CN1498921A - Usage of indophenol salt in direct dyeing in situ - Google Patents
Usage of indophenol salt in direct dyeing in situ Download PDFInfo
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- CN1498921A CN1498921A CNA021573980A CN02157398A CN1498921A CN 1498921 A CN1498921 A CN 1498921A CN A021573980 A CNA021573980 A CN A021573980A CN 02157398 A CN02157398 A CN 02157398A CN 1498921 A CN1498921 A CN 1498921A
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Abstract
An application of 3-indolol salt instead of indigo and indigo white in direct in-situ dyeing of fabric and the process for preparing said 3-indolol salt are disclosed. Its advantages are simplified process and high utilization rate of equipment.
Description
(1) technical field
The present invention relates to a kind of in-situ oxidation and become indigo direct 3-indoles phenates dyeing textiles, the preparation method of this indoles phenates, and this indoles phenates is oxidized to indigo directly to the purposes on the dyeing textiles in position.
(2) background technology
Indigo is a kind of vat dyes, and it is used for the textile materials of cellulose, especially the dyeing of the cotton warp yarns of blue jeans's cloth products.
How to prepare indigo at present (referring to JP-B-2024817, DE-A-2643877) via the oxidation of 3-indoles phenates.React down at 220-250 ℃ comprising mixed base by anilino-acetate, sodium amide and sodium hydroxide and potassium hydroxide, obtain containing the melts (hereinafter to be referred as the alkali fusion thing) of the 3-indoles phenates of 24-30%, this alkali is melted thing put into big water gaging (4-6 doubly), blowing air is oxidized to, and again through press filtration, washing (comprises pickling, alkali cleaning, washing), drying, granulation obtains indigo.Indigo water insoluble, in dyeing course, it is indigo white earlier it to be reduced into water miscible leuco compound, on dye wait to dye on the material after, indigo whitely be reoxidised into indigo and colour developing again.For example US-A-4283198 has reported the method for being printed and dyed by indigo white oxidation.In the pre-treatment, with a large amount of vat powders and alkaline solution add indigo in, make indigo reduction become indigo white, in the textile dyeing process, add air make as oxygenant indigo white salt be oxidized to indigo finish painted.
Indigo reduction process needs a large amount of vat powder and alkali (indigo: vat powder: alkali (w/w/w)=1: 1.6: 1.1).At present, printing and dyeing mill all adopts continuous multiple-grooved (general 6-8 groove) dyeing, the intermittence of groove and groove indigo white being oxidized to dye on the fabric on indigo, but after entering next groove, on dye indigo on the fabric and be reduced once more, so repeat 6-8 time, the consumption of alkali and vat powder is further increased, the amount of alkali in the waste water, vitriol sulphite is increased.
In the prior art, the indigo existence in dyeing course repeats redox, and step is many and complicated, also will use a large amount of potassium hydroxide, sodium hydroxide and vat powder.In addition, the recovery of potassium hydroxide and sodium hydroxide and re-using, and the processing of the vitriol of waste water middle and high concentration not only consumed energy but also water consumption, and pollute also big.
For this reason, people proposed multiple improvement way.For example, CN1120357A discloses a kind of dyeing process, adopts catalytic hydrogenation to prepare the indigo white aqueous solution, dye on the textile materials on indigo white after, be transformed into it indigo again with traditional atmospheric oxidation method.Though it is stable under the oxygen barrier condition that this method has the indigo white aqueous solution, can avoid indigotin to consume a large amount of reductive agent and alkali, produce the shortcoming of a large amount of waste water then, but, this method still needs earlier indigo reduction to be become could be used after indigo white, and cost is still very high, is not generally adopted as yet at present.CN1282816A has reported by 3-indolone or its tautomer in-situ oxidation and has become indigo, thus the method for direct printing.Point out in this patent application that one of the indigo reason that can not thoroughly permeate yarn is because indigo molecular structure causes more greatly, therefore selects for use indolone or its tautomer to carry out oxidising dyeing.But because the poor chemical stability of indolone or its tautomer indolol does not still have purifying process so far and develops, more do not have merchandise sales, therefore, this method is not seen application as yet yet.DE-A-2643877 discloses the method that continuous processing prepares indolol sodium.In the method, indolol sodium is as intermediate, directly is used for preparing indigo, but not mentioned or hint extracts the indoles phenates method of purification of more not mentioned indoles phenates in the literary composition from reactant.
