CN107217499A - A kind of combined oxidation acid and its application method for sulfur dyeing - Google Patents
A kind of combined oxidation acid and its application method for sulfur dyeing Download PDFInfo
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- CN107217499A CN107217499A CN201710582479.8A CN201710582479A CN107217499A CN 107217499 A CN107217499 A CN 107217499A CN 201710582479 A CN201710582479 A CN 201710582479A CN 107217499 A CN107217499 A CN 107217499A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General 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
- D06P1/30—General 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 sulfur dyes
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General 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
- D06P1/44—General 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 insoluble pigments or auxiliary substances, e.g. binders
- D06P1/62—General 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 insoluble pigments or auxiliary substances, e.g. binders using compositions containing low-molecular-weight organic compounds with sulfate, sulfonate, sulfenic or sulfinic groups
- D06P1/628—Compounds containing nitrogen
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/58—Material containing hydroxyl groups
- D06P3/60—Natural or regenerated cellulose
- D06P3/6025—Natural or regenerated cellulose using vat or sulfur dyes
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
- D06P5/02—After-treatment
- D06P5/04—After-treatment with organic compounds
- D06P5/06—After-treatment with organic compounds containing nitrogen
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- Textile Engineering (AREA)
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Abstract
Textile dyeing field of the present invention, specifically related to a kind of combined oxidation acid and its application method for sulfur dyeing, by sulfamic acid and the acid composition combined oxidation acid with pH cushioning effects, the subsequent oxidation process after contaminating is reduced for sulfur dye, make sulfur dye leuco compound fully oxidized, color depth and color-light stability are improved, the problem of solving environmental pollution or the not enough oxidability that conventional oxidant is present.Weight part ratio of the sulfamic acid in combined oxidation acid is 0.01~100, combined oxidation acid is configured to the oxidation solution of 5~10g/L containing sulfamic acid when in use, fabric after dyeing impregnates 5s~3min in oxidation acid solution, and the control of oxidation acid liquor temperature is in room temperature between 75 DEG C.
Description
Technical field
The invention belongs to textile dyeing field, and in particular to a kind of combined oxidation acid for sulfur dyeing and its
Application method.
Background technology
Sulfur dye is one of primary dye in cellulose dyeing application, Year's consumption come reactive dye it
Afterwards, second is occupied.Sulfur dye is cheap, Exposure to Sunlight and washing fastness good, strong applicability, does not contain azo group, heavy metal
And Adsorbable organic halogens, no anaphylaxis and carcinogenicity, it is considered to be a kind of non-toxic dye, it is the deep-colour fabric dye such as blue, black
The most important dyestuff of color.
Sulfur dye is water insoluble in itself, it is impossible to above contaminate fiber, needs addition reducing agent to be reduced into and fibre during dyeing
Dimension has the water-soluble form (leuco compound) of affinity, and sulfur dye needs to be oxidized to from leuco compound insoluble in dyeing course
Color lake is deposited on fiber, could obtain excellent dyefastness.
All the time, sulfur dyeing generally uses vulcanized sodium as reducing agent, except that can be washed with water after upper dye
Outside wind oxidation technology, maximally effective oxidation technology is to use bichromate (red sulfone) always in the past, but due to the toxicity of Cr VI,
It is big to environmental protection harm, so various countries chemist competitively studies new oxidant and oxidation technology in recent years.Mainly there is (1) bromine
Sour sodium+acetic acid+catalyst (such as sodium metavanadate, NaVO3), pH value is 4~4.5,70 DEG C；(2) hydrogen peroxide, acidic oxidation (plus second
Acid), pH value is 4~4.5,70 DEG C；(3) hydrogen peroxide, alkaline oxygenated (plus soda ash), pH value is 10,40 DEG C；(4) Potassiumiodate+second
Acid, pH value is 4~4.5,70 DEG C；(5) sodium chlorite, pH value is 10,98 DEG C；(6) sodium chlorate, pH value is 4~4.5,70 DEG C；
(7) sodium perborate, 60 DEG C；(8) toluene-sodium-sulfonchloramide, pH value is 10,60~70 DEG C.
