CN109337408A - A kind of extracting method and its application of roselle natural dye - Google Patents

A kind of extracting method and its application of roselle natural dye Download PDF

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Publication number
CN109337408A
CN109337408A CN201811441374.1A CN201811441374A CN109337408A CN 109337408 A CN109337408 A CN 109337408A CN 201811441374 A CN201811441374 A CN 201811441374A CN 109337408 A CN109337408 A CN 109337408A
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China
Prior art keywords
roselle
natural dye
dyestuff
extracting method
extraction
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CN201811441374.1A
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Chinese (zh)
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CN109337408B (en
Inventor
马小强
潘婷
李岳
黄洪万
万权汗
陈莹
洪润
陈紫蓉
吴帆
张健
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Wuhan Polytechnic University
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Wuhan Polytechnic University
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B61/00Dyes of natural origin prepared from natural sources, e.g. vegetable sources
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
    • C09B67/0096Purification; Precipitation; Filtration
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/34General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using natural dyestuffs
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P3/00Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
    • D06P3/02Material containing basic nitrogen
    • D06P3/04Material containing basic nitrogen containing amide groups
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P3/00Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
    • D06P3/02Material containing basic nitrogen
    • D06P3/04Material containing basic nitrogen containing amide groups
    • D06P3/14Wool

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Coloring (AREA)

Abstract

The invention discloses the extracting methods and its application of a kind of roselle natural dye, it is extracted by raw material preparation, dyestuff and dyestuff purifies three steps and roselle natural dye can be obtained, extraction process is simple, extraction efficiency is high, it is at low cost, extract safety and have sterilization and other effects, it is good with ecological environment compatibility, it is biodegradable;On the fabric, dyefastness is high for the roselle application of extraction, and dyeing effect is good.

