is in 70%～80% aqueous ethanolic solution, heating for dissolving, crystallization 30～40 hours at 0～10 ℃, obtain crystal, after oven dry, obtain raffinose finished product.
4. the method for utilizing cotton dregs dephenolize technology to prepare raffinose from cotton dregs as claimed in claim 3, is characterized in that it is 75%-80% aqueous ethanolic solution replacement dehydrated alcohol that described raffinose crude product can utilize the concentration expressed in percentage by volume that salt is saturated.
5. the cotton dregs dephenolize technology of utilizing as described in claim 3 or 4 is prepared the method for raffinose from cotton dregs, it is characterized in that the alcoholic solution in described alkyd solution is the one in methyl alcohol or ethanol, and aqueous acid is wherein the one in hydrochloric acid or sulfuric acid.
6. the cotton dregs dephenolize technology of utilizing as described in claim 3 or 4 is prepared the method for raffinose from cotton dregs, it is characterized in that described filter is diatomite plate and frame filter.
7. the method for utilizing cotton dregs dephenolize technology to prepare raffinose from cotton dregs as claimed in claim 5, is characterized in that described filter is diatomite plate and frame filter.
8. the cotton dregs dephenolize technology of utilizing as described in claim 3 or 4 is prepared the method for raffinose from cotton dregs, it is characterized in that described Na
2cO
3can use NaOH, ammoniacal liquor, liming one wherein to replace.
9. the method for utilizing cotton dregs dephenolize technology to prepare raffinose from cotton dregs as claimed in claim 7, is characterized in that described Na
2cO
3can use NaOH, ammoniacal liquor, liming one wherein to replace.
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| CN104489259A (en) * | 2014-12-31 | 2015-04-08 | 石勇 | Method for preparing feed by cotton stalks |
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Cited By (2)
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| CN104489259A (en) * | 2014-12-31 | 2015-04-08 | 石勇 | Method for preparing feed by cotton stalks |
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