From several index comprehensive analyses such as color yield, wet fastness, environmental protection, cost, preceding 3 kinds of oxidants and its technique are more
With Practical significance.(1) is planted method and approached with arsenic technological effect, coloured light is not interfered with, particularly with more dysoxidizable sulphur
Change is reddish brown, after catalyst is added, also can smoothly aoxidize；(2) plant method washing be with the more other methods of staining fastness
It is excellent；(3) are planted after method oxidation, and pure color, cost is low, but staining fastness is slightly poor, and peroxide passivation still has oxidation whard to control
Shortcoming；(4) kind method oxidation effectiveness is good, but price is higher, influence actual use；(5) plant method to (8) and plant method
All it is difficult to consider actual use because of factors such as environmental protection or costs.In fact, being made using the compound containing halogen (bromine, iodine, chlorine)
Oxidant, although solve chromium evil problem, but AOX values (absorbable organohalogen compounds content) to environmental protection still not
Profit.General sulphur black dyeing, it is not necessary to oxidation trough is specially set, air oxidation is directly utilized.Such as carry out colored sulfur dye dye
During color, then need specially to set oxidation trough, using oxidizing.Can generally hydrogen peroxide be used to be aoxidized in pH value for 4.5 times,
But hydrogen peroxide is not sufficiently stable, control is difficult, while not enough to some colors (as red) oxidation effectiveness, it is impossible to fine color development.This
The oxidant that Shi Zexu selects some special is aoxidized, such as using Diresul Oxidant BRI (liquid).Some scholars adopt
With ammonium persulfate as oxidant, the discoloration problem of sulphur red brown is reduced, but have release free radical during ammonium persulfate use
Cause the danger of fabric damage.
Due to the pressure of environmental protection, traditional reducing agent vulcanized sodium and its colouring method can not meet the need of clean manufacturing
Will, replace vulcanized sodium to be using the reducing agent of environmentally safe (no sulphur or low-sulfur) to reduce in pollution, dyeing course
Most important approach.In the work that research staff did, being used to substitute the reducing agent of vulcanized sodium includes reduced sugar, dioxy
Change thiocarbamide, beta -mercaptoethanol etc..Recuding sugars includes pectinose, fructose, galactolipin, glucose, lactose and maltose etc., this
After being contaminated on class reducing agent, using hydrogen peroxide as oxidant, because oxidability is weak, it is impossible to make leuco dye fully oxidized,
Cause tinctorial yield low, coloured light is not pure enough, it is long-term to place the problems such as coloured light changes, it is impossible to meet production needs.Need out
Send out novel environment-friendly oxidant a kind of, meet production needs.
The content of the invention
The present invention provides a kind of combined oxidation acid and its application method for sulfur dyeing, by sulfamic acid and one
Organic or inorganic acid of the series with cushioning effect is constituted, and by using combined oxidation acid, is made leuco dye fully oxidized, is carried
High dye level and colour stability.The problem of solving environmental pollution or the not enough oxidability that conventional oxidant is present.
The present invention is achieved using following technical scheme：
A kind of combined oxidation acid for sulfur dyeing in the present invention, combined oxidation acid include sulfamic acid and
Buffering acid, the buffering acid is with pH cushioning effects carboxyl or phosphate acid.
It is preferred that, a kind of described combined oxidation for sulfur dyeing is sour, and the carboxylic buffering acid is first
Acid, acetic acid, propionic acid, butyric acid, octanoic acid, adipic acid, ethanedioic acid, malonic acid, succinic acid, maleic acid, tartaric acid, benzoic acid, benzene second
Acid, phthalic acid, terephthalic acid (TPA), valeric acid, caproic acid, capric acid, stearic acid, palmitic acid, acrylic acid, amion acetic acid, citric acid
In one kind.
