CN109054432A - A kind of brazilwood vegetable dye and its textile fabric coloring composition - Google Patents

A kind of brazilwood vegetable dye and its textile fabric coloring composition Download PDF

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Publication number
CN109054432A
CN109054432A CN201810729123.7A CN201810729123A CN109054432A CN 109054432 A CN109054432 A CN 109054432A CN 201810729123 A CN201810729123 A CN 201810729123A CN 109054432 A CN109054432 A CN 109054432A
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China
Prior art keywords
parts
brazilwood
vegetable dye
textile fabric
methanol
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CN201810729123.7A
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Chinese (zh)
Inventor
刘广飞
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Foshan City Clothing Design Co Ltd
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Foshan City Clothing Design Co Ltd
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Priority to CN201810729123.7A priority Critical patent/CN109054432A/en
Publication of CN109054432A publication Critical patent/CN109054432A/en
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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
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/54Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

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

Abstract

A kind of brazilwood vegetable dye and its textile fabric coloring composition, in brazilwood vegetable dye's extraction process, use ammonium hydroxide can be with extremely low dosage as entrainer, improve solvent degree of the hematoxylin in supercritical solvent, the usage amount for greatly reducing supercritical solvent improves extraction efficiency and increases the amount of precipitation of hematoxylin.The present invention is reasonably matched by plurality of raw materials, to realize that colouring is simple and textile dyeing agent not easy to fade, the present invention can improve the color fastness of fabric, color stability after dyeing will not also influence artificial adult body.