(3) summary of the invention
[problem that will solve]
The objective of the invention is to seek the use new way of 3-indoles phenates on dyeing textiles, obtain a kind of preparation and be used for in-situ oxidation and become indigo directly to the method for the 3-indoles phenates of dyeing textiles.
[technical scheme]
At the deficiencies in the prior art, the inventor has carried out intensive research.Found that: will prepare indigo intermediate 3-indoles phenates can crystallize out under certain solvent water yield and temperature condition, whereby can separation and purification, and further find that original position is oxidized to indigo in the textile dyeing process and be a kind of feasible and effective ways directly, finished the present invention on this basis textile dyeing.
The invention provides a kind of in-situ oxidation and become indigo direct 3-indoles phenates dyeing textiles.
The present invention also provides a kind of and has been used for in-situ oxidation from 3-indoles phenates crude product preparation and becomes indigo directly to the method for the 3-indoles phenates of dyeing textiles, and this method may further comprise the steps:
A) add weight and be equivalent to the solvent that 3-indoles phenates crude product 1-5 doubly measures, add in the process of solvent, solution temperature is controlled at 80-100 ℃, preferably be controlled at 90-100 ℃.
B) solution with step a) is cooled to-10 to 50 ℃, makes the crystallization of indoles phenates.The crystal of gained is stirred, and suction filtration obtains the indoles phenates crystallization with crystal water, isolates this crystallization, dehydrates then, packs.
In above method, wherein said solvent is de-oxygenised water, deoxidation methyl alcohol, deoxidation ethanol or their solution.Preferred solvent is a de-oxygenised water.The preferred Tc of wherein said crystalline is 20-40 ℃.
The present invention also provides a kind of 3-indoles phenates to be oxidized in position indigoly to it is characterized in that directly to the purposes on the dyeing textiles, 3-indoles phenates is directly put in the dye liquor, make its in-situ oxidation become indigo, thereby directly to dyeing textiles.
Said 3-indoles phenates comprises 3-indolol potassium or 3-indolol sodium or their both mixtures, preferably both mixtures among the present invention.Both are mixed, and there is no particular limitation for the ratio of two kinds of salt.
The 3-indoles phenates crude product that adopts among the present invention can be by the method preparation of routine, for example, adopt the mixed base of anilino-acetate, sodium amide and sodium hydroxide and potassium hydroxide to react the alkali fusion thing that obtains containing 3-indoles phenates 24-35% (W%) down at 220-250 ℃.This alkali fusion thing can direct oxidation prepare indigo, referring to JP-B-2024817, DE-A-2643877.The 3-indoles phenates that adopts among the present invention can also be by the alkali neutralization reaction preparation of 3-indolol.
The 3-indoles phenates that obtains with method purifying of the present invention also can be used to prepare indigo, and can be used to prepare high-quality indigo.The 3-indoles phenates that the inventor obtains with method purifying of the present invention is that the indigo various indexs of indigo and standard of principle preparation fit like a glove.
With dyeing textiles the time, can adopt following embodiment when adopting method direct printing of the present invention:
1. yarn carries out pre-wash by prewashing equipment.
2. the dyeing installation formed by the groove that all contains of the indolol salts solution or several polyphones of yarn dyes to it, and from a groove to the stroke of another groove, carry out oxidizing reaction in the air by yarn is exposed to, make the indoles phenates change into indigo and be able to yarn is dyeed.
3. the yarn after the dyeing washs with predrying it by a series of washing and predrying equipment.
4. yarn carries out starching by the device for sizing that contains groove, so that form transparent film on yarn fibers.
5. yarn carries out drying by the drying plant that contains roller.
6. yarn is collected warp thread by reel.
In the method for the invention, when adopting 3-indolol salt dyeing,, therefore, before yarn on the dye liquor, must prevent its oxidation because it is easy to oxidation.