It is preferred that, a kind of described combined oxidation acid for sulfur dyeing, the buffering acid be formic acid, acetic acid,
One kind in amion acetic acid, citric acid.
It is preferred that, a kind of described combined oxidation for sulfur dyeing is sour, and the phosphate buffering acid is phosphoric acid
And ackd salt, 1-hydroxy ethylidene-1,1-diphosphonic acid and its sodium salt and sylvite, ATMP and its sodium salt and sylvite, ethylenediamine tetramethyl
Pitch phosphonic acids and its sodium salt and sylvite, diethylene triamine pentamethylene phosphonic and its sodium salt and sylvite.
It is preferred that, a kind of described combined oxidation for sulfur dyeing is sour, and described phosphate buffering acid is phosphorus
One kind in acid, 1-hydroxy ethylidene-1,1-diphosphonic acid, ATMP.
It is preferred that, a kind of described combined oxidation for sulfur dyeing is sour, each component in the combined oxidation acid
It is by weight：
Sulfamic acid：0.01~100.0
Buffering acid:0~99.9.
It is preferred that, each component is by weight in the combined oxidation acid：
Sulfamic acid：20.0~90.0
Buffering acid:10.0~80.0.
It is preferred that, each component is by weight in the combined oxidation acid：
Sulfamic acid：50.0~75.0
Buffering acid:25.0~50.0.
The application method of the above-mentioned combined oxidation acid for sulfur dyeing, comprises the following steps：
Combined oxidation acid solution is made in sulfamic acid and buffering acid by weight ratio, then combined oxidation acid solution is dilute
The oxidation solution of 0.01~30g/L Han effective sulfamic acid content is interpreted into, control oxidation solution is between 25~75 DEG C, after upper dye
Fabric is immersed in after oxidation solution 5s~3min, pressure rolling drying.
It is preferred that, the application method of the combined oxidation acid for sulfur dyeing, it is characterized in that the oxidation
The effective sulfamic acid content of liquid is 5~10g/L, and temperature is 25 DEG C, and dip time is 10~60s.
The present invention innovative point be：
1. using safety and the excellent sulfamic acid of environmental-protecting performance as the oxidant after sulfur dyeing, it both had
Certain acidity, can neutralize the alkalescence on fabric after dyeing, further through the oxidability of itself, leuco dye is aoxidized
Into insoluble color lake, it is attached on fabric.
2. by sulfamic acid and the acid composition combined oxidation acid with pH cushioning effects, with sulfamic acid is used alone
Compare, the dye level of fabric is further improved.
The present invention have the advantage that compared with prior art for：
The present invention in sulfur dye oxidation system by using sulfamic acid as oxidant, solve sodium bromate, iodine
Sour potassium, sodium chlorite, sodium chlorate, sodium perborate, the environmental issue that chloramines etc. is brought；Solve hydrogen peroxide easily to decompose, cause
Oxidizing process is difficult to control to, the problem of fabric color is unstable after oxidation；Sulfur dyeing is solved using recuding sugars thing
After matter on reducing agent as contaminating, compared with traditional reducing agent vulcanized sodium, it is difficult to aoxidize, because hydrogen peroxide oxidation ability is weak, no
Leuco dye can be made fully oxidized, cause tinctorial yield low, coloured light is not pure enough, it is long-term to place the problem of coloured light changes.
Embodiment
With reference to specific embodiment, the present invention is further illustrated.
Drift deviation pattern fabric (the grammes per square metre 135g/m of pure cotton half that present invention experiment is used2) it preferably is selected from Hebei Ning Fang groups.