Description

A kind of extracting method and its application of roselle natural dye
Technical field
The invention belongs to dyestuff manufacture technology fields, and in particular to a kind of extracting method of roselle natural dye and its answer With.
Background technique
Natural dye has drawn from plant, animal, mineral in nature etc., helps in dyeing course without adding a large amount of chemistry Agent, and waste water will not be generated;The sediment for extracting dyestuff can be used as paper making raw material or fertilizer utilization, not generate pollution, real Existing " zero-emission ".In dyeing course, drug ingedient can be absorbed together with pigment by fabric, and the fabric after making dyeing is to human body There are special medicinal health-care function, such as relaxing tendons and activating collaterals, sterilization, faint scent, uvioresistant.
Roselle is root, the seed of malvaceae plant roselle.Alias roselle, very popular actor or actress certain herbaceous plants with big flowers, red sorrel etc..Roselle tool There are the clearing heat and detoxicating, Li Shui that promotes the production of body fluid, prevention and cure of cardiovascular disease and other effects.
Summary of the invention
In view of this, the embodiment provides the extracting methods and its application of a kind of roselle natural dye.
The embodiment of the present invention the technical solution adopted is that, a kind of extracting method of roselle natural dye, a kind of rose The extracting method of eggplant natural dye, comprising the following steps:
(1) feedstock processing;Roselle is taken to clean heat baking grind into powder after natural drying spare;
(2) dyestuff is extracted;It is appropriate to weigh above-mentioned dusty raw materials, sequentially adds deionized water, cellulase thereto, adopts With ultrasonic extraction, the filtrate of roselle natural dye must be contained by extracting supernatant liquid filtering;
(3) purifying dyestuff;Above-mentioned filtrate is adjusted as acidity, is filtered after standing, filtered liquid is dry until obtaining rose Rare nightshade pigment.
Preferably, in the step (1), grind into powder crosses 180~210 mesh mesh screens and obtains powder after roselle clean dry Last shape raw material for standby.
The embodiment of the invention also provides a kind of Roselle flower pigments of the extracting method of roselle natural dye extraction Using the Roselle flower pigment of extraction is applied in textile dyeing.
Preferably, it takes the Roselle flower pigment to be added in deionized water to dilute, and adjusts pH value and obtain dye liquor, will pass through The fabric of pre-treatment, which immerses in the dye liquor, to be dyed, and is washed and is dried after dyeing, obtains dyed fabric.
The technical solution that the embodiment of the present invention provides has the benefit that roselle natural dye of the invention Extracting method, extraction process is simple, and extraction efficiency is high, at low cost, and extract is safe and with sterilization and other effects, with ecological ring Border compatibility is good, biodegradable;The pigment of extraction, which is used as dyestuff, to be dyed on the fabric well.
Detailed description of the invention
Fig. 1 is the infrared spectrum for the Roselle flower pigment that the method for the embodiment of the present invention is extracted.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with attached drawing to embodiment party of the present invention Formula is further described.
Embodiment one
The embodiment provides a kind of extracting methods of roselle natural dye, comprising the following steps:
(1) feedstock processing;Roselle is taken to clean heat baking grind into powder after natural drying spare;
Specifically, ground 180~210 mesh mesh screen obtains dusty raw materials after roselle clean dry;
(2) dyestuff is extracted;It is appropriate to weigh above-mentioned dusty raw materials, deionized water, cellulase are added thereto, using 65 DEG C~75 DEG C of ultrasonic extraction 50min~70min, the filtrate of roselle natural dye must be contained by extracting supernatant liquid filtering;Wherein, supernatant The filtered residue of liquid repeats ultrasonic extraction, extracts supernatant liquid filtering, and merges obtained filtrate;Ultrasonic extraction is repeated several times can Guarantee that the dyestuff in raw material is all extracted, improves the recovery rate of dyestuff;
(3) purifying dyestuff;Above-mentioned filtrate is adjusted as acidity, is filtered after standing, filtered liquid is dry until obtaining rose Rare nightshade pigment.