In actual production process, on the one hand for to overcome the defective that 3-indoles phenates is easy to oxidation, consider user's possible needs and easy to use on the other hand, it is a kind of valid approach that 3-indoles phenates and vat powder and/or alkali are made up.Weight ratio in the composition of the present invention between 3-indoles phenates, vat powder and/or alkali can be decided as required, but generally can these components be mixed according to the weight ratio that adopts in the dyeing method of the present invention, with user-friendly.For example, when composition of the present invention comprised 3-indoles phenates, vat powder and/or alkali, its weight ratio was a 3-indoles phenates: vat powder: alkali=1: 0: 0.1-1.0 or 1: 0.1-1.0: 0 or 1: 0.1-1.0: 0.1-1.0.In dyeing course, in dye liquor, add a spot of vat powder and/or sodium hydroxide, its role is to the oxygen that oxygen in the reductive water and yarn are brought into, can guarantee the stability of dye liquor.
In the method for the present invention; dyeing course preferably uses rare gas element (preferably the rare gas element that uses is nitrogen) protection and uses fluidizing air and warm air blowoff fabric; help promote the oxidation and improve coloring effect; reduce dye vat; and secluding air; prevent the dye liquor oxidation, reduce, even need not use vat powder and alkali.
In specific embodiment,, can realize by for example following method in order to guarantee the stability of dye liquor:
(1) hydromining de-oxygenised water that dye liquor is used, and staining bath is accomplished almost airtight, the dye liquor surface covers with rare gas elementes such as nitrogen, makes slightly malleation of system, and air can not enter, and keeps stable thereby dye liquor is not oxidized.And indoles phenates itself just has certain alkali, and in order to guarantee its stability, it is necessary containing a certain amount of alkali, and like this, dye liquor directly adds above-mentioned composition, thereby just directly dyeing and finishing reduces the dyeing and finishing cost, realizes green printing and dyeing.
(2) as staining bath is not changed, adopt existing installation, then only need in dye liquor, add a spot of vat powder and/or sodium hydroxide, its effect only is the oxygen that oxygen in the reductive water and yarn are brought into, with the stability of assurance dye liquor.
[beneficial effect]
The present invention changes into indigo repetition redox process with indoles phenates in the traditional technology and is reduced to a step.Simplify operation thus, saved repeatedly alkali and vat powder that the redox process is consumed, saved manpower and materials, thereby improved plant factor, reduced cost, helped environment protection and market competition.Particularly, the present invention has following superiority:
1. adopt cloth specimen color and luster that the indoles phenates with indigo a great deal of dyed and indigo quite and the cloth specimen infiltration is more even, dyeing time shortens half when more indigo than use.The present invention is directly used in in-situ oxidation dyeing with 3-indoles phenates, improve in staining bath oxidation and pre-caustic dip stage, thereby the absorption and the dipping ability of yarn have been improved, can not only reach and the existing suitable Color of indigo intensity, and the cloth specimen infiltration is more even, and dyeing time shortens half when more indigo than use.Also can obtain coloured light (ruddiness head) effect after fabric coloured light (green glow head) is different from indigo dyeing with 3-indoles phenates in-situ oxidation dyeing.In dyeing course, pass through the consumption of control 3-indoles phenates, dyeing time and other processing parameter can be realized painted (surface colour is to the complete imbue) of different depths, and during indigo dyeing because indigo molecule is bigger, can not be in the short period of time imbue fully.3-indoles phenates is a kind of eco-friendly leuco compound, can replace cotton warp yarns line and other coloration of textile materials of the indigo indigo white blue jeans's of being used for cloth products.
2. stablize dye liquor if adopt take a policy powder and sodium hydroxide, by conventional now printing and dyeing proportioning, indigo: vat powder: sodium hydroxide=1.0: 1.6: 1.1 (W: W: W) meter, adopt the inventive method, use 3-indoles phenates can save vat powder and/or sodium hydroxide greatly, even do not use vat powder or/or sodium hydroxide.Method of the present invention has changed to utilize indigoly carries out painted routine operation mode to yarn, especially significantly reduced the indigo synthetic number of times that repeats redox (6-8 time) when dyeing that reaches, and the sodium hydroxide of corresponding consumption, vat powder and other additive, thereby reduced labour intensity, and significantly reduced the dyeing cost, founded friendly process.