The sulfur red brown b3r (100%) that present invention experiment is used, sulphur yellow 5G (100%), SULPHAR DYES BLUE BRN
(100%), the various dyestuffs such as sulphur bright green (100%) preferably are selected from Tianjin Mei Jietong Chemical Co., Ltd.s.ATMP
(ATMP) 1-hydroxy ethylidene-1,1-diphosphonic acid (HEDP) preferably is selected from Shandong Xin Tai water technologies limited company.Recuding sugars reducing agent
AS preferably is selected from Shijiazhuang Mei Shida biochemical industries Co., Ltd.Hydrogen peroxide (27.5%), acetic acid, formic acid, amion acetic acid, hydroxide
Sodium, soap flakes etc. are analysis pure chemistry reagent.
The method for experiment implement of the present invention is as follows：
1. aoxidize the preparation of acid solution：
In 250mL beakers, various acid, sodium hydroxides are added by ormal weight, are dissolved in water, and be settled to 100mL, matching somebody with somebody
The solution made constant temperature 30min in 25 DEG C of waters bath with thermostatic control, test oxidation-reduction potential and pH value.
2. the dyeing course of fabric
(1) consumption of dyestuff, reducing agent, sodium hydroxide and water needed for being calculated with total solution weight 200.0g.Measure
The running water of amount of calculation 70% is added in 250mL conical flask, is added after the sodium hydroxide of ormal weight, stirring and dissolving, is added
After reducing agent stirs, sulfur dye is added, 200.0g is weighed surely.It is put into 90 DEG C of constant temperature oscillation water-bath, reductase 12 0min.
(2) weight 10.0g pure cottons half are floated twill in the dye liquor dipping 30s reduced, took out padding machine, and controlled pick-up
80%, 30s is aoxidized in 200mL concentration is 5g/L oxidation solution, clear water is rinsed once, soap (soap flakes 2g/L, bath raio 1:
20,95 DEG C, 1min), dry rear colour examining.
The method of testing of the present invention is as follows：
(1) measure side of the oxidation-reduction potential (ORP) of solution with reference to professional standard SL94-1994 oxidation-reduction potentials
Method, the data inserted using not bright FLP201B oxidation-reduction potentiometers, recording electrode after solution 5min.
(2) pH value of solution is counted, recording electrode with reference to GB/T1717-1986 method of testing using thunder magnetic PHS-25pH
The data inserted after solution 5min.
(3) colour index of fabric is passed through frequently with selection in colour photometer data measured after the dyeing of Shade of Dyed Textiles index
K/S values under the chromaticity coordinates (L*, a*, b*) and maximum absorption wavelength surveyed under D65 light sources reflect.Under light source D65, L* tables
Degree of showing, numerical value is bigger, and color is brighter, otherwise darker；A* represents inclined feux rouges or inclined green glow, and numerical value is bigger, and color is redder, mutually reverse-biased
It is green；B* represents partially yellow or inclined blue light, on the occasion of Huang, and the bigger color of numerical value is more yellow, mutually reverse-biased indigo plant partially；It is deep that K/S represents padding
Degree, numerical value is bigger to represent that color is deeper, and tinctorial yield is big, otherwise K/S smaller, and color is more shallow, and tinctorial yield is small.Utilize Colori5-D
Color measurement and color match instrument, 10 ° of visual fields, D65Light source, is folded into 4 layers (light tight) by fabric after dye and is placed on colour examining hole, test fabric
L*, a*, b*, K/S value, 5 different points of every piece of fabric test, average.
Application example 1
1. the pH value and reduction potential of different proportion：
Sulfamic acid, ATMP (ATMP) and acetic acid are prepared 100mL solution according to the concentration of table 1, matching somebody with somebody
The solution made constant temperature 30min in 25 DEG C of waters bath with thermostatic control, test oxidation-reduction potential and pH value, the numerical value measured such as institute of table 2
Show.
