CN106590012A - Method of using CLT acid isomer mixture to prepare acid dye powder and production - Google Patents
Method of using CLT acid isomer mixture to prepare acid dye powder and production Download PDFInfo
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- CN106590012A CN106590012A CN201611082229.XA CN201611082229A CN106590012A CN 106590012 A CN106590012 A CN 106590012A CN 201611082229 A CN201611082229 A CN 201611082229A CN 106590012 A CN106590012 A CN 106590012A
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- acid
- clt
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B29/00—Monoazo dyes prepared by diazotising and coupling
- C09B29/0003—Monoazo dyes prepared by diazotising and coupling from diazotized anilines
- C09B29/0007—Monoazo dyes prepared by diazotising and coupling from diazotized anilines containing acid groups, e.g. CO2H, SO3H, PO3H2, OSO3H, OPO2H2; Salts thereof
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B29/00—Monoazo dyes prepared by diazotising and coupling
- C09B29/10—Monoazo dyes prepared by diazotising and coupling from coupling components containing hydroxy as the only directing group
- C09B29/16—Naphthol-sulfonic acids
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Abstract
The invention discloses a method of using a CLT acid isomer mixture to prepare an acid dye powder. The method mainly comprises the steps of carrying out diazotization and coupling reactions of a by-product generated in the production process of the CLT acid which is an organic pigment intermediate with a G salt or a by-product generated in the production process of the G salt to produce the acid dye powder--acid xanthan powder/acid orange powder under certain conditions. The method has the advantages of preparing cheap and fine acid dyes used for dyeing nylon and reducing environment pollution caused by the by-product of the intermediate so as to achieve comprehensive and sustainable development of industrial production.
Description
Technical field
The invention belongs to organic chemical industry field, and in particular to it is former that a kind of isomer mixture of CLT acid prepares acid dyes
The method and product of powder.
Background technology
Acid dyes (Acid Dyes) is the water-soluble dye with acidic-group in a class chemical constitution, in acid Jie
Dyeed in matter.Acid dyes great majority contain sulfonate sodium, can be dissolved in water, and bright in colour, chromatogram is complete.It is mainly used in sheep
The dyeing such as hair, silk and polyamide fibre, it can also be used to the aspect such as leather, paper, ink.To the general non-coloring power of cellulose fibre.
Acid dyes is mostly aromatic sulfonic group sodium salt in chemical constitution, azo and anthraquinone in its chromogen structure
Occupy very big proportion, in addition also all kinds of color developments such as triaryl methane, azine, mouth xanthenes, indigo, quinoline, phthalocyanine and nitro-imine
Body.In various chemical constitutions, azo acid dye all accounts for first place, especially monoazo and disazo in kind and yield
At most, including the assorted kind such as yellow, orange, red, dark blue and black.The light fastness of anthraquinone acid dye is preferable, color and luster
Bright-coloured, mainly some purple, blue, green colouring materials are especially mostly important with blueness.
Compare with direct dyes, acid dyes simple structure, lack longer common often double bond and coplanarity structure, so
Direct is lacked to cellulose fibre, it is impossible to for the dyeing of cellulose fibre.Different types of acid dyes, due to molecule knot
Structure is different, thus their dyeability is also different, and the colouring method for being adopted is also different.
The process of the isomeric by-products in organic pigment intermediate CLT acid, dyestuff intermediate G salt production processes, utilization
Problem：
The chloro- 3- amino toluenes -4- sulfonic acid of CLT acid scientific name 6-, is an important intermediate in organic red pigment synthesis,
The CLT acid production process route will typically experience the operations such as toluene sulfonation, chlorination, nitrification, hydrogenating reduction, neutralization, extraction certified products,
Production process route is very long, further relates to use strong acid, highly basic in a large number.According to current production process route, produced at it
Cheng Zhong, after the completion of the hydrogenation reduction stage, can produce nearly 1/4 CLT acid isomeric by-products, this CLT acid isomers
Side components are more complicated, the mixture of the various isomers of predominantly chloride aminotoluene sulfonic acid, if be isolated not in time
Fall, it will the product purity for affecting the chloro- 3- amino toluenes -4- sulfonic acid of certified products 6- and the organic red pigment being synthesized later
Coloured light.These separate nearly 1/4 CLT acid isomeric by-products when being chemically treated cost it is very high, so such as
What is processed and using these CLT acid isomeric by-products, is made the raw material in industrial production, always puzzlement research
The difficult problem of personnel.