3. the present invention is by providing the method for the alkali fusion thing in the indigo production process being separated purification 3-indoles phenates; and 3-indolol product salt is carried out in-situ oxidation to textile materials at normal temperatures dye; realized cleaning industrial production; and all alkali lye in the whole sepn process are all recyclable; therefore the wastewater treatment capacity of having avoided a large amount of use vat powder and sodium hydroxide to be produced helps protecting environment.
4. the indoles phenates is little more many than indigo molecule, and this has increased its perviousness, can accelerate dyeing kinetics, reduces the dyeing number of times, shortens dyeing time, makes on the fiber that is colored white core very little or white core phenomenon can occur hardly.Thereby eliminate because the fabric that fading due to the washing caused wears out.
5. adopt method of the present invention to obtain highly purified indoles phenates and only need on former indigo production system, to increase seldom equipment, do not change former system and produced.
6. adopt method of the present invention that the indoles phenates is proposed in the alkali of high density, remove water a large amount of in the low concentration alkali, help saving energy and reduce the cost thereby needn't consume lot of energy when alkali is reclaimed.
CN1282816A has introduced with 3-indolone painted method, the present invention by comparison, superiority is:
(1) preparation of 3-indoles phenates is to carry out on the basis of former indigo technology, less investment, and instant effect can be realized suitability for industrialized production.The preparation of 3-indolone is then comparatively loaded down with trivial details, not only will pass through the preparation process of 3-indoles phenates, but also will convert it into indolone, this not only wants consumption acids, and technology controlling and process is also relatively more difficult, is not easy to realize industrial production, thereby has limited its application.
(2) the 3-indolone time need consume sodium hydroxide in printing and dyeing and uses it to be converted into 3-indoles phenates, and this increases operation, and increased the printing and dyeing cost not only around a circle.
In addition, the needs that prior art is not purified the indoles phenates, therefore, nobody proposes the method for purification of this salt, more nobody mentions it is directly acted on fabric, it is indigo that in-situ oxidation becomes, and fabric is carried out painted methods and applications, and therefore of the present invention finishing has important academic significance to the dyeing textiles field.
(4) description of drawings
Fig. 1 is the 3-indoles phenates of purifying
13C NMR spectrogram.
Fig. 2, the 3rd, indigo infrared spectrogram.
(5) embodiment
Further specify the present invention with non-limiting example below.
Embodiment 1: purifying 3-indoles phenates (3-indolol sodium and 3-indolol potassium)
In the Erlenmeyer flask with 250 milliliters of 25 gram 3-indoles phenates crude products (25%) addings, add 40 milliliters of de-oxygenised waters, make it 90 ℃ of dissolvings down, be cooled to 40 ℃, suction filtration is stirred in crystallization, get 13.83 gram filter cakes, dehydrate then, its 3-indoles phenates (containing crystal water) content is 82% by analysis.
Embodiment 2: purifying 3-indolol sodium
In the Erlenmeyer flask with 250 milliliters of 25 gram 3-indolol sodium crude products (24%) addings, add 25 milliliters of de-oxygenised waters, make it 100 ℃ of dissolvings down, be cooled to 50 ℃, suction filtration is stirred in crystallization, get 11.80 gram filter cakes, dehydrate then, its 3-indoles phenates (containing crystal water) content is 80% by analysis.
Embodiment 3: purifying 3-indolol potassium
In the Erlenmeyer flask with 250 milliliters of 25 gram 3-indolol potassium crude products (28%) addings, add 125 milliliters of de-oxygenised waters, make it 80 ℃ of dissolvings down, be cooled to 20 ℃, suction filtration is stirred in crystallization, get 14.30 gram filter cakes, dehydrate then, its 3-indoles phenates (containing crystal water) content is 81% by analysis.
Embodiment 4: purifying 3-indoles phenates (3-indolol sodium and 3-indolol potassium)
In the Erlenmeyer flask with 250 milliliters of 25 gram 3-indoles phenates crude products (25%) addings, add 40 milliliters of deoxidation methyl alcohol, make it 90 ℃ of dissolvings down, be cooled to-10 ℃, suction filtration is stirred in crystallization, get 14.55 gram filter cakes, dehydrate then, its 3-indoles phenates (containing crystal water) content is 79% by analysis.
