CN105559095A - Method for preparing and separating plant fiber and lignin from rose flower residues - Google Patents
Method for preparing and separating plant fiber and lignin from rose flower residues Download PDFInfo
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- CN105559095A CN105559095A CN201510899301.7A CN201510899301A CN105559095A CN 105559095 A CN105559095 A CN 105559095A CN 201510899301 A CN201510899301 A CN 201510899301A CN 105559095 A CN105559095 A CN 105559095A
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- lignin
- rose
- slag
- plant fiber
- rose slag
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- 241000220317 Rosa Species 0.000 title claims abstract description 62
- 229920005610 lignin Polymers 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000000835 fiber Substances 0.000 title claims abstract description 20
- 241000196324 Embryophyta Species 0.000 title claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000001035 drying Methods 0.000 claims abstract description 16
- 239000000706 filtrate Substances 0.000 claims abstract description 12
- 238000000605 extraction Methods 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 230000008569 process Effects 0.000 claims abstract description 6
- 239000000341 volatile oil Substances 0.000 claims abstract description 6
- 239000002699 waste material Substances 0.000 claims abstract description 6
- 238000010992 reflux Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract 4
- 239000002893 slag Substances 0.000 claims description 49
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 21
- 239000002904 solvent Substances 0.000 claims description 16
- 239000000284 extract Substances 0.000 claims description 15
- 239000003054 catalyst Substances 0.000 claims description 11
- 229920002678 cellulose Polymers 0.000 claims description 11
- 239000001913 cellulose Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 10
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 8
- 230000006837 decompression Effects 0.000 claims description 8
- 238000004821 distillation Methods 0.000 claims description 8
- 239000008213 purified water Substances 0.000 claims description 8
- 230000035484 reaction time Effects 0.000 claims description 6
- 238000011084 recovery Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 230000001476 alcoholic effect Effects 0.000 claims description 4
- 238000010298 pulverizing process Methods 0.000 claims description 4
- 238000004064 recycling Methods 0.000 claims description 4
- 235000011449 Rosa Nutrition 0.000 claims description 2
- 238000010411 cooking Methods 0.000 claims 1
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical class CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 claims 1
- 238000009835 boiling Methods 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 241000109329 Rosa xanthina Species 0.000 abstract 1
- 235000004789 Rosa xanthina Nutrition 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 6
- 230000003064 anti-oxidating effect Effects 0.000 description 5
- 235000013325 dietary fiber Nutrition 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000000926 separation method Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 229920002488 Hemicellulose Polymers 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 206010028980 Neoplasm Diseases 0.000 description 1
- 241000220222 Rosaceae Species 0.000 description 1
- 241000592342 Tracheophyta Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- AEMOLEFTQBMNLQ-BKBMJHBISA-N alpha-D-galacturonic acid Chemical compound O[C@H]1O[C@H](C(O)=O)[C@H](O)[C@H](O)[C@H]1O AEMOLEFTQBMNLQ-BKBMJHBISA-N 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 235000018927 edible plant Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 229930003944 flavone Natural products 0.000 description 1
- 150000002213 flavones Chemical class 0.000 description 1
- 235000011949 flavones Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 210000001035 gastrointestinal tract Anatomy 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 235000006486 human diet Nutrition 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000002608 ionic liquid Substances 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000005445 natural material Substances 0.000 description 1
- 231100000957 no side effect Toxicity 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
- D21C5/00—Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Abstract
The invention discloses a method for preparing and separating plant fiber and lignin from waste flower residues generated in a process of producing rose essential oil. The method comprises the following specific steps: smashing rose waste residues serving as a raw material left after extraction of essential oil, and performing ethanol-reflux extraction; catalyzing reaction of the refluxed rose residues in a high-boiling alcohol solution at a high temperature; filtering to obtain filter residues, and performing washing, drying and smashing to obtain the plant fiber; recovering the high-boiling alcohol solution from the filtrate, washing and drying to obtain the lignin. According to the method, the plant fiber and the lignin are obtained separately from the rose residues, so that the comprehensive utilization value of roses is increased. The method is easy to operate, is low in production cost, and is environmentally friendly.
Description
Technical field
The present invention relates to a kind of method of preparation and separating plant fiber and lignin in useless colored slag produced from production rose ethereal oil process.