G salt scientific names beta naphthal -6,8- disulfonic acid di-potassiums are a kind of important dyestuff intermediates, can manufacture various acidity
Azo dyes.In dyestuff intermediate G salt production processes, after the completion of the sulfonating reaction stage, the G salt isomeries of a part can be produced
Body accessory substance, G salt isomeric by-products are mainly the various isomer mixtures of beta naphthal disulfonic acid, and this component of mixture is more multiple
It is miscellaneous, if be isolated not in time, it will affect G salt certified products (6- naphthols -6,8- disulfonic acid) product purity and after
The coloured light of the dyestuff being synthesized.But how about G salt isomeric by-products produced by after separating are used, and are allowed to
Become the raw material in industrial production, be also a difficult problem.
Report that the document of relevant CLT acid production waste water recycling is less both at home and abroad.The China of Publication No. CN102731011A
Patent document discloses a kind of high efficiency water reducing agent and its production technology of the CLT acid production waste water for Material synthesis, specifically include by
CLT acid production waste water, phenol compound and solvent mixture heating for dissolving, adjust pH value；After adding aldehyde compound and auxiliary agent,
Insulation reaction；Reaction is cooled down after terminating.Above-mentioned technique is made with the waste water of the phenyl ring class isomer mixture produced in CLT acid production
For the raw materials for production of sulfamate high-effective water-reducing agent, one side regeneration industrial waste, on the other hand, sulfamate
The cost of material of high efficiency water reducing agent reduces about 30%, greatly improves the competitiveness of product.
Report both at home and abroad less about the document of G salt production waste water recycling.The China of Publication No. CN105800989A is specially
The method that sharp document discloses waste water synthesis modification sulfamate water reducer produced in a kind of utilization G salt production processes,
The method is prepared using the compound to waste water, sodium sulfanilate salt and phenolic hydroxyl group produced in G salt production processes and changed
Property sulfamate water reducer.Modified amido sulfoacid synthesized by this method not only has higher concrete water-reducing ratio and excellent
Slump-retaining energy, open dye intermediate wastewater comprehensive utilization new way.Reduce the raw material of the water reducer into
This alleviates the environmental pressure in dyestuff intermediate production process simultaneously, with good economical and environmentally friendly benefit.
But the amount of the annual domestic CLT acid production waste water for producing is very huge, so, it is to reduce environmental pressure, reduce
Enterprise's input cost, develops the waste water recycling mode of diversification, with great strategic importance.
The content of the invention
Technical problem solved by the invention is to provide a kind of isomer mixture of CLT acid and prepares acid dyes original powder
Method and product, the method preparation process is simple, cost is relatively low.
A kind of method that isomer mixture of CLT acid prepares acid dyes original powder, including：
(1) in acid condition, the isomer mixture of CLT acid carries out diazo-reaction with natrium nitrosum, obtains diazonium
Salt；
(2) with the isomer mixture of G salt or G salt there is coupling reaction in the diazol that step (1) is obtained, after reaction completely
Described acid dyes original powder is obtained through post processing.
Diazo component in raw materials for production of the present invention takes from pair produced in organic pigment intermediate CLT acid production process
Product --- the various isomer mixtures of CLT acid, coupling component can be G salt certified products, it is also possible to be taken from dyestuff intermediate G salt
Produced accessory substance in production process --- the various isomer mixtures of G salt, amount is easy to get greatly, both can prepare good and cheap
The acid dyes that can be used for dyeing nylon, accessory substance produced in intermediate production process is reduced again may be made to environment
Into pollution, make industrialized production obtain the development of synthesis, sustainability.
The isomer mixture of the CLT acid can be arbitrary isomers of CLT acid or the mixture of isomers.As
It is preferred that, the isomer mixture of the CLT acid is at least one in formula (1)-compound shown in (6)：
Preferably, the isomer mixture of the CLT acid be formula (1)-compound group shown in (6) into any ratio
Mixture.
In CLT acid production waste water, the compound shown in formula (1)-(6) is mainly contained, when actually used, can be directly added into
CLT acid produces waste water, and the weight percent content of the compound shown in waste water Chinese style (1)-(6) is generally 15～40%.
The isomer mixture of the G salt can be arbitrary isomers of G salt or the mixture of isomers.As excellent
Choosing, the isomer mixture of the G salt is at least one in formula (7)-compound shown in (8)：
When actually used, G salt or G salt production waste water can be directly added into, in G salt production waste water formula (7)-(8) are mainly contained
Shown compound, the weight percent content of the compound shown in G salt production waste water Chinese style (7)-(8) is generally 5～
10%.