Embodiment 5: purifying 3-indoles phenates (3-indolol sodium and 3-indolol potassium)
In the Erlenmeyer flask with 250 milliliters of 25 gram 3-indoles phenates crude products (25%) addings, add 40 milliliters of deoxidation ethanol, make it 90 ℃ of dissolvings down, be cooled to-10 ℃, suction filtration is stirred in crystallization, get 13.25 gram filter cakes, dehydrate then, its 3-indoles phenates (containing crystal water) content is 78% by analysis.
Embodiment 6: purifying 3-indoles phenates (3-indolol sodium and 3-indolol potassium)
With 3-indoles phenates 13.83 grams of embodiment 1, add 6 milliliters de-oxygenised water again, 40-80 ℃ of dissolving down, be cooled to room temperature then, crystallization, suction filtration gets 5.55 gram filter cakes, and it is 92% that oven dry records its content.
Embodiment 7: structure and the rerum natura of determining 3-indoles phenates
The 3-indoles phenates of the purification of embodiment 6 is used
13C NMR carries out structure and determines, has confirmed that gained is the 3-indolol.Referring to accompanying drawing 1.
The basic physical properties of 3-indoles phenates is as follows: outward appearance: blackish green to golden yellow solid; Content (containing crystal water): 80-92%; Basicity: 5-15%; Moisture: 3-5%; If the band crystal water, not drying then, content is: 40-45%, basicity: 5-10%, moisture: 40-45%.Thermostability: 45 ℃ store transportation down; Solubleness (25 ℃): 30g/100ml water.
Embodiment 8: draw a design with 3-indoles phenates
In 500 milliliters beaker, add 2 milliliters of 95% ethanol, 10% draw back 2 milliliters in powder, vat powder 0.5 gram, sodium hydroxide 0.5 gram, 10% 40 milliliters in sodium sulfate, 360 milliliters in water.3-indoles phenates 1.09 grams (pure about 1 gram) that under nitrogen protection, add embodiment 6 then.Under 25-30 ℃, 10 gram sample cloth were contaminated 45 minutes.Taking-up oxidation 30 minutes in air, water and 2% acetic acid solution washing then.Be washed with water to neutrality again, dry, cloth specimen intensity is with suitable by the cloth specimen intensity of indigo dyeing, and coloured light is green head.
Embodiment 9: draw a design with 3-indoles phenates
In 500 milliliters beaker, add 2 milliliters of 95% ethanol, 10% draw back 2 milliliters in powder, vat powder 0.5 gram, 10% 40 milliliters in sodium sulfate, 360 milliliters in water.3-indoles phenates 1.09 grams (pure about 1 gram) that add embodiment 6 then.Under 25-30 ℃, 10 gram sample cloth were contaminated 45 minutes.Taking-up oxidation 30 minutes in air, water and 2% acetic acid solution washing then.Be washed with water to neutrality again, dry, cloth specimen intensity is with suitable by the cloth specimen intensity of indigo dyeing, and coloured light is green head.
Embodiment 10: draw a design with 3-indoles phenates
In 500 milliliters beaker, add 2 milliliters of 95% ethanol, 10% draw back 2 milliliters in powder, sodium hydroxide 0.5 gram, 10% 40 milliliters in sodium sulfate, 360 milliliters in water.3-indoles phenates 1.09 grams (pure about 1 gram) that under nitrogen protection, add embodiment 6 then.Under 25-30 ℃, 10 gram sample cloth were contaminated 45 minutes.Taking-up oxidation 30 minutes in air, water and 2% acetic acid solution washing then.Be washed with water to neutrality again, dry, cloth specimen intensity is with suitable by the cloth specimen intensity of indigo dyeing, and coloured light is green head.
Embodiment 11: draw a design with 3-indoles phenates
In 500 milliliters beaker, add 2 milliliters of 95% ethanol, 10% draw back 2 milliliters in powder, vat powder 0.1 gram, sodium hydroxide 1.5 grams, 10% 40 milliliters in sodium sulfate, 360 milliliters in water.3-indoles phenates 1.09 grams (pure about 1 gram) that under nitrogen protection, add embodiment 6 then.Under 25-30 ℃, 10 gram sample cloth were contaminated 45 minutes.Taking-up oxidation 30 minutes in air, water and 2% acetic acid solution washing then.Be washed with water to neutrality again, dry, cloth specimen intensity is with suitable by the cloth specimen intensity of indigo dyeing, and coloured light is green head.
