A kind of extracting method of lavandula angustifolia dyestuff and the application in regenerated cellulose fibre dyeing thereof
Technical field
The present invention relates to a kind of extracting method of lavandula angustifolia dyestuff and the application in regenerated cellulose fibre dyeing thereof, belong to dyeing keratin-fiber field.
Background technology
From 19 end of the centurys, due to developing rapidly of synthetic dyestuff, natural dyestuff is made substantially to have exited textile dyeing field.Along with the continuous enhancing of mankind's environmental consciousness and the growing interest to own health, the harm that partial synthesis dyestuff produces human health and ecotope is more and more noticeable, under global Green Revolution tide, natural dyestuff starts again as people are paid attention to, in natural dyestuff, vegetable dye extracts by organism, good with Environmental compatibility, biodegradable, in dyeing course, its flavour ingredient is absorbed by fabric together with pigment, except dyeing function, natural dyestuff also has the several functions such as spices.
Lavandula angustifolia is perennial herb or stunted brushwood, though be called grass, actual is a kind of hyacinthine little Hua, lavandula angustifolia grows thickly, multi-branched, and common is vertical growth, plant height has 30 ~ 40 centimetres, 45 ~ 90 centimetres according to kind, and in the mountain area that height above sea level is quite high, individual plant can grow to 1 meter.Leaf alternate, ellipse drapes over one's shoulders sharp leaf, or the aciculiform that blade face is larger, leaf margin warp, and spike top is raw, long 15 ~ 25 centimetres; Corolla lower barrel, top lip, upper lip 2 splits, and lower lip 3 splits; Flower is about 1.2 centimetres, and have indigo plant, dark purple, pink, white isochrome, common is hyacinthine, the florescence 6-8 month.
Prior art adopts plant milk extract to carry out dyeing process regenerated cellulose fibre, has the following disadvantages:
(1) dye uptake and degree of fixation low;
(2) dyefastness is low, and aberration is large;
(3) need add inorganic salt during dyeing, soda ash add-on is high, and dye dosage is many, and dyeing waste-water discharge is many, and production cost is high, big for environment pollution;
(4) without ultraviolet performance or UV resistance poor performance.
Summary of the invention
The present invention, for solving above technical problem, provides a kind of extracting method of lavandula angustifolia dyestuff and the application in regenerated cellulose fibre dyeing thereof, to realize following goal of the invention:
(1) extracting method of lavandula angustifolia dyestuff of the present invention, application in regenerated cellulose fibre dyeing, dye uptake and degree of fixation significantly improve, and dye uptake reaches 94.2-96.8%, and degree of fixation reaches 94.4-95.6%.
(2) extracting method of lavandula angustifolia dyestuff of the present invention, application in regenerated cellulose fibre dyeing,
Intensity of soaping reaches 4 grades, and crock fastness reaches 4-5 level, and K/S value is 21-21.3, and staining fastness reaches 5 grades, and value of chromatism △ E is less than 0.04.
(3) extracting method of lavandula angustifolia dyestuff of the present invention, application in regenerated cellulose fibre dyeing, without the need to adding inorganic salt (Sodium sulfate anhydrous.min(99) and sodium-chlor) during dyeing, the add-on of soda ash is reduced to 2g/L, dyestuff consumption reduces by 35%, reduce production cost, dyeing waste-water discharge minimizing 55%, reduces the pollution to environment.
(4) extracting method of lavandula angustifolia dyestuff of the present invention, application in regenerated cellulose fibre dyeing, ultraviolet resistance is good.
For solving above technical problem, the technical solution used in the present invention is as follows:
Below the further improvement to technique scheme:
An extracting method for lavandula angustifolia dyestuff, comprises microwave frequency measurment, the extraction of subcritical liquefied ammonia, resin elution.
Described microwave frequency measurment, selects the ethanol of 50-65% as solvent, and the lavandula angustifolia powder after process and the mass ratio of solvent are 1:50-80, be placed in the temperature of 60-70 DEG C, microwave radiation 3-5 minute, microwave wavelength is 120-140 millimeter, frequency is 2000 megahertzes, obtains lavandula angustifolia extraction thing.