Description

A kind of brazilwood vegetable dye and its textile fabric coloring composition
Technical field
The present invention relates to textile technology field, in particular to a kind of brazilwood vegetable dye and its textile fabric coloring agent group Close object.
Background technique
" textile industry scientific and technological progress development outline " proposes: the development and application of environmental protection type dye are that development textile printing and dyeing is novel The task of top priority of technology, directly affects enterprise competitiveness and benefit, it has also become hinders the bottleneck of dyeing industry development.It spins now Knitting the dyestuff that printing and dyeing enterprise uses is essentially all chemical dye, and chemical dye was born in Britain in 1846, by coloring jail It spends, quick advantage of printing and dyeing, soon instead of the natural plant dye for having adopted thousands of years after successor China.But Be with chemical dye pollution environment, it is unhealthful the problems such as gradually show, natural plant dye is with its distinctive green ring Guaranteed cost becomes the hot spot and research direction of stakeholder in the industry and enterprises pay attention again.Natural plants dyeing is a Gu Old textile dyeing, dye source used can generally drop naturally in the root of plant, stem, leaf, flower, fruit etc., pigment Solution, therefore have the characteristics that nonhazardous, free of contamination, many chemical dye brings harm are avoided, it is simultaneous with good environment Capacitive.And many natural plant dyes have antibacterial, anti-inflammatory, health care and other effects due to its own as middle medicinal herbs.? Today back to nature social theme in, using natural plant dye exploitation health environment-friendly product catered to textile printing and dyeing product to Ecology, environmental protection, health, comfortable and function sexual development trend.
Traditional plant dye most common problem of textile fabric is exactly that color fastness is not ideal enough, according to existing research, On the one hand reason is that the unstable chromophoric group of vegetable colour reduces its washable and color fastness to light, on the other hand, plant dye The pigment of material also affects it to fabric color after dyeing from different plant, and with environment, geography, the difference in season The stability of fastness and the reproducibility of color.
Summary of the invention
The purpose of the present invention is being directed to technological deficiency existing in the prior art, a kind of brazilwood vegetable dye and its spinning are provided Knitted fabric coloring composition is not only good to the coloring effect of textile fabric but also harmless.
In order to solve the above-mentioned technical problem, technical scheme is as follows:
A kind of textile fabric brazilwood vegetable dye, which is characterized in that preparation method the following steps are included:
1) it will be put into extraction kettle after bush dry powder, be passed through supercritical methanol as extractant, ammonium hydroxide is added as entrainment Agent, extraction temperature are 20~25 DEG C, 6~7MPa of extracting pressure, and extraction time is 10~15 minutes, and methanol flow rate is 1~10L/ H, 0.1~0.55ml/min of entrainer flow velocity;
2) supercritical methanol containing extract is depressurized, to isolate extraction product, 10~20 DEG C of separation temperature, Separating pressure is 1~5MPa, collects resulting extract liquor;
3) it is concentrated into paste, upper macroreticular resin is successively washed till clarification of water with the ethyl alcohol of water, 5~10%, finally uses 80- 85% ethanol elution, eluent ethyl alcohol of going out obtain concentrate A;
4) it will be filtered after concentrate A alcohol solvent, filtrate mixes sample, upper polyamide chromatography column, using volume with polyamide Ratio is that 10:1~1:1 water and methanol mixed solution carry out gradient elution, and collect water: methanol is that 8:1~5:1 eluent is concentrated to give Concentrate B, then by concentrate B freeze-drying after to obtain the final product.
Use ammonium hydroxide that can improve solvent of the hematoxylin in supercritical solvent as entrainer with extremely low dosage Degree, greatly reduces the usage amount of supercritical solvent, improves extraction efficiency and increase the amount of precipitation of hematoxylin.
It further, further include the preparation step of bush dry powder, the preparation step of the bush dry powder before step 1) are as follows: Vacuum freeze drying processing will be carried out after bush stripping and slicing, then the Chinese aloe leaf after drying process is crushed, is sieved.Further The drying temperature on ground, the vacuum freeze drying processing is -30~-50 DEG C, and drying time is 10~20 hours, the sieving Sieve is 30~50 mesh.
Further, extraction temperature described in step 1) is 25 DEG C, extracting pressure 6MPa, extraction time 10min, first Alcohol flow velocity is 6L/h, entrainer flow velocity 0.2ml/min.
Macroreticular resin is D-101 type or AB-8 type in step 3).
Another aspect of the present invention also provides a kind of textile fabric coloring composition, wherein preparing institute comprising the above method The brazilwood vegetable dye obtained, content are calculated by weight as 10~15 parts.
Further, the textile fabric coloring composition also includes following component: diphenyl ether tetracid dianhydride 8~ 10 parts, 2~5 parts of polypropylene glycol, 18~20 parts of mica powder, 2~5 parts of zinc stearate, 7~10 parts of ethyl triethoxysilane, carbon 4~7 parts of sour sodium, 3~5 parts of ethyl alcohol, 40~45 parts of water, 5~8 parts of polyvinylpyrrolidone.
Further, the textile fabric is silk.
Compared with prior art, a kind of textile fabric coloring agent of the invention, has the following beneficial effects:
1) in brazilwood vegetable dye's extraction process, use ammonium hydroxide that can improve Soviet Union as entrainer with extremely low dosage Solvent degree of the wooden pigment in supercritical solvent, greatly reduces the usage amount of supercritical solvent, improves extraction efficiency and increase The amount of precipitation of hematoxylin is added.