Table 1.
| Sample number | Sulfamic acid/(g/L) | ATMP/(g/L) | Acetic acid/(g/L) | pH | Current potential/mv |
| 1 | 5 | 1.51 | 188 | ||
| 2 | 5 | 1.87 | -322 | ||
| 3 | 5 | 3.34 | -46 | ||
| 4 | 1.25 | 3.75 | 1.76 | -90 | |
| 5 | 1.25 | 3.75 | 2.07 | 50 | |
| 6 | 2.5 | 2.5 | 1.68 | -18 | |
| 7 | 2.5 | 2.5 | 1.75 | 117 | |
| 8 | 3.75 | 1.25 | 1.62 | 84 | |
| 9 | 3.75 | 1.25 | 1.50 | 149 | |
| 10 | 3.75 | 1.50 | 149 |
Found out by table 1, the oxidation-reduction potential of single sulfamic acid solution is on the occasion of that is, with oxidisability, thus can
To be used as oxidant, and the oxidation-reduction potential of other acid solutions is negative value, i.e., with reproducibility, it is impossible to separately as oxygen
Agent is used.Sulfamic acid is used in mixed way with ATMP, when weight part ratio is less than 1:When 1, current potential is negative, non-oxidative, works as weight
Part compares 3:When 1, current potential is just, mixed solution is provided with oxidisability.And mixed with acetic acid, when weight part ratio 1:3 start, and oxidation is also
Former current potential is on the occasion of with oxidisability, thus between the two percentage by weight of the sulfamic acid in acetic acid mixed solution is high
When 25%, mixed acid can be used as oxidant and use.
Due to needing to be carried out in stronger alkaline environment during being contaminated on sulfur dye, fabric enters oxidation after upper dye
A certain amount of alkali can be brought in liquid into, with the progress of processing, the alkali number brought into can gradually increase, and cause pH value liter in oxidation solution
Height, influences the oxidizing potential of oxidation solution, so as to cause the change of fabric color.In order to evaluate shock-absorbing capacity of the oxidation solution to alkali,
Sulfamic acid, ATMP, acetic acid and sodium hydroxide are prepared 100mL solution according to the concentration of table 2, the solution prepared at 25 DEG C
Constant temperature 30min in water bath with thermostatic control, test oxidation-reduction potential and pH value, the numerical value measured are as shown in table 2.
Table 2
| Sample number | Sulfamic acid/(g/L) | ATMP/(g/L) | Acetic acid/(g/L) | NaOH/(g/L) | pH | Current potential/mv |
| 1 | 5 | 2 | 10.13 | -41 | ||
| 2 | 5 | 2 | 6.84 | -126 | ||
| 3 | 5 | 2 | 4.69 | -130 | ||
| 5 | 1.25 | 2 | 13.32 | -81 | ||
| 6 | 1.25 | 3.75 | 2 | 6.62 | 20 | |
| 7 | 1.25 | 3.75 | 2 | 4.94 | 158 | |
| 9 | 2.5 | 2 | 13.06 | -84 | ||
| 10 | 2.5 | 2.5 | 2 | 6.38 | 32 | |
| 11 | 2.5 | 2.5 | 2 | 5.07 | 155 | |
| 13 | 3.75 | 2 | 12.33 | -10 | ||
| 14 | 3.75 | 1.25 | 2 | 6.65 | 22 | |
| 15 | 3.75 | 1.25 | 2 | 5.00 | 155 |
Table 2 is as can be seen that the buffer capacity of single sulfamic acid is very poor, and the weight ratio with sodium hydroxide is 2.5:When 1,
The pH value of 5g/L solution is that can reach 10.13, and current potential is negative, loses oxidisability.The buffer capacity of itself of ATMP and acetic acid compared with
Good, when ATMP and sulfamic acid percentage by weight are 25%~75%, the weight ratio of mixed acid and sodium hydroxide is 2.5:When 1,
PH is held between 6.38~6.84, with oxidisability, when acetic acid and sulfamic acid percentage by weight 25%~75% it
Between, the weight ratio of mixed acid and sodium hydroxide is 2.5:When 1, pH is held between 4.69~5.07, with excellent buffering
Ability and oxidisability.