Background technology
Rose (Roserugosa) is rose family chamiso, has soft liver and to wake up stomach, and thin gas such as to be invigorated blood circulation at the effect.In current document, the research of rose is mainly concentrated on to the research of the aspects such as extraction of essential oil, aromatic substance, Rose Pigment and polyphenoils, rose slag rich in nutrition content, containing polysaccharide, flavones, cellulose, protein, multivitamin, carrotene and mineral nutrient element, it is a kind of natural material being worth developing further.Rose slag is the rose residue produced after extracting Rosa Damascana.At present, both at home and abroad the accessory substances such as the colored slag after extraction essential oil are used as just feed, rose slag is not goed deep into the relevant report of integrated application, only have document to conduct a preliminary study comprehensive exploitation.
String is a kind of material that can not be digested, and it comprises cellulose, hemicellulose, lignin, pectic substance, gumminess and some non-cellulose sugar.Dietary fiber is the edible strings of the mankind.Rose is as a kind of medicinal and edible plant, and the string prepared as raw material with it is a kind of excellent dietary fiber.
Lignin is the natural high molecular substance with phenolic structure, extensively be present in xylophyta, herbaceous plant, vascular plant, being that occurring in nature is quantitatively only second to cellulosic second largest natural macromolecular material, is industrial unique aromatic compound that can obtain from renewable resource.Lignin is all widely used in building materials industry, petroleum industry, light industry, agricultural.Lignin is also the important component part in human diet fiber (Dietaryfibres, DF), can change the activity of microorganism in intestinal tract, reduce the content of Blood Cholesterol and blood sugar, have the effect of angiocardiopathy preventing; Lignin also has the function such as antioxidation activity, inhibition cancer cell activity.As natural anti-oxidation active substance, people conduct extensive research the anti-oxidizing activities of lignin in timber and agricultural crop straw, and also rare to the research of lignin in the dietary fibers such as veterinary antibiotics.From rose slag, extract lignin and its structure and antioxidation activity are studied, being expected to obtain a kind of natural, anti-oxidation active substance of having no side effect, being with a wide range of applications in food industry, cosmetic, health products etc.The extraction separation method of lignin generally has acid, alkali, overcritical, the means such as aqueous two-phase, ionic liquid, organic solvent, and wherein organic solvent method becomes extraction separation method most popular in recent years because of its environmental protection, economy, the feature such as easily separated.But it needs the condition of HTHP mostly, industrialization remains many technical difficulties completely at present, makes it apply and is very limited.
The technological principle that high boiling solvent method prepares lignin is that height boils alcohol solution at appropriate catalyst and under the condition of heating, allows the cellulose in plant material be separated with HBS lignin liquor.Adding suitable water just makes HBS lignin deposit separate out.Centrifugation, is filtered dry after being washed by filter cake warm water, then freeze drying, obtains Powdered brown HBS lignin.Filtrate sloughs moisture under decompression distillation condition, is concentrated to containing alcohol about 80%, can again recycles.1, the boiling points such as 4-butanediol are higher, so volatility is very low, compared with lower boiling ethanol, acetone, when producing, evaporation loss is less, whole process does not have exhaust emission material, and the height after using boils after alcoholic solution can slough moisture by decompression distillation and reuses, and the boil recovery utilization rate of alcohol of height reaches more than 98%.The boiling point of ethylene glycol is 190 DEG C, and the solvent that also can be used as high boiling solvent method uses.
Rose slag is a large amount of solid slags produced in the process of preparing rose flower, and main component comprises cellulose, hemicellulose and lignin.According to the yearly productive capacity of Chinese Enterprises, there are nearly 10-30 ten thousand tons of rose waste sludge discharges every year.Therefore these rose waste residues of Appropriate application, not only protect environment, and turn waste into wealth, and create great economic benefit.
Summary of the invention
The object of the present invention is to provide a kind of method utilizing string and lignin in the high alcohol separation rose slag that boils.
The invention solves the problem of a large amount of useless flower slag wasting of resources produced in rose production process, be separated simultaneously and prepared string and lignin.Solvent used in the present invention is high boiling solvent, and the problem effectively solving solvent volatilization and recycle, leaching process has stopped the generation of waste water,waste gas and industrial residue.Be separated the string obtained and can be used as dietary fibre materials; Lignin purity is high, quality better, can be used for the lignin derivative product obtaining high added value further.