Described subcritical liquefied ammonia extraction, extracting pressure 1.8-2.2MPa, temperature is 42-45 DEG C, and liquefied ammonia flow is 12-15L/h; Described subcritical liquefied ammonia extraction, primary separator pressure 0.3-0.6MPa, temperature is 35-42 DEG C, and second-stage separator pressure is 0.1-0.3MPa, and temperature is 35-40 DEG C.
Described subcritical liquefied ammonia extraction, obtain lavandula angustifolia dyestuff crude extract after extraction, containing 7-10% entrainment agent in described liquefied ammonia, described entrainment agent, comprises 60-70% ethanol, ethyl acetate 15-20%, butanols 15-20%.
Described resin elution, gets lavandula angustifolia dyestuff crude extract, adds the water dilution of 10 times of weight parts, preparation lavandula angustifolia dye solution, upper macroporous adsorptive resins, coutroi velocity 2-3BV/h; Described resin column, amount of resin is 12 times of parts by volume of lavandula angustifolia dyestuff crude extract, and blade diameter length ratio is 1: 8.
Described resin elution, after lavandula angustifolia dye solution stream is complete, first washes 14-15BV with water, flow velocity 2-3BV/h, then uses the ethanol elution 11-12BV of 40-45%, flow velocity 4-5BV/h; Finally use the ethanol elution 6BV of 60-70%, flow velocity 3BV/h.
A kind of application of extracting method in regenerated cellulose fibre dyeing of lavandula angustifolia dyestuff, comprise regenerated cellulose fibre modification, described regenerated cellulose fibre properties-correcting agent, the mass ratio of each component is: containing carboxyl water-borne acrylic resin 20 parts, treated starch 25 parts, polydimethylsiloxane 5 parts, polyepichlorohydrin amine compound 3 parts, xylenylphosphate 2 parts, 3 parts, 2-pyridinethiol-1-zinc oxide, nano zirconium dioxide 5 parts.
Described containing carboxyl water-borne acrylic resin, acid number is 150-180mgKOH/g, and second-order transition temperature is-50 DEG C ~ 50 DEG C; Described treated starch: molecular weight is 80-100 ten thousand, acid number is 80-100mgKOH/g, and substitution value is 0.03-0.05; Described regenerated cellulose fibre is the one in viscose fiber, modalic fiber.
Described application, comprises modified regenerated cellulose fibre and dyes, lavandula angustifolia dyestuff and water are made into dye liquor, the concentration of dye liquor is 4-6wt%, and bath raio is 1:50-60, adds the levelling agent of 1-2wt%, at 45-50 DEG C, contaminate 100-120 minute, at 48-50 DEG C of fixation 45-55 minute.
Described levelling agent, the mass ratio of each component is: 1-propyl group phosphoric acid cyclic anhydride 10 parts, hexanolactam 5-7 part, iridoid glucoside 9 parts, cithrol 1-2 part, methylene-succinic acid-maleic acid 3 parts, butylated hydroxy anisole 2 parts, methylene-bis naphthalenesulfonate 2 parts.
Adopt above technical scheme, beneficial effect of the present invention is:
(1) extracting method of lavandula angustifolia dyestuff of the present invention, application in regenerated cellulose fibre dyeing, dye uptake and degree of fixation significantly improve, and dye uptake reaches 94.2-96.8%, and degree of fixation reaches 94.4-95.6%.
(2) extracting method of lavandula angustifolia dyestuff of the present invention, application in regenerated cellulose fibre dyeing, intensity of soaping is 4 grades, and crock fastness is 4-5 level, and K/S value is 21-21.3, and staining fastness is 5 grades, and value of chromatism △ E is 0.03-0.04.