Application example 2
The drift deviation line cloth specimen 5.0g of pure cotton half is cut, bath raio 1 is controlled:20, dyeing is prepared respectively by the raw material proportioning in table 3
Liquid, oxidation solution and soap boiling liquid, corresponding technological process are respectively A, B, C, D, and dyeing liquor shakes in 90 DEG C of waters bath with thermostatic control
20min, cloth specimen impregnates 1min in dye liquor, crosses padding machine, controls pick-up 80%, 30s is impregnated in oxidation solution, washes, soap boiling,
Dried in 80 DEG C of baking ovens.
Table 3.
In the technique that table 3 is listed, A, B is using akali sulphide as reducing agent, and oxidation solution is respectively adopted industrial at present common
Hydrogen peroxide 5g/L, acetic acid 5g/L and combined oxidation acid 5g/L (wherein 3.5g/L containing sulfamic acid and acetic acid 1.5g/L) .C, D adopt
With reducing agent AS as reducing agent, industrial common hydrogen peroxide 5g/L, acetic acid 5g/L at present is respectively adopted and compound in oxidation solution
Oxidizing acid 5g/L (wherein 3.5g/L containing sulfamic acid and acetic acid 1.5g/L), the sulfur dye of various different colours is surveyed after dyeing
The colour index obtained is shown in Table 4.
Table 4.
Note：K/S represents padding depth, and numerical value is bigger to represent that color is deeper, and tinctorial yield is big, otherwise K/S smaller, color
More shallow, tinctorial yield is small.
As can be seen from Table 4, A, B flow either using akali sulphide as reducing agent, or to be main by reduced sugar
The reducing agent AS of composition is above using hydrogen peroxide as C, D flow of reducing agent using the fabric K/S values after oxidation acid oxidase
Obtained by acetic acid oxidation, show that it aoxidizes color development ability and is dominant.
Cloth specimen after sulphur red brown is dyed is placed 4 weeks at lucifuge indoors, the colour index of test cloth specimen, obtained knot
Shown in fruit table 5.
Table 5.
Compared with the data after sulphur red brown dyeing in table 4, after placing 4 weeks, oxidant is used as using hydrogen peroxide and acetic acid
A, C, a of color, b value changes are larger, show that obvious change occurs for the coloured light of color, and use sulfamic acid and acetic acid to make
For the B of oxidant, D, a of color, b value changes are smaller, show that the coloured light of color is not changed significantly, color-light stability is good.
Application example 3
Using sulphur bright green as dyestuff, using with the identical colouring method of application example 2 and dyeing liquor, oxidation solution and soap boiling liquid
Proportioning, but oxidation solution temperature is separately positioned on 25 DEG C, 50 DEG C, 75 DEG C, its corresponding dyeing flow is respectively A1, A2, A3；
B1, B2, B3；C1, C2, C3；The colour index measured after D1, D2, D3. dyeing is shown in Table 6.
Table 6
| Dyeing flow | L | a | B | K/S |
| A1 | 20.82 | -14.03 | 0.78 | 31.6 |
| A2 | 21.56 | -14.07 | 0.54 | 31.5 |
| A3 | 21.68 | -14.96 | 0.61 | 29.0 |
| B1 | 20.73 | -13.91 | -0.14 | 33.0 |
| B2 | 20.82 | -14.01 | 0.06 | 31.5 |
| B3 | 21.03 | -14.35 | 0.31 | 31.4 |
| C1 | 23.65 | -16.40 | -1.00 | 29.0 |
| C2 | 23.35 | -15.90 | -1.40 | 28.8 |
| C3 | 25.05 | -17.62 | -2.03 | 26.2 |
| D1 | 21.25 | -12.69 | -0.60 | 29.0 |
| D2 | 21.41 | -13.09 | -0.71 | 28.2 |
| D3 | 21.61 | -12.91 | -0.56 | 27.8 |
As can be seen from Table 6, either which kind of technique, lifts the temperature of oxidation solution, and K/S is not lifted, slightly had on the contrary
Decline, at that same temperature, using the B of Compound-acid, D techniques are than the A using hydrogen peroxide and acetic acid, and C process colours are deep.