A method for preparation and separating plant fiber and lignin from rose slag, is characterized in that this technique is made up of following steps:
(1) rose slag is crushed to 20-120 order, obtains rose ground-slag, for subsequent use.In the present invention, preferably rose slag is crushed to 100 orders;
(2) get the rose ground-slag of pulverizing, add 60%-95% ethanol, make solid-liquid ratio reach 1:10-20.Heating and refluxing extraction 2 times, each 2 hours, filter, filter residue is dried; Filtrate recycling ethanol.In this law, preferred solid-liquid ratio is 1:15;
(3) rose slag of drying in (2) is placed in the autoclave with temperature control and paddle, adds catalyst, add height and boil alcohol solution as solvent; Rose slag and catalyst quality are than being 100:2-5; The height alcohol that boils is 60%-85%; Rose slag quality (g) is 1:5-1:15 with volume (ml) proportioning of the high alcohol solution that boils; Reaction temperature is 160-230 DEG C, reaction time 1-3 hour.In the present invention, the height preferably the added alcohol that boils is BDO, and concentration is 65%; Rose slag quality (g) is 1:10 with volume (ml) proportioning of the high alcohol solution that boils; Reaction temperature is 190 DEG C, 1.5 hours reaction time;
(4) react complete, filter under normal temperature, the purified water obtaining 20-50 DEG C of cellulose 10-15 times amount is washed 2-3 time, filters, obtains fiber after drying;
(5) filtrate is through decompression distillation, reclaims the high alcoholic solution that boils, and recycles during in order to again extracting; The medicinal extract obtained, through vacuum microwave drying, obtains lignin dry medicinal extract;
(6) dry extract obtained after the high alcohol that boils of recovery in (5) is pulverized, cross 80-120 mesh sieve; Wash 2 times by the purified water of 20-50 DEG C of 10-15 times amount, after drying, obtain lignin.
Beneficial effect of the present invention is as follows:
The invention solves because low boiling point solvent volatilizees the rising of the environmental pollution that causes and cost, the solvent used is high boiling solvent and water, the problem effectively solving solvent volatilization and recycle;
This invention also solves the problem of the rose slag wasting of resources, in rose slag, the recovery rate of string and lignin is at 60%-75%;
The method extracting fiber and lignin from rose slag of the present invention, can extract string and lignin with the high alcoholic solution that boils of one simultaneously.Improve the comprehensive utilization value of rose, widen the purposes of rose.Method of operating of the present invention is simple, and producing cost is low; And non-environmental-pollution.
Detailed description of the invention
Below in conjunction with specific embodiment, the specific embodiment of the present invention is described, but the present invention is not limited only to these embodiments, under the prerequisite not departing from present inventive concept, any improvement done all drops within protection scope of the present invention.
Embodiment 1:
(1) rose slag is crushed to 80 orders, obtains rose ground-slag, for subsequent use;
(2) get the rose ground-slag 100g of pulverizing, add 75% ethanol, 500ml makes solid-liquid ratio reach 1:5.Heating and refluxing extraction 2 times, each 2 hours, filter, filter residue is dried; Filtrate recycling ethanol;
(3) rose slag of drying in (2) is placed in the autoclave with temperature control and paddle, adds 3gMg(NO
3) 26H
2o is as catalyst, and adding concentration is that 1200ml65%1,4-butanediol is as solvent.Stir, reaction temperature is 190 DEG C, 2 hours reaction time;
(4) react complete, filter under normal temperature, the purified water obtaining 30 DEG C of cellulose 10-15 times amount washs 3 times, filters, obtains fiber 26.7g after drying;
(5) filtrate is through decompression distillation, reclaims BDO solution, recycles during in order to again extracting; The medicinal extract obtained, through vacuum microwave drying, obtains lignin dry medicinal extract;
(6) dry extract obtained after recovery BDO in (5) is pulverized, cross 80 mesh sieves; Wash 2 times by the purified water of 20-30 DEG C of 10 times amount, after dry, obtain lignin 15g.3; Containing the filtrate of BDO through decompression distillation, after sloughing moisture, BDO solvent can recycle.