Referring to attached drawing 1, the structure and group and its characteristic absorption contained in roselle calyx red pigment molecule has: 3392cm-1For Phenolic hydroxyl group (O-H) stretching vibration peak, 29327cm-1For hydrocarbon (C-H) stretching vibration, 1366cm-1It shakes for the angle of hydrocarbon (C-H) It is dynamic, show to contain glucosides in the roselle calyx red pigment of extraction of the embodiment of the present invention;1080cm-1For ehter bond in saccharide ring (C-O-C) Asymmetry vibration is sucked, 605-670cm-1There are the characteristic absorption peak of glucose, 1638cm in place-1For phenyl ring skeletal vibration, 707cm-1 It is vibrated for the fold of phenyl ring;Show there is the flexible vibration of obvious-OH, phenyl ring, C-H and C-O-C in structural formula by infrared characteristic peak Dynamic and phenyl ring fold vibration, show roselle calyx red pigment that the embodiment of the present invention is extracted be corn flower-glucose glycoside or Person delphinium-glucose glycoside pigment.
The embodiment of the invention also provides a kind of answering for the roselle dyestuff of the extracting method of roselle natural dye extraction With the Roselle flower pigment of extraction is applied in textile dyeing.Roselle is root, the seed of malvaceae plant roselle;Alias Roselle, very popular actor or actress certain herbaceous plants with big flowers, red sorrel etc.;With the clearing heat and detoxicating, Li Shui that promotes the production of body fluid, prevention and cure of cardiovascular disease and other effects.
Further, the Roselle flower pigment of extraction is applied to silk, wool fabric dyeing.
Further, the Roselle flower pigment of extraction is added in deionized water and dilutes, and adjusts pH value and obtains dye liquor, will be through The fabric for crossing pre-treatment, which immerses in the dye liquor, to be dyed, and is washed and is dried after dyeing, obtains dyed fabric.
Further, the pH value of the dye liquor is 3~7, and mass concentration is 5~30g/L;To the dyeing condition of fabric Are as follows: bath raio 1:20~30,5~15g/L of mordant dosage, 90~95 DEG C of dyeing temperature, dyeing time are 60~90min.It is added The dyefastness of the dyestuff of extraction of the embodiment of the present invention can be improved in mordant;The mordant using aluminum aluminum sulfate, magnesium chloride or Calcium chloride;Electrolyte is added in dyeing course.
Embodiment two
According to embodiments of the present invention one method extracts roselle natural dye, comprising the following steps:
(1) feedstock processing;Ground 200 mesh mesh screen after roselle clean dry is taken to obtain dusty raw materials;
(2) dyestuff is extracted;Above-mentioned dusty raw materials 5g is weighed, sequentially adds 200mL deionized water, cellulase thereto 0.08g, using ultrasound in 70 DEG C of extraction 60min, the filtrate of roselle natural dye must be contained by extracting supernatant liquid filtering, filtered Residue repeats ultrasonic extraction and then extracts supernatant liquid filtering, repeats extraction filtering three times, the filtrate merged;
(3) purifying dyestuff;Above-mentioned filtrate is adjusted as acidity, 3~6h is stood at room temperature and filters, filtered liquid is dry straight To obtaining roselle dyestuff.Wherein, filtered solid residue is drug residue, can be used for other purposes.
Using the embodiment of the present invention extract Roselle flower pigment be applied to textile dyeing on, be particularly applicable to silk, Wool fabric dyeing.
Further, the Roselle flower pigment of extraction is added in deionized water and dilutes, and adjusts pH value and obtains dye liquor, will be through The fabric for crossing pre-treatment, which immerses in the dye liquor, to be dyed, and is washed and is dried after dyeing, obtains dyed fabric.Remaining is same Embodiment one.
Embodiment three
The Roselle flower pigment that the method for the reference embodiment of the present invention two is extracted is in 95 DEG C of temperature, time 90min, electrolyte Fabric is dyed by different bath raioes under conditions of 8g/L, pH value 7, its color feature value of the Fabric Detection after dyeing (L Value, a value, b value) and K/S value, it is shown in Table 1.
Fabric L value, a value, b value and the K/S value dyed under the different bath raioes of table 1
Textile dyeing fastness is maximum under conditions of bath raio 1:10.
In the absence of conflict, the feature in embodiment and embodiment herein-above set forth can be combined with each other.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.

