CN107011698A - A kind of extracting method of the willow leaf colouring substance of high stability - Google Patents
A kind of extracting method of the willow leaf colouring substance of high stability Download PDFInfo
- Publication number
- CN107011698A CN107011698A CN201710220075.4A CN201710220075A CN107011698A CN 107011698 A CN107011698 A CN 107011698A CN 201710220075 A CN201710220075 A CN 201710220075A CN 107011698 A CN107011698 A CN 107011698A
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- CN
- China
- Prior art keywords
- willow leaf
- chitosan
- pigment
- high stability
- colouring substance
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B68/00—Organic pigments surface-modified by grafting, e.g. by establishing covalent or complex bonds, in order to improve the pigment properties, e.g. dispersibility or rheology
- C09B68/20—Organic pigments surface-modified by grafting, e.g. by establishing covalent or complex bonds, in order to improve the pigment properties, e.g. dispersibility or rheology characterised by the process features
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B68/00—Organic pigments surface-modified by grafting, e.g. by establishing covalent or complex bonds, in order to improve the pigment properties, e.g. dispersibility or rheology
- C09B68/40—Organic pigments surface-modified by grafting, e.g. by establishing covalent or complex bonds, in order to improve the pigment properties, e.g. dispersibility or rheology characterised by the chemical nature of the attached groups
- C09B68/48—Non-aromatic cyclic groups
- C09B68/485—Substituted non-aromatic cyclic groups
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Cosmetics (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Coloring (AREA)
Abstract
The invention discloses a kind of extracting method of the willow leaf colouring substance of high stability, it is extracted the various pigments in willow leaf to greatest extent with the method for alcohol extracting, it is more highly efficient than traditional alkali carries means, auxiliary agent is used as using nano silicon during defibrination simultaneously, the dissolution of pigment can be accelerated, while the salicylic acid in compound and pigment of the chitosan after amido protecting into effective esterification occur, produce salicylic acid esterification derivative, it has good assisting-dyeing performance, pigment stability after chitosan-modified is higher, pigment saponification process will be finally modified again, water miscible high stable natural pigment dyestuff is made, realize the efficient of pigment in willow leaf, it is stable to extract, realize the higher value application of willow leaf.
Description
Technical field
The present invention relates to nature strength technical field, and in particular to the willow leaf colouring substance of high stability a kind of is carried
Take method.
Background technology
Huaihe river in Anhui abounds with purple willow from ancient times, and common people gather materials on the spot, made of purple willow a large amount of production apparatus with
Life instrument, artist comes forth in large number, and passes on from generation to generation, and it works out of superb skills, and character of artwork is unique, with strong folk culture gas
Breath.With the development of the social economy, traditional wicker plaiting article production gradually develops into modern wicker plaiting article industry, traditional willow-plaited process is being kept
The cycle development of industry is realized on the basis of elite, the utilization rate of resource is improved, forms the development mould of a set of many industrial chains
Formula is the prerequisite of wicker plaiting article techno-globalism and the marketization.
Purple willow belongs to Salicaceae Salix, and the purple willow bar after peeling is elongated pure white smooth, is the main former material for making wicker plaiting article product
Material, have the advantages that planting cost is low, income is high, manageability and be widely cultivated, yield increases year by year.Done manual work using purple willow
Skill product are needed withy peeling defoliation processing, and this creates the terminal substantial amounts of willow leaf discarded object, processing method traditional at present
It is exactly not high as the agriculture roughing field economic value such as feed or fertilizer.
With the improvement of living standards, security requirement more and more higher of the consumer to product, natural attribute it is chemicalization
Work class raw material always is what consumer was willing to accept.Wherein dye substance is ubiquitous in daily life, synthesizes class chemical industry
A large amount of using being undoubtedly to consumer and the potential potential safety hazard of natural environment, and the chemical dyestuff of the high-quality often valency of dyestuff
Value is high.Natural plant dyestuff is the dyestuff that a class is obtained from plant, possesses vast potential for future development, due to natural pigment by
Extraneous factor influence is big, and less stable has certain limitation in actual application.
A variety of pigments, resource and very abundant are rich in Folium Pterocaryae, the extraction and application of pigment is carried out from Folium Pterocaryae weight
The application value realistic wanted, is also the effective way for improving willow leaf added value, and contain salicylic acid, salicylic esterification in willow leaf
Thing plays the role of good assisting-dyeing and protection pigment so that Folium Pterocaryae colouring substance practicality is stronger.Document《Folium Pterocaryae natural colour
Element extraction and for silk broadcloth dying》Folium Pterocaryae is extracted in 80-100 DEG C of condition with sodium hydroxide solution, extract solution
Effective dyeing to silk broadcloth is realized, but this extracting method does not have the work(effectively using salicylic acid and its derivative
Effect, the stability of pigment and upper dye effect on the Fiber Materials such as chemical fibre be not good.