Embodiment 2
(1) rose slag is crushed to 100 orders, obtains rose ground-slag, for subsequent use;
(2) get the rose ground-slag 100g of pulverizing, add 85% ethanol, 500ml makes solid-liquid ratio reach 1:5.Ultrasonic wave extracts 2 times, each 45 minutes, filters, and filter residue is dried; Filtrate recycling ethanol;
(3) rose slag of drying in (2) is placed in the autoclave with temperature control and paddle, adds 2gMgCl6H
2o is as catalyst, and adding concentration is that 1000ml70% ethylene glycol is as solvent.Stir, reaction temperature is 180 DEG C, 2 hours reaction time;
(4) react complete, filter under normal temperature, the purified water obtaining 30 DEG C of cellulose 10-15 times amount washs 3 times, filters, obtains fiber 27.1g after drying;
(5) filtrate is through decompression distillation, reclaims ethylene glycol solution, recycles during in order to again extracting; The medicinal extract obtained, through vacuum microwave drying, obtains lignin dry medicinal extract;
(6) dry extract obtained after recovery 1 ethylene glycol in (5) is pulverized, cross 80 mesh sieves; Wash 2 times by the purified water of 20-30 DEG C of 10 times amount, after dry, obtain lignin 13.3g; Containing the filtrate of ethylene glycol through decompression distillation, after sloughing moisture, ethylene glycol solvent can recycle.
Claims (7)
1.
oneplant the method for preparation and separating plant fiber and lignin from rose slag, it is characterized in that this technique is made up of following steps:
(1) rose slag is crushed to 20-120 order, obtains rose ground-slag, for subsequent use;
(2) get the rose ground-slag of pulverizing, add 60%-95% ethanol, make solid-liquid ratio reach 1:10-20; Heating and refluxing extraction 2 times, each 2 hours, filter, filter residue is dried; Filtrate recycling ethanol;
(3) rose slag of drying in (2) is placed in the autoclave with temperature control and paddle, adds catalyst, add height and boil alcohol solution as solvent; Rose slag and catalyst quality are than being 100:2-5; The height alcohol that boils is 60%-85%; Rose slag quality (g) is 1:5-1:15 with volume (ml) proportioning of the high alcohol solution that boils; Reaction temperature is 160-230 DEG C, reaction time 1-3 hour;
(4) react complete, filter, the purified water obtaining 20-50 DEG C of cellulose 10-15 times amount is washed 2-3 time, filters, obtains fiber after drying;
(5) filtrate is through decompression distillation, reclaims the high alcoholic solution that boils, and recycles during in order to again extracting; The medicinal extract obtained, through vacuum microwave drying, obtains lignin dry medicinal extract;
(6) dry extract obtained after the high alcohol that boils of recovery in (5) is pulverized, cross 80-120 mesh sieve; Wash 2 times by the purified water of 20-50 DEG C of 10-15 times amount, after drying, obtain lignin.
2. according to claim 1 a kind of from rose slag preparation and the method for separating plant fiber and lignin, described rose slag is the waste residue produced after extracting Rosa Damascana by hydrodistillation or decocting cooking method.
3. according to claim 1 a kind of from rose slag preparation and the method for separating plant fiber and lignin, it is characterized in that: the rose slag described in step (1) is produce the useless colored slag produced in rose ethereal oil process.
4. according to claim 1 a kind of from rose slag preparation and the method for separating plant fiber and lignin, it is characterized in that: in step (2), heating reflux temperature is 80-100 DEG C.
5. according to claim 1 a kind of from rose slag preparation and the method for separating plant fiber and lignin, it is characterized in that: described in step (3), catalyst is Mg(NO
3) 26H
2o or MgCl6H
2one or both arbitrary scalemic thereof in O; The described height alcohol that boils is the one of BDO, ethylene glycol and propane diols; Rose slag and catalyst quality are than being 100:2-5; The height alcohol that boils is 60%-85%; Rose slag quality (g) is 1:5-1:15 with volume (ml) proportioning of the high alcohol solution that boils; Reaction temperature is 160-230 DEG C, reaction time 1-3 hour.
6. according to claim 1 a kind of from rose slag preparation and the method for separating plant fiber and lignin, it is characterized in that: the washing described in step (4) to be boiled alcohol and catalyst to remove the height remained in cellulose, obtains purer cellulose.
7. according to claim 1 a kind of from rose slag preparation and the method for separating plant fiber and lignin, it is characterized in that: the washing described in step (6) is to remove the catalyst remained in lignin, obtains purer lignin.
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CN1424459A (en) * | 2002-12-17 | 2003-06-18 | 闽江学院 | Preparation of cellulose and lignin by high boiling alcohol solvent |
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2015
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