Claims (8)

1. a kind of extracting method of roselle natural dye, characterized in that the following steps are included:
(1) feedstock processing;Roselle is taken to clean heat baking grind into powder after natural drying spare;
(2) dyestuff is extracted;It is appropriate to weigh above-mentioned dusty raw materials, sequentially adds deionized water, cellulase thereto, using adding Hot ultrasonic extraction, the filtrate of roselle natural dye must be contained by extracting supernatant liquid filtering;
(3) purifying dyestuff;Above-mentioned filtrate is adjusted as acidity, is filtered after standing, filtered liquid is dry until obtaining roselle Anthocyanidin.
2. a kind of extracting method of roselle natural dye according to claim 1, characterized in that in the step (1), Ground 180~210 mesh mesh screen obtains dusty raw materials after roselle clean dry.
3. a kind of extracting method of roselle natural dye according to claim 1, characterized in that in the step (2), Ultrasonic extraction 50min~70min under 65 DEG C~75 DEG C heating conditions;Residue after supernatant liquid filtering repeats ultrasonic extraction, extracts Supernatant liquid filtering, and merge obtained filtrate.
4. a kind of extracting method of roselle natural dye according to claim 1, characterized in that the following steps are included:
(1) feedstock processing;Ground 200 mesh mesh screen after roselle clean dry is taken to obtain dusty raw materials;
(2) dyestuff is extracted;Above-mentioned dusty raw materials 5g is weighed, sequentially adds 200mL deionized water, cellulase thereto 0.08g, 70 DEG C of ultrasonic extraction 60min, the filtrate of roselle natural dye, filtered residue weight must be contained by extracting supernatant liquid filtering Then supernatant liquid filtering is extracted in multiple ultrasonic extraction, repeat extraction filtering three times, the filtrate merged;
(3) purifying dyestuff;Above-mentioned filtrate is adjusted to be acid, 3~6h is stood at room temperature and filters, filtered liquid is dry until obtaining To Roselle flower pigment.
5. the roselle dye that a kind of extracting method of roselle natural dye according to any one of claims 1 to 4 is extracted The application of material, characterized in that the Roselle flower pigment of extraction is applied in textile dyeing.
6. the application for the roselle dyestuff that a kind of extracting method of roselle natural dye according to claim 5 is extracted, It is characterized in that the Roselle flower pigment of extraction is used for silk, wool fabric dyeing.
7. the application for the roselle dyestuff that a kind of extracting method of roselle natural dye according to claim 5 is extracted, It is diluted it is characterized in that the Roselle flower pigment of extraction is added in deionized water, and adjusts pH value and obtain dye liquor, pre-treatment will be passed through Fabric immerse in the dye liquor and dyed, wash and dry after dyeing, obtain dyed fabric.
8. the application for the roselle dyestuff that a kind of extracting method of roselle natural dye according to claim 7 is extracted, It is characterized in that the pH value of the dye liquor is 3~7, mass concentration is 15~30g/L;To the dyeing condition of fabric are as follows: bath raio 1:20~30,5~15g/L of mordant dosage, 90~95 DEG C of dyeing temperature, dyeing time are 60~90min.
CN201811441374.1A 2018-11-29 2018-11-29 Extraction method and application of roselle natural dye Active CN109337408B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112111172A (en) * 2020-09-14 2020-12-22 苏州森创纺织科技有限公司 Extraction method of anti-bacterial plant dye combining cellulose mildew and ultrasonic waves
CN114388273A (en) * 2022-01-07 2022-04-22 青海大学 Preparation method and application of anthocyanin-sensitized P5FIN/ITO nano composite material

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CN102433018A (en) * 2011-11-17 2012-05-02 安徽杜鹃花生物科技有限公司 Method for extracting azalea pigment
CN103665924A (en) * 2013-11-19 2014-03-26 婺源县聚芳永茶业有限公司 Extraction method of roselle red color
CN108558971A (en) * 2018-05-31 2018-09-21 福州大学 A kind of preparation method of roselle anthocyanin

Patent Citations (4)

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CN103665924A (en) * 2013-11-19 2014-03-26 婺源县聚芳永茶业有限公司 Extraction method of roselle red color
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112111172A (en) * 2020-09-14 2020-12-22 苏州森创纺织科技有限公司 Extraction method of anti-bacterial plant dye combining cellulose mildew and ultrasonic waves
CN114388273A (en) * 2022-01-07 2022-04-22 青海大学 Preparation method and application of anthocyanin-sensitized P5FIN/ITO nano composite material
CN114388273B (en) * 2022-01-07 2022-10-14 青海大学 Preparation method and application of anthocyanin-sensitized P5FIN/ITO nano composite material

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Inventor after: Ma Xiaoqiang

Inventor after: Pan Ting

Inventor after: Li Yue

Inventor after: Chen Zirong

Inventor before: Ma Xiaoqiang

Inventor before: Zhang Jian

Inventor before: Pan Ting

Inventor before: Li Yue

Inventor before: Huang Hongwan

Inventor before: Wan Quanhan

Inventor before: Chen Ying

Inventor before: Hong Run

Inventor before: Chen Zirong

Inventor before: Wu Fan

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Application publication date: 20190215

Assignee: Wuhan Huanran Technology Co.,Ltd.

Assignor: WUHAN POLYTECHNIC

Contract record no.: X2022420000116

Denomination of invention: Extraction and Application of a Natural Dye from Roselle

Granted publication date: 20201030

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Record date: 20221020