(3) extracting method of lavandula angustifolia dyestuff of the present invention, application in regenerated cellulose fibre dyeing, without the need to adding inorganic salt (Sodium sulfate anhydrous.min(99) and sodium-chlor) during dyeing, the add-on of soda ash is reduced to 2g/L, dyestuff consumption reduces by 35%, reduce production cost, dyeing waste-water discharge minimizing 55%, reduces the pollution to environment.
(4) extracting method of lavandula angustifolia dyestuff of the present invention, application in regenerated cellulose fibre dyeing, ultraviolet resistance is good, after 35 washings, regenerated cellulose fibre at the spectral transmittance T=2.0-3.0% of UVB and UVA wave band, UPF UPF=55-60.
Embodiment
Below the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein is only for instruction and explanation of the present invention, is not intended to limit the present invention.
the extracting method of embodiment 1 one kinds of lavandula angustifolia dyestuffs
an extracting method for lavandula angustifolia dyestuff, comprises the following steps
(1) pre-treatment of raw material
Get the flower of lavandula angustifolia, rinse well with clear water, low-temperature air-drying, be crushed to 100 orders.
(2) microwave frequency measurment
By the lavandula angustifolia powder crushed, select the ethanol of 65% as solvent, the mass ratio of lavandula angustifolia powder and solvent is 1:80, is placed in the temperature of 70 DEG C, microwave radiation 3 minutes, and microwave wavelength is 140 millimeters, and frequency is 2000 megahertzes, obtains lavandula angustifolia extraction thing.
(3) subcritical liquefied ammonia extraction
Get lavandula angustifolia extraction thing 100kg, send in the extractor of construction of pressure vessel, after closing feeding-passage, device internal pressure is made to be down to-0.095MPa after deflating, inject liquefied ammonia to extract, extracting pressure 1.8MPa, temperature is 45 DEG C, liquefied ammonia flow is 15L/h, containing 7% entrainment agent in liquefied ammonia, comprise 70% ethanol, ethyl acetate 15%, butanols 15%, primary separator pressure 0.3MPa, temperature is 42 DEG C, second-stage separator pressure is 0.3MPa, temperature is 40 DEG C, extraction gained extraction liquid, enter vapo(u)rization system, solvent is gasified be separated with extract, collect extract, obtain lavandula angustifolia dyestuff crude extract, after having extracted, remove the solvent in material, residue is taken out from extractor, recycling design recycles.
(4) resin elution
Get lavandula angustifolia dyestuff crude extract, add the water dilution of 10 times of weight parts, upper D101 type macroporous adsorptive resins, amount of resin is 12 times of parts by volume of lavandula angustifolia dyestuff crude extract, and blade diameter length ratio is 1: 8, coutroi velocity 3BV/h; After lavandula angustifolia dye solution stream is complete, first wash 14BV with water, flow velocity 3BV/h, then use the ethanol elution 11BV of 45%, flow velocity 5BV/h; Finally use the ethanol elution 6BV of 70%, flow velocity 3BV/h, the elutriant obtained carries out underpressure distillation and concentrates, solidifies, pulverizes, and reclaims ethanol, obtains lavandula angustifolia dyestuff extract.
the extracting method of embodiment 2 one kinds of lavandula angustifolia dyestuffs
(1) pre-treatment of raw material
Get the flower of lavandula angustifolia, rinse well with clear water, low-temperature air-drying, be crushed to 200 orders.
(2) microwave frequency measurment
By the lavandula angustifolia powder crushed, select the ethanol of 50% as solvent, the mass ratio of lavandula angustifolia powder and solvent is 1:50, is placed in the temperature of 60 DEG C, microwave radiation 5 minutes, and microwave wavelength is 120 millimeters, and frequency is 2000 megahertzes, obtains lavandula angustifolia extraction thing.