2) present invention is reasonably matched by plurality of raw materials, to realize that colouring is simply contaminated with fabric not easy to fade Toner, the present invention can improve the color fastness of fabric, and color stability after dyeing will not also influence artificial adult body.
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects It encloses.
[embodiment 1]
The present embodiment provides a kind of textile fabric coloring agent, which includes consisting of composition by weight: 10 parts of brazilwood vegetable dye, 8 parts of diphenyl ether tetracid dianhydride, 5 parts of polypropylene glycol, 20 parts of mica powder, 5 parts of zinc stearate, ethyl three 10 parts of Ethoxysilane, 7 parts of sodium carbonate, 5 parts of ethyl alcohol, 45 parts of water, 8 parts of polyvinylpyrrolidone.
Wherein, brazilwood vegetable dye is prepared using following preparation method:
1) being carried out after bush stripping and slicing -- 50 DEG C of vacuum freeze dryings are handled 10 hours, then to the aloe after drying process Leaf is crushed, 50 meshes excessively obtain aloe dry powder.
It will be put into extraction kettle after bush dry powder, be passed through supercritical methanol as extractant, ammonium hydroxide is added as entrainer, Extraction temperature is 25 DEG C, extracting pressure 7MPa, and extraction time is 10 minutes, methanol flow rate 5L/h, entrainer flow velocity 0.1ml/ min;
2) supercritical methanol containing extract is depressurized, to isolate extraction product, 10 DEG C of separation temperature, is separated Pressure is 1MPa, collects resulting extract liquor;
4) it is concentrated into paste, upper D-101 type macroreticular resin is successively washed till clarification of water with the ethyl alcohol of water, 10%, finally uses 85% ethanol elution, eluent ethyl alcohol of going out obtain concentrate A;
5) it will be filtered after concentrate A alcohol solvent, filtrate mixes sample, upper polyamide chromatography column, using volume with polyamide Ratio is that 10:1~1:1 water and methanol mixed solution carry out gradient elution, and collect water: methanol is that 8:1~5:1 eluent is concentrated to give Concentrate B, then by concentrate B freeze-drying after to obtain the final product.
[embodiment 2]
The present embodiment provides a kind of textile fabric coloring agent, which includes consisting of composition by weight: 15 parts of brazilwood vegetable dye, 10 parts of diphenyl ether tetracid dianhydride, 5 parts of polypropylene glycol, 19 parts of mica powder, 4 parts of zinc stearate, ethyl three 8 parts of Ethoxysilane, 5 parts of sodium carbonate, 4 parts of ethyl alcohol, 45 parts of water, 6 parts of polyvinylpyrrolidone.
Wherein, brazilwood vegetable dye is prepared using following preparation method:
To be carried out after bush stripping and slicing -- 50 DEG C of vacuum freeze dryings are handled 10 hours, then to the Chinese aloe leaf after drying process It is crushed, 50 meshes excessively obtain aloe dry powder.
It will be put into extraction kettle after bush dry powder, be passed through supercritical methanol as extractant, ammonium hydroxide is added as entrainer, Extraction temperature is 25 DEG C, extracting pressure 6MPa, and extraction time is 15 minutes, methanol flow rate 10L/h, entrainer flow velocity 0.1ml/ min;
2) supercritical methanol containing extract is depressurized, to isolate extraction product, 20 DEG C of separation temperature, is separated Pressure is 5MPa, collects resulting extract liquor;
4) it is concentrated into paste, upper D-101 macroreticular resin is successively washed till clarification of water with the ethyl alcohol of water, 10%, finally with 80% Ethanol elution, eluent ethyl alcohol of going out obtain concentrate A;
5) it will be filtered after concentrate A alcohol solvent, filtrate mixes sample, upper polyamide chromatography column, using volume with polyamide Ratio is that 10:1~1:1 water and methanol mixed solution carry out gradient elution, and collect water: methanol is that 8:1~5:1 eluent is concentrated to give Concentrate B, then by concentrate B freeze-drying after to obtain the final product.
[embodiment 3]
The present embodiment provides a kind of textile fabric coloring agent, which includes consisting of composition by weight: 12 parts of brazilwood vegetable dye, 9 parts of diphenyl ether tetracid dianhydride, 3 parts of polypropylene glycol, 20 parts of mica powder, 5 parts of zinc stearate, ethyl three 10 parts of Ethoxysilane, 7 parts of sodium carbonate, 5 parts of ethyl alcohol, 40 parts of water, 7 parts of polyvinylpyrrolidone.
Wherein, brazilwood vegetable dye is prepared using following preparation method:
To be carried out after bush stripping and slicing -- 50 DEG C of vacuum freeze dryings are handled 10 hours, then to the Chinese aloe leaf after drying process It is crushed, 50 meshes excessively obtain aloe dry powder.
It will be put into extraction kettle after bush dry powder, be passed through supercritical methanol as extractant, ammonium hydroxide is added as entrainer, Extraction temperature is 20 DEG C, extracting pressure 6MPa, and extraction time is 10 minutes, methanol flow rate 10L/h, entrainer flow velocity 0.55ml/min;
2) supercritical methanol containing extract is depressurized, to isolate extraction product, 20 DEG C of separation temperature, is separated Pressure is 5MPa, collects resulting extract liquor;
4) it is concentrated into paste, upper macroreticular resin is successively washed till clarification of water with the ethyl alcohol of water, 10%, finally with 85% ethyl alcohol Elution, eluent ethyl alcohol of going out obtain concentrate A;
5) it will be filtered after concentrate A alcohol solvent, filtrate mixes sample, upper polyamide chromatography column, using volume with polyamide Ratio is that 10:1~1:1 water and methanol mixed solution carry out gradient elution, and collect water: methanol is that 8:1~5:1 eluent is concentrated to give Concentrate B, then by concentrate B freeze-drying after to obtain the final product.
Above description sufficiently discloses a specific embodiment of the invention.It should be pointed out that being familiar with the field Range of any change that technical staff does a specific embodiment of the invention all without departing from claims of the present invention. Correspondingly, the scope of the claims of the invention is also not limited only to previous embodiment.