The content of the invention
There is provided a kind of extraction side of the willow leaf colouring substance of high stability for the defect that makes up prior art by the present invention
Method.
The present invention is achieved by the following technical solutions：
A kind of extracting method of the willow leaf colouring substance of high stability, comprises the following steps：
（1）Fresh, complete, the ripe willow leaf of harvesting, puts into grinder after cleaning up, sequentially adds absolute ethyl alcohol, nanometer
Ground after silica, slurry is extracted 2-3 times under the conditions of 60-80 DEG C, and 2-3h is extracted every time, obtains extract solution；
（2）By extract solution through ultrafiltration membrance filter, filtrate is collected, filtrate is concentrated and dried, and obtains pigmented powder standby；
（3）Chitosan, phthalic anhydride are taken, puts into successively in DMF, is warming up to 100 DEG C, is stirred at reflux under nitrogen atmosphere anti-
Answer after 4-5h and to pour into reaction product in frozen water, drying process after gained sediment is washed till neutrality through alcohol, material grinds to form fine powder,
Obtain modification of chitosan standby；
（4）Pigmented powder, modification of chitosan are put into dichloromethane successively, the stirring reaction 20-30min under condition of ice bath, instead
System is dried in vacuo after should terminating, recycling design；
（5）By step（4）Resulting material is put into the 10-15 times of ethanol measured, and is stirring evenly and then adding into the hydrogen that concentration is 10-15%
Aqueous solution of sodium oxide, regulation system pH value to 10-12, heating water bath backflow 1-1.5h, saponification knot under the conditions of 50-60 DEG C
Saponification liquor is concentrated under reduced pressure processing after beam, described willow leaf colouring substance is produced, concentration and pH value needed for being diluted to when using are i.e.
Can.
Described step（1）The weight ratio of middle willow leaf and absolute ethyl alcohol is 1:15-20.
Described step（1）The addition of middle nano silicon is 1 ‰.
Described step（3）In chitosan, phthalic anhydride, DMF three amount ratio be 1g:3g:20ml.
Described step（4）In pigmented powder, modification of chitosan, dichloromethane three amount ratio be 1g:0.01g:
10ml。
The present invention is extracted the various pigments in willow leaf with the method for alcohol extracting to greatest extent, than traditional alkali carries means more
To be efficient, while using nano silicon as auxiliary agent during defibrination, the dissolution of pigment can be accelerated, while chitosan is passed through
Effective esterification occurs for the salicylic acid in the compound and pigment after amido protecting, produces salicylic acid esterification derivative, its
Have a good assisting-dyeing performance, it is chitosan-modified after pigment stability it is higher, finally again will modified pigment saponification process, water is made
The high stable natural pigment dyestuff of dissolubility, realizes the efficient, stable of pigment in willow leaf and extracts, realize the high-valued profit of willow leaf
With.
Embodiment
A kind of extracting method of the willow leaf colouring substance of high stability, comprises the following steps：
（1）Fresh, complete, the ripe willow leaf of harvesting, puts into grinder after cleaning up, sequentially adds absolute ethyl alcohol, nanometer
Ground after silica, slurry is extracted 2 times under the conditions of 60 DEG C, and 2h is extracted every time, extract solution is obtained；
（2）By extract solution through ultrafiltration membrance filter, filtrate is collected, filtrate is concentrated and dried, and obtains pigmented powder standby；
（3）Chitosan, phthalic anhydride are taken, puts into successively in DMF, is warming up to 100 DEG C, is stirred at reflux under nitrogen atmosphere anti-
Answer after 4h and to pour into reaction product in frozen water, drying process after gained sediment is washed till neutrality through alcohol, material grinds to form fine powder, obtains
Modification of chitosan is standby；
（4）Pigmented powder, modification of chitosan are put into dichloromethane successively, the stirring reaction 20min under condition of ice bath, reaction knot
System is dried in vacuo after beam, recycling design；
（5）By step（4）Resulting material is put into the ethanol of 10 times of amounts, is stirring evenly and then adding into the sodium hydroxide that concentration is 10%
The aqueous solution, regulation system pH value to 10, the heating water bath backflow 1h under the conditions of 50 DEG C, saponification depressurizes saponification liquor after terminating
Concentration, produces described willow leaf colouring substance, concentration and pH value needed for being diluted to when using.
Wherein step（1）The weight ratio of middle willow leaf and absolute ethyl alcohol is 1:15.
Wherein step（1）The addition of middle nano silicon is 1 ‰.
Wherein step（3）In chitosan, phthalic anhydride, DMF three amount ratio be 1g:3g:20ml.
Wherein step（4）In pigmented powder, modification of chitosan, dichloromethane three amount ratio be 1g:0.01g:10ml.