(3) subcritical liquefied ammonia extraction
Get lavandula angustifolia extraction thing 150kg, send in the extractor of construction of pressure vessel, after closing feeding-passage, device internal pressure is made to be down to-0.10MPa after deflating, inject liquefied ammonia to extract, extracting pressure 2.2MPa, temperature is 42 DEG C, liquefied ammonia flow is 12L/h, containing 10% entrainment agent in liquefied ammonia, comprise 60% ethanol, ethyl acetate 20%, butanols 20%, primary separator pressure 0.6MPa, temperature is 35 DEG C, second-stage separator pressure is 0.1MPa, temperature is 35 DEG C, extraction gained extraction liquid, enter vapo(u)rization system, solvent is gasified be separated with extract, collect extract, obtain lavandula angustifolia dyestuff crude extract, after having extracted, remove the solvent in material, residue is taken out from extractor, recycling design recycles.
(4) resin elution
Get lavandula angustifolia dyestuff crude extract, add the water dilution of 10 times of weight parts, upper D101 type macroporous adsorptive resins, amount of resin is 12 times of parts by volume of lavandula angustifolia dyestuff crude extract, and blade diameter length ratio is 1: 8, coutroi velocity 2BV/h; After lavandula angustifolia dye solution stream is complete, first wash 15BV with water, flow velocity 2BV/h, then use the ethanol elution 12BV of 40%, flow velocity 4BV/h; Finally use the ethanol elution 6BV of 60%, flow velocity 3BV/h, the elutriant obtained carries out underpressure distillation and concentrates, solidifies, pulverizes, and reclaims ethanol, obtains lavandula angustifolia dyestuff extract.
the application of embodiment 3 in regenerated cellulose fibre (viscose fiber) dyeing
(1) regenerated cellulose fibre modification
Preparation modifier solution, strength of solution is 12g/L, add sodium hydroxide according to 5g/L and regulate pH, regenerated cellulose fibre is put into modifier solution and be heated to 60 DEG C, react 40 minutes, bath raio (mass ratio of regenerated cellulose fibre and modifier solution) is 1:30, and on padding machine, two leachings two are rolled, pick-up is 80%, then on shaping drying 60 DEG C cure 20 minutes.
Described regenerated cellulose fibre properties-correcting agent, the mass ratio of each component is:
Containing carboxyl water-borne acrylic resin 20 parts, treated starch 25 parts, polydimethylsiloxane 5 parts, polyepichlorohydrin amine compound 3 parts, xylenylphosphate 2 parts, 3 parts, 2-pyridinethiol-1-zinc oxide, nano zirconium dioxide 5 parts.
Described regenerated cellulose fibre is viscose fiber, and dry breaking tenacity is 2.26CN/dtex, and wet breaking strength is 1.1CN/dtex, and residual sulfur content is 5.1mg/100mg, and whiteness is 50%.
Described containing carboxyl water-borne acrylic resin, acid number is 150mgKOH/g, and second-order transition temperature is 48.6;
Described treated starch: molecular weight is 800,000, acid number is 80mgKOH/g, and substitution value is 0.03;
Modification regeneration cellulosic fibre, pH is 7.2, Zeta electrode potential value is 32mV.
(2) modified regenerated cellulose fibre dyes:
Lavandula angustifolia dyestuff is water-soluble is made into dye liquor, the concentration of dye liquor is 4wt%, adding modified regenerated cellulose fibre bath raio (modified regenerated cellulose fibre weight and the mass ratio of dye liquor) is 1:60, add the levelling agent of 2wt%, at 50 DEG C, contaminate 100 minutes, add the soda ash solution of 2g/L, at 48 DEG C, be incubated 45 minutes.
Described levelling agent, the mass ratio of each component is:
1-propyl group phosphoric acid cyclic anhydride 10 parts, hexanolactam 7 parts, iridoid glucoside 9 parts, cithrol 1 part, methylene-succinic acid-maleic acid 3 parts, butylated hydroxy anisole 2 parts, methylene-bis naphthalenesulfonate 2 parts.