Embodiment 12: draw a design with 3-indoles phenates
In 500 milliliters beaker, add 2 milliliters of 95% ethanol, 10% draw back 2 milliliters in powder, vat powder 1 gram, sodium hydroxide 0.1 gram, 10% 40 milliliters in sodium sulfate, 360 milliliters in water.3-indoles phenates 1.09 grams (pure about 1 gram) that add embodiment 6 then.Under 25-30 ℃, 30 gram sample cloth were contaminated 45 minutes.Taking-up oxidation 30 minutes in air, water and 2% acetic acid solution washing then.Be washed with water to neutrality again, dry, cloth specimen intensity is with suitable by the cloth specimen intensity of indigo dyeing, and coloured light is green head.
Embodiment 13: draw a design with 3-indoles phenates
In 500 milliliters beaker, add 2 milliliters of 95% ethanol, 10% draw back 2 milliliters in powder, vat powder 0.5 gram, sodium hydroxide 0.5 gram, 10% 40 milliliters in sodium sulfate, 360 milliliters in water.3-indoles phenates 1.28 grams (pure about 1 gram) that under nitrogen protection, add embodiment 5 then.Under 25-30 ℃, 50 gram sample cloth were contaminated 45 minutes.Taking-up oxidation 30 minutes in air, water and 2% acetic acid solution washing then.Be washed with water to neutrality again, dry, cloth specimen intensity is with suitable by the cloth specimen intensity of indigo dyeing, and coloured light is green head.
Embodiment 14: draw a design with 3-indolol sodium
In 500 milliliters beaker, add 2 milliliters of 95% ethanol, 10% draw back 2 milliliters in powder, vat powder 0.5 gram, sodium hydroxide 0.5 gram, 10% 40 milliliters in sodium sulfate, 360 milliliters in water.3-indoles phenates 1.25 grams (pure about 1 gram) that under nitrogen protection, add embodiment 2 then.Under 25-30 ℃, 10 gram sample cloth were contaminated 45 minutes.Taking-up oxidation 30 minutes in air, water and 2% acetic acid solution washing then.Be washed with water to neutrality again, dry, cloth specimen intensity is with suitable by the cloth specimen intensity of indigo dyeing, and coloured light is green head.
Embodiment 15: draw a design with 3-indolol potassium
In 500 milliliters beaker, add 2 milliliters of 95% ethanol, 10% draw back 2 milliliters in powder, vat powder 0.5 gram, sodium hydroxide 0.5 gram, 10% 40 milliliters in sodium sulfate, 360 milliliters in water.3-indolol potassium 1.23 grams (pure about 1 gram) that under nitrogen protection, add embodiment 3 then.Under 25-30 ℃, 10 gram sample cloth were contaminated 45 minutes.Taking-up oxidation 30 minutes in air, water and 2% acetic acid solution washing then.Be washed with water to neutrality again, dry, cloth specimen intensity is with suitable by the cloth specimen intensity of indigo dyeing, and coloured light is green head.
Embodiment 16: prepare indigo from 3-indoles phenates
The 3-indoles phenates oxidation that embodiment 6 is purified is prepared into indigo, the indigo content about 94% that obtains, and what its reductibility and existing method obtained is indigo suitable.Its infrared spectrogram and existing method obtain indigo compare in full accord.Referring to accompanying drawing 2 and 3.
The comparative example 1: draw a design with indigo
In 500 milliliters beaker, add 2 milliliters of 95% ethanol, 10% draw back 2 milliliters in powder, vat powder 1.6 grams, sodium hydroxide 1.1 grams, 10% 40 milliliters in sodium sulfate, 360 milliliters in water.Indigo 1.06 grams (pure about 1 gram) that under nitrogen protection, add embodiment 25 then.Under 25-30 ℃, 10 gram sample cloth were contaminated 45 minutes.Taking-up oxidation 30 minutes in air, water and 2% acetic acid solution washing then.Be washed with water to neutrality again, dry, coloured light is green head.