Application example 4
Sulfamic acid and acetic acid are pressed weight part ratio listed in table 7 respectively, 5g/L combined oxidation acid oxidase is configured to
Liquid.
Table 7
| Sequence number | 1# | 2# | 3# | 4# | 5 |
| Sulfamic acid | 1 | 25 | 50 | 75 | 100 |
| Acetic acid | 99 | 75 | 50 | 25 | 0 |
The drift deviation line cloth specimen 5.0g of pure cotton half is cut, bath raio 1 is controlled:20, by the red LGF 50g/L and akali sulphide 50g/L of vulcanization
Prepare dyeing liquor, soap flakes 1g/L and Na2CO3, 1g/L prepares soap boiling liquid.Dyeing liquor shakes 20min, cloth in 90 DEG C of waters bath with thermostatic control
Sample impregnates 1min in dye liquor, crosses padding machine, controls pick-up 80%, then the dipping in oxidation solution 1#, 2#, 3#, 4#, 5# respectively
30s, washing, soap boiling is dried in 80 DEG C of baking ovens, and the colour index of resulting dyed fabric is as shown in table 8.
Table 8
Found out by table 8, the small 1# of sulfamic acid accounting, the oxidability of oxidation solution is low, aoxidize color development scarce capacity, fabric
K/S values it is smaller.And individually use the 5# of sulfamic acid, K/S values are higher than 1#, but less than 2#, 3#, 4#, show sulfamic acid and
The weight percent accounting of acetic acid action effect between 25~75 is preferable.
Application example 5
Sulfamic acid and acetic acid are pressed weight part ratio listed in table 9 respectively, 5g/L combined oxidation acid oxidase is configured to
Liquid.
Table 9
The drift deviation line cloth specimen 5.0g of pure cotton half is cut, bath raio 1 is controlled:20, by sulphur yellow brown 50g/L and akali sulphide 50g/L systems
Standby dyeing liquor, soap flakes 1g/L and Na2CO3, 1g/L prepares soap boiling liquid.Dyeing liquor shakes 20min, cloth specimen in 90 DEG C of waters bath with thermostatic control
1min is impregnated in dye liquor, padding machine is crossed, pick-up 80% is controlled, is impregnating 30s in oxidation solution 1#, 2#, 3#, 4#, 5# respectively,
Washing, soap boiling is dried in 80 DEG C of baking ovens, and the colour index of resulting dyed fabric is as shown in table 10.
Table 10
| Oxidizing acid | L | a | b | K/S |
| 1# | 29.34 | 21.92 | 14.57 | 24.0 |
| 2# | 30.36 | 24.09 | 15.63 | 23.0 |
| 3# | 35.01 | 27.83 | 19.09 | 21.9 |
| 4# | 32.93 | 25.20 | 17.48 | 22.8 |
| 5# | 29.27 | 21.79 | 14.29 | 22.4 |
| 6# | 28.86 | 21.29 | 14.12 | 22.2 |
| 7# | 29.16 | 22.29 | 14.72 | 23.2 |
| 8# | 29.56 | 20.80 | 14.17 | 21.0 |
Found out by table 10, sulfamic acid is with other 7 kinds of buffering acids with weight percent accounting 70:30, it is configured to answering for 5g/L
Oxidizing acid oxidation solution is closed, K/S values 1#, 2# and 7# of fabric are larger after dyeing, but 1# -7# is than individually using sulfamic acid
8# is high, shows that sulfamic acid is mixed with the acid with buffer capacity, the oxidation color development ability to sulfur dye is improved.
Claims (10)
1. a kind of combined oxidation acid for sulfur dyeing, it is characterized in that, combined oxidation acid include sulfamic acid and
Buffering acid, the buffering acid is with pH cushioning effects carboxyl or phosphate acid.