(3) aftertreatment
Comprise that acidity is soaped, washed, oven drying at low temperature.
result:
Lavandula angustifolia extracting method of the present invention, in regenerated cellulose fibre dyeing after application,
(1) without the need to adding inorganic salt (Sodium sulfate anhydrous.min(99) and sodium-chlor) when dyeing, the add-on of soda ash is reduced to 2g/L, and dyestuff consumption reduces by 35%, reduces production cost, and dyeing waste-water discharge minimizing 55%, reduces the pollution to environment.
(2) ultraviolet resistance is good, through 35 times washing after, regenerated cellulose fibre at the spectral transmittance T=3.0% of UVB and UVA wave band, UPF UPF=55.
Other results that test obtains are as following table 1:
Table 1
the application of embodiment 4 in regenerated cellulose fibre (modalic fiber) dyeing
(1) regenerated cellulose fibre modification
Preparation modifier solution, strength of solution is 15g/L, add sodium hydroxide according to 4g/L and regulate pH, regenerated cellulose fibre is put into modifier solution and be heated to 75 DEG C, react 30 minutes, bath raio (mass ratio of regenerated cellulose fibre and modifier solution) is 1:30, and on padding machine, two leachings two are rolled, pick-up is 60%, then on shaping drying 50 DEG C cure 20 minutes.
Described regenerated cellulose fibre properties-correcting agent, the mass ratio of each component is:
Containing carboxyl water-borne acrylic resin 20 parts, treated starch 25 parts, polydimethylsiloxane 5 parts, polyepichlorohydrin amine compound 3 parts, xylenylphosphate 2 parts, 3 parts, 2-pyridinethiol-1-zinc oxide, nano zirconium dioxide 5 parts.
Described regenerated cellulose fibre is modalic fiber, and dry breaking tenacity is 3.36CN/dtex, and wet breaking strength is 2.2CN/dtex, and residual sulfur content is 4.6mg/100mg, and whiteness is 60%.
Described containing carboxyl water-borne acrylic resin, acid number is 180mgKOH/g, and second-order transition temperature is-50 DEG C;
Described treated starch: molecular weight is 1,000,000, acid number is 100mgKOH/g, and substitution value is 0.05;
Modification regeneration cellulosic fibre, pH is 8.0, Zeta electrode potential value is 35mV.
(2) modified regenerated cellulose fibre dyes:
Lavandula angustifolia dyestuff is water-soluble is made into dye liquor, the concentration of dye liquor is 6wt%, adding modified regenerated cellulose fibre bath raio (modified regenerated cellulose fibre weight and the mass ratio of dye liquor) is 1:50, add the levelling agent of 1wt%, at 50 DEG C, contaminate 120 minutes, add the soda ash solution of 2g/L, make solution alkaline, at 50 DEG C, be incubated 55 minutes.
Described levelling agent, the mass ratio of each component is:
1-propyl group phosphoric acid cyclic anhydride 10 parts, hexanolactam 5 parts, iridoid glucoside 9 parts, cithrol 2 parts, methylene-succinic acid-maleic acid 3 parts, butylated hydroxy anisole 2 parts, methylene-bis naphthalenesulfonate 2 parts.
(3) aftertreatment
Comprise that acidity is soaped, washed, oven drying at low temperature.
result:
Lavandula angustifolia extracting method of the present invention, in regenerated cellulose fibre dyeing after application,
(1) without the need to adding inorganic salt (Sodium sulfate anhydrous.min(99) and sodium-chlor) when dyeing, the add-on of soda ash is reduced to 2g/L, and dyestuff consumption reduces by 35%, reduces production cost, and dyeing waste-water discharge minimizing 55%, reduces the pollution to environment.
(2) ultraviolet resistance is good, through 35 times washing after, regenerated cellulose fibre at the spectral transmittance T=2.0% of UVB and UVA wave band, UPF UPF=60.
Other results that test obtains are as following table 2:
Table 2
Except as otherwise noted, the percentage ratio adopted in the present invention is mass percent, and the ratio adopted, is mass ratio.
Last it is noted that the foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although with reference to previous embodiment to invention has been detailed description, for a person skilled in the art, it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.