The comparative example 2: draw a design with indigo
In 500 milliliters beaker, add 2 milliliters of 95% ethanol, 10% draw back 2 milliliters in powder, vat powder 0.5 gram, sodium hydroxide 0.5 gram, 10% 40 milliliters in sodium sulfate, 360 milliliters in water.Indigo 1.06 grams (pure about 1 gram) that under nitrogen protection, add embodiment 25 then.Under 25-30 ℃, 10 gram sample cloth were contaminated 45 minutes.Taking-up oxidation 30 minutes in air, water and 2% acetic acid solution washing then.Be washed with water to neutrality again, dry, dyeing flower, surface luster obfuscation, coloured light obfuscation, Bai Xin.
Claims (9)
1. an in-situ oxidation becomes indigo direct 3-indoles phenates to dyeing textiles.
2. according to the 3-indoles phenates of claim 1, this salt is 3-indolol potassium and/or 3-indolol sodium.
3. one kind is used for in-situ oxidation from 3-indoles phenates crude product preparation and becomes indigo directly to the method for the 3-indoles phenates of dyeing textiles, and this method may further comprise the steps:
A) in 3-indoles phenates crude product, add weight and be equivalent to the solvent that this crude product 1-5 doubly measures, add in the process of solvent, solution temperature is controlled at 80-100 ℃.
B) solution with step a) is cooled to-10 ℃ to 50 ℃, and crystallization and fractional crystallization dehydrate then.
4. according to the method for claim 3, wherein said solvent is de-oxygenised water, deoxidation methyl alcohol, deoxidation ethanol or their solution.
5. according to the method for claim 4, wherein said solvent is a de-oxygenised water.
6. according to arbitrary method of claim 3-5, wherein said crystalline Tc is 20-40 ℃.
7. according to arbitrary method of claim 3-6, wherein said 3-indoles phenates is 3-indolol sodium and/or 3-indolol potassium.
8. a 3-indoles phenates is oxidized in position and indigoly it is characterized in that directly to the purposes on the dyeing textiles, and 3-indoles phenates is directly put in the dye liquor, makes its in-situ oxidation become indigo, thereby directly to dyeing textiles.
9. purposes according to Claim 8, wherein said 3-indoles phenates is 3-indolol potassium and/or 3-indolol sodium.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02157398 CN1204202C (en) | 2002-11-11 | 2002-12-25 | Usage of indophenol salt in direct dyeing in situ |
| PCT/CN2003/001057 WO2004058898A1 (en) | 2002-12-25 | 2003-12-12 | A process for dyeing directly a textile fabric in situ |
| AU2003289648A AU2003289648A1 (en) | 2002-12-25 | 2003-12-12 | A process for dyeing directly a textile fabric in situ |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN02149258.1 | 2002-11-11 | ||
| CN02149258 | 2002-11-11 | ||
| CN 02157398 CN1204202C (en) | 2002-11-11 | 2002-12-25 | Usage of indophenol salt in direct dyeing in situ |
Publications (2)
| Publication Number | Publication Date |
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| CN1498921A true CN1498921A (en) | 2004-05-26 |
| CN1204202C CN1204202C (en) | 2005-06-01 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 02157398 Expired - Fee Related CN1204202C (en) | 2002-11-11 | 2002-12-25 | Usage of indophenol salt in direct dyeing in situ |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102046875B (en) * | 2008-06-09 | 2012-10-17 | 德司达染料德国有限责任公司 | Dyeing warp yarns with leucoindigo foam |
| CN113969508A (en) * | 2021-11-30 | 2022-01-25 | 韶关市北纺智造科技有限公司 | Method for dyeing yarn |
-
2002
- 2002-12-25 CN CN 02157398 patent/CN1204202C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102046875B (en) * | 2008-06-09 | 2012-10-17 | 德司达染料德国有限责任公司 | Dyeing warp yarns with leucoindigo foam |
| CN113969508A (en) * | 2021-11-30 | 2022-01-25 | 韶关市北纺智造科技有限公司 | Method for dyeing yarn |
| CN113969508B (en) * | 2021-11-30 | 2024-03-22 | 韶关市北纺智造科技有限公司 | Yarn dyeing method |
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| Publication number | Publication date |
|---|---|
| CN1204202C (en) | 2005-06-01 |
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