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 PDF

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Publication number
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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China
Prior art keywords
lignin
rose
slag
plant fiber
rose slag
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Pending
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CN201510899301.7A
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Chinese (zh)
Inventor
代友彪
来海中
刘盼盼
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Huan Tuo Bio Tech Ltd Xinjiang
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Huan Tuo Bio Tech Ltd Xinjiang
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Priority to CN201510899301.7A priority Critical patent/CN105559095A/en
Publication of CN105559095A publication Critical patent/CN105559095A/en
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    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21CPRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C5/00Other processes for obtaining cellulose, e.g. cooking cotton linters ; Processes characterised by the choice of cellulose-containing starting materials
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food 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

A kind of method of preparation and separating plant fiber and lignin from rose slag
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.
CN201510899301.7A 2015-12-09 2015-12-09 Method for preparing and separating plant fiber and lignin from rose flower residues Pending CN105559095A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1424459A (en) * 2002-12-17 2003-06-18 闽江学院 Preparation of cellulose and lignin by high boiling alcohol solvent
CN101372815A (en) * 2008-09-24 2009-02-25 天津科技大学 Method for separating lignose and cellulose in licorice waste slag by means of ultrasonic technology
CN102276847A (en) * 2011-07-29 2011-12-14 长春工业大学 Method for separating nut shell lignin by utilizing high-boiling alcohol
CN102895152A (en) * 2012-10-29 2013-01-30 广州栋方日化有限公司 Preparation method for rose extract and cosmetic
CN103711017A (en) * 2014-01-06 2014-04-09 海宁朗赛纤维科技有限公司 Normal pressure ultrasonic-assisted method for preparing cellulose and lignin by using high boiling alcohol as solvent
CN104292471A (en) * 2014-10-27 2015-01-21 镇江拜因诺生物科技有限公司 Method for preparing protolignin by using corn cob residues
CN104906007A (en) * 2015-06-24 2015-09-16 陈琳仁 Method for extracting rose essential oil, pigment and flavone from roses simultaneously and application of extracts

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1424459A (en) * 2002-12-17 2003-06-18 闽江学院 Preparation of cellulose and lignin by high boiling alcohol solvent
CN101372815A (en) * 2008-09-24 2009-02-25 天津科技大学 Method for separating lignose and cellulose in licorice waste slag by means of ultrasonic technology
CN102276847A (en) * 2011-07-29 2011-12-14 长春工业大学 Method for separating nut shell lignin by utilizing high-boiling alcohol
CN102895152A (en) * 2012-10-29 2013-01-30 广州栋方日化有限公司 Preparation method for rose extract and cosmetic
CN103711017A (en) * 2014-01-06 2014-04-09 海宁朗赛纤维科技有限公司 Normal pressure ultrasonic-assisted method for preparing cellulose and lignin by using high boiling alcohol as solvent
CN104292471A (en) * 2014-10-27 2015-01-21 镇江拜因诺生物科技有限公司 Method for preparing protolignin by using corn cob residues
CN104906007A (en) * 2015-06-24 2015-09-16 陈琳仁 Method for extracting rose essential oil, pigment and flavone from roses simultaneously and application of extracts

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* Cited by examiner, † Cited by third party
Title
吴瑛 等: "和田玫瑰残渣纤维素及蛋白质含量分析", 《江苏农业科学》 *

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