2. a kind of combined oxidation acid for sulfur dyeing as claimed in claim 1, it is characterized in that, it is described carboxylic
Buffering acid is formic acid, acetic acid, propionic acid, butyric acid, octanoic acid, adipic acid, ethanedioic acid, malonic acid, succinic acid, maleic acid, tartaric acid, benzene
Formic acid, phenylacetic acid, phthalic acid, terephthalic acid (TPA), valeric acid, caproic acid, capric acid, stearic acid, palmitic acid, acrylic acid, amino second
One kind in acid, citric acid.
3. a kind of combined oxidation acid for sulfur dyeing as claimed in claim 2, it is characterized in that, the buffering acid is
One kind in formic acid, acetic acid, amion acetic acid, citric acid.
4. a kind of combined oxidation acid for sulfur dyeing as claimed in claim 1, it is characterized in that, the phosphate delays
Punching acid is phosphoric acid and ackd salt, 1-hydroxy ethylidene-1,1-diphosphonic acid and its sodium salt and sylvite, ATMP and its sodium salt and sylvite,
Ethylene diamine tetra methylene phosphonic acid and its sodium salt and sylvite, diethylene triamine pentamethylene phosphonic and its sodium salt and sylvite.
5. a kind of combined oxidation acid for sulfur dyeing as claimed in claim 4, it is characterized in that, described phosphate
Buffering acid is one kind in phosphoric acid, 1-hydroxy ethylidene-1,1-diphosphonic acid, ATMP.
6. a kind of combined oxidation acid for sulfur dyeing as claimed in claim 1, it is characterized in that, the combined oxidation
Each component is by weight in acid：
Sulfamic acid：0.01~100.0
Buffering acid:0~99.9.
7. a kind of combined oxidation acid for sulfur dyeing as claimed in claim 6, it is characterized in that, the combined oxidation
Each component is by weight in acid：
Sulfamic acid：20.0~90.0
Buffering acid:10.0~80.0.
8. a kind of combined oxidation acid for sulfur dyeing as claimed in claim 7, it is characterized in that, the composite oxygen
Change each component in acid is by weight：
Sulfamic acid：50.0~75.0
Buffering acid:25.0~50.0.
9. the application method sour for the combined oxidation of sulfur dyeing as described in claim 1 to claim 8, it is special
Levy is to comprise the following steps：
Combined oxidation acid solution is made in sulfamic acid and buffering acid by weight ratio, then combined oxidation acid solution is diluted to
The oxidation solution of 0.01~30g/L containing effective sulfamic acid content, control oxidation solution is between 25~75 DEG C, the fabric after upper dye
It is immersed in after oxidation solution 5s~3min, pressure rolling drying.
10. it is used for the application method of the combined oxidation acid of sulfur dyeing as claimed in claim 9, it is characterized in that the oxygen
It is 5~10g/L to change the effective sulfamic acid content of liquid, and temperature is 25 DEG C, and dip time is 10~60s.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101302711A (en) * | 2008-06-20 | 2008-11-12 | 杭州下沙恒升化工有限公司 | Solid odorless organic acid agent for textile dyeing and finishing |
| CN102619109A (en) * | 2012-03-05 | 2012-08-01 | 清远市金沣顺助剂有限公司 | Oxidant for dyeing of sulfide dye |
| CN104805706A (en) * | 2015-04-02 | 2015-07-29 | 北京服装学院 | Reduction system for vat dye or sulfur dyestuff dyeing and reduction method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101302711A (en) * | 2008-06-20 | 2008-11-12 | 杭州下沙恒升化工有限公司 | Solid odorless organic acid agent for textile dyeing and finishing |
| CN102619109A (en) * | 2012-03-05 | 2012-08-01 | 清远市金沣顺助剂有限公司 | Oxidant for dyeing of sulfide dye |
| CN104805706A (en) * | 2015-04-02 | 2015-07-29 | 北京服装学院 | Reduction system for vat dye or sulfur dyestuff dyeing and reduction method |
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