Claims (5)
1. the extracting method of the willow leaf colouring substance of a kind of high stability, it is characterised in that comprise the following steps：
（1）Fresh, complete, the ripe willow leaf of harvesting, puts into grinder after cleaning up, sequentially adds absolute ethyl alcohol, nanometer
Ground after silica, slurry is extracted 2-3 times under the conditions of 60-80 DEG C, and 2-3h is extracted every time, obtains extract solution；
（2）By extract solution through ultrafiltration membrance filter, filtrate is collected, filtrate is concentrated and dried, and obtains pigmented powder standby；
（3）Chitosan, phthalic anhydride are taken, puts into successively in DMF, is warming up to 100 DEG C, is stirred at reflux under nitrogen atmosphere anti-
Answer after 4-5h and to pour into reaction product in frozen water, drying process after gained sediment is washed till neutrality through alcohol, material grinds to form fine powder,
Obtain modification of chitosan standby；
（4）Pigmented powder, modification of chitosan are put into dichloromethane successively, the stirring reaction 20-30min under condition of ice bath, instead
System is dried in vacuo after should terminating, recycling design；
（5）By step（4）Resulting material is put into the 10-15 times of ethanol measured, and is stirring evenly and then adding into the hydrogen that concentration is 10-15%
Aqueous solution of sodium oxide, regulation system pH value to 10-12, heating water bath backflow 1-1.5h, saponification knot under the conditions of 50-60 DEG C
Saponification liquor is concentrated under reduced pressure processing after beam, described willow leaf colouring substance is produced, concentration and pH value needed for being diluted to when using are i.e.
Can.
2. the extracting method of the willow leaf colouring substance of a kind of high stability as claimed in claim 1, it is characterised in that described
Step（1）The weight ratio of middle willow leaf and absolute ethyl alcohol is 1:15-20.
3. the extracting method of the willow leaf colouring substance of a kind of high stability as claimed in claim 1, it is characterised in that described
Step（1）The addition of middle nano silicon is 1 ‰.
4. the extracting method of the willow leaf colouring substance of a kind of high stability as claimed in claim 1, it is characterised in that described
Step（3）In chitosan, phthalic anhydride, DMF three amount ratio be 1g:3g:20ml.
5. the extracting method of the willow leaf colouring substance of a kind of high stability as claimed in claim 1, it is characterised in that described
Step（4）In pigmented powder, modification of chitosan, dichloromethane three amount ratio be 1g:0.01g:10ml.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710220075.4A CN107011698A (en) | 2017-04-06 | 2017-04-06 | A kind of extracting method of the willow leaf colouring substance of high stability |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710220075.4A CN107011698A (en) | 2017-04-06 | 2017-04-06 | A kind of extracting method of the willow leaf colouring substance of high stability |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107011698A true CN107011698A (en) | 2017-08-04 |
Family
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| Application Number | Title | Priority Date | Filing Date |
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| CN201710220075.4A Pending CN107011698A (en) | 2017-04-06 | 2017-04-06 | A kind of extracting method of the willow leaf colouring substance of high stability |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104087020A (en) * | 2014-07-01 | 2014-10-08 | 常州大学 | Preparation method and application of chitosan-natural plant pigment macromolecular dye solution |
| CN104877376A (en) * | 2014-02-27 | 2015-09-02 | 哈尔滨市工艺美术有限责任公司 | A dye for preparing moss green wheat straw and a producing method thereof |
| CN105061773A (en) * | 2015-09-08 | 2015-11-18 | 湖州新创丝织品有限公司 | Novel chitosan-modified epoxy-resin-base high-polymer dye and preparation method thereof |
| CN106280873A (en) * | 2016-08-08 | 2017-01-04 | 雷春生 | A kind of preparation method of child's pattern finish |
-
2017
- 2017-04-06 CN CN201710220075.4A patent/CN107011698A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104877376A (en) * | 2014-02-27 | 2015-09-02 | 哈尔滨市工艺美术有限责任公司 | A dye for preparing moss green wheat straw and a producing method thereof |
| CN104087020A (en) * | 2014-07-01 | 2014-10-08 | 常州大学 | Preparation method and application of chitosan-natural plant pigment macromolecular dye solution |
| CN105061773A (en) * | 2015-09-08 | 2015-11-18 | 湖州新创丝织品有限公司 | Novel chitosan-modified epoxy-resin-base high-polymer dye and preparation method thereof |
| CN106280873A (en) * | 2016-08-08 | 2017-01-04 | 雷春生 | A kind of preparation method of child's pattern finish |
Non-Patent Citations (2)
| Title |
|---|
| 陈洪玉: ""柳树叶中原花青素含量测定"", 《应用化工》 * |
| 陶永瑛: ""柳树叶天然色素的提取及用于真丝绸染色"", 《纺织科技进展》 * |
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Application publication date: 20170804 |