Claims (8)

1. a kind of brazilwood vegetable dye, which is characterized in that preparation method the following steps are included:
1) it will be put into extraction kettle after bush dry powder, be passed through supercritical methanol as extractant, ammonium hydroxide is added as entrainer, extraction Taking temperature is 20~25 DEG C, 6~7MPa of extracting pressure, and extraction time is 10~15 minutes, and methanol flow rate is 1~10L/h, entrainment 0.1~0.55ml/min of agent flow velocity;
2) supercritical methanol containing extract is depressurized, to isolate extraction product, 10~20 DEG C of separation temperature, is separated Pressure is 1~5MPa, collects resulting extract liquor;
3) it is concentrated into paste, upper macroreticular resin is successively washed till clarification of water with the ethyl alcohol of water, 5~10%, finally uses 80-85% second Alcohol elution, eluent ethyl alcohol of going out obtain concentrate A;
4) it will be filtered after concentrate A alcohol solvent, filtrate mixes sample, upper polyamide chromatography column, using volume ratio with polyamide Gradient elution is carried out for 10:1~1:1 water and methanol mixed solution, collect water: methanol is that 8:1~5:1 eluent is concentrated to give concentration Liquid B, then by concentrate B freeze-drying after to obtain the final product.
2. brazilwood vegetable dye according to claim 1, which is characterized in that further include the system of bush dry powder before step 1) Standby step, the preparation step of the bush dry powder are as follows: vacuum freeze drying processing will be carried out after bush stripping and slicing, then at dry Chinese aloe leaf after reason is crushed, is sieved.
3. brazilwood vegetable dye according to claim 2, which is characterized in that the dry temperature of the vacuum freeze drying processing Degree is -30~-50 DEG C, and drying time is 10~20 hours, and the sieve of the sieving is 30~50 mesh.
4. a kind of brazilwood vegetable dye according to claim 1, which is characterized in that extraction temperature described in step 1) is 25 DEG C, extracting pressure 6MPa, extraction time 10min, methanol flow rate 6L/h, entrainer flow velocity 0.2ml/min.
5. brazilwood vegetable dye's agent according to claim 1, which is characterized in that macroreticular resin is D-101 type in step 3) Or AB-8 type.
6. a kind of textile fabric coloring composition, which is characterized in that wherein comprising any one of the Claims 1 to 5 Soviet Union Wood plant dyestuff, content are calculated by weight as 10~15 parts.
7. textile fabric coloring composition according to claim 6, which is characterized in that also include following component: two 8~10 parts of phenylate tetracid dianhydride, 2~5 parts of polypropylene glycol, 18~20 parts of mica powder, 2~5 parts of zinc stearate, ethyl triethoxy 7~10 parts of silane, 4~7 parts of sodium carbonate, 3~5 parts of ethyl alcohol, 40~45 parts of water, 5~8 parts of polyvinylpyrrolidone.
8. textile fabric coloring composition according to claim 6, which is characterized in that the textile fabric is silk Silk fabric.
CN201810729123.7A 2018-07-05 2018-07-05 A kind of brazilwood vegetable dye and its textile fabric coloring composition Pending CN109054432A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102232994A (en) * 2011-05-06 2011-11-09 南京泽朗医药科技有限公司 Method for preparing total phenols of Lignum Sappan
CN107201671A (en) * 2017-05-22 2017-09-26 如皋市下原科技创业服务有限公司 A kind of weaving face fabric coloring agent
CN107326705A (en) * 2017-05-23 2017-11-07 如皋市下原科技创业服务有限公司 A kind of coloring agent for weaving face fabric
CN107641986A (en) * 2017-11-10 2018-01-30 湖州南浔金吉宝纺织有限公司 A kind of colouring method of thermal fabric
CN107761414A (en) * 2017-10-27 2018-03-06 如皋市协和印染有限公司 A kind of coloring agent for weaving face fabric

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102232994A (en) * 2011-05-06 2011-11-09 南京泽朗医药科技有限公司 Method for preparing total phenols of Lignum Sappan
CN107201671A (en) * 2017-05-22 2017-09-26 如皋市下原科技创业服务有限公司 A kind of weaving face fabric coloring agent
CN107326705A (en) * 2017-05-23 2017-11-07 如皋市下原科技创业服务有限公司 A kind of coloring agent for weaving face fabric
CN107761414A (en) * 2017-10-27 2018-03-06 如皋市协和印染有限公司 A kind of coloring agent for weaving face fabric
CN107641986A (en) * 2017-11-10 2018-01-30 湖州南浔金吉宝纺织有限公司 A kind of colouring method of thermal fabric

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
孙天竹等: "天然苏木色素羊毛染色中不同媒染剂染色工艺研究", 《针织工业》 *

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