In step (1), the acidity of system is controlled by hydrochloric acid, and as active ingredients, the isomers of the CLT acid is mixed
Compound is 110～310 with the mass ratio of hydrochloric acid：51～113.Preferably, the mass percentage concentration of the hydrochloric acid be 10～
35%.
In step (1), as active ingredients, the isomer mixture of the CLT acid is 110 with the mass ratio of natrium nitrosum
～310：48～110.Preferably, the isomer mixture of the CLT acid is 200～250 with the mass ratio of natrium nitrosum：60
～80.
Preferably, the isomer mixture of the CLT acid that pH is 7～8 is warming up to into 60～100 DEG C, hydrochloric acid is slowly dropped into
Solution, stirs 0.5～1.5h after completion of dropping.Hydrochloric acid solution is instilled at such a temperature, can accelerate the isomer mixture of CLT acid
Hydrochloride is generated, makes reaction more abundant.
In step (1), the temperature of the diazo-reaction is -5～15 DEG C.Preferably, the temperature of the diazo-reaction
Spend for 0～5 DEG C.
In step (1), the time of the diazo-reaction is 0.5～4h.Preferably, the time of the diazo-reaction
For 2～3h.
In step (2), as active ingredients, the input amount of the isomer mixture of G salt or G salt and the initially CLT of input
The mass ratio of the isomer mixture of acid is 98～522：110～310.Preferably, the isomer mixture of G salt or G salt
Input amount is 240～350 with the mass ratio of the isomer mixture of the CLT acid of initial input：200～250.
In step (2), the temperature of the coupling reaction is 0～25 DEG C.
In step (2), the time of the coupling reaction is 0.5～4h.Preferably, the time of the coupling reaction is 2
～3h.
In step (2), described post processing includes that saltouing, be dried or spray tower is dried.
Present invention also offers a kind of acid dyes original powder product prepared by said method.Wherein, with CLT acid
Isomer mixture and G salt are acid xanthan powder for the acid dyes original powder product that raw material is prepared, with the isomers of CLT acid
The isomers of mixture and G salt is acid orange original powder for the acid dyes original powder product that raw material is prepared.
Compared with prior art, the invention has the advantages that：
(1) this method is a kind of commercial run, and its preparation process operating procedure is simple, in common response kettle
Complete；
(2) present invention mainly uses accessory substance --- CLT produced in organic pigment intermediate CLT acid production process
The various isomer mixtures of acid, by with accessory substance produced in G salt or G salt production processes --- the various isomers of G salt are mixed
Compound, through diazo-reaction under certain reaction condition, coupling reaction obtains acid xanthan powder or acid orange original powder, both can be with
The cheap and good-quality acid dyes that can be used for dyeing nylon is prepared, by-product produced in intermediate production process is reduced again
The possible pollution on the environment of thing, makes industrialized production obtain the development of synthesis, sustainability.
Description of the drawings
Fig. 1 is the dyeing curve of the embodiment of the present invention 9.
Specific embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than restriction the scope of the present invention.In addition, it is to be understood that after the content for having read elaboration of the present invention, people in the art
Member such as makes various changes or modifications to the present invention, and these equivalent form of values equally fall within what the application appended claims were limited
Within the scope of.
Embodiment 1
First, acid dyes original powder --- the factory formula (weight portion) of acid xanthan powder：
2nd, the preparation method of acid dyes original powder：
Natrium nitrosum is dissolved in 80 DEG C of hot water in advance, is made into the sodium nitrite in aqueous solution that mass fraction is 30%, treated
With；G salt certified products is dissolved in a certain amount of 80 DEG C of hot water, pH value is adjusted to 6.0～6.5 with 30% sodium hydrate aqueous solution,
The G saline solutions that mass fraction is 30% are made into, it is stand-by.
(1) in the reactor, the CLT acid waste water of the various isomers of the acid containing 18%CLT is added, 80 DEG C are heated to, is stirred,
30% aqueous hydrochloric acid solution is slowly added dropwise in 0.5 hour, completion of dropping is stirred for 1.0 hours.Then ice bath is changed into, 0～5
Sodium nitrite in aqueous solution was slowly added dropwise in 0.5 hour under the conditions of DEG C, completion of dropping continues insulation and stirs under the conditions of 0～5 DEG C
Mix 2.0 hours, diazo-reaction is completed, and obtains diazol.
(2) G saline solutions are slowly added dropwise in 0.5 hour, in the diazol that step (1) is obtained, completion of dropping,
Continue insulated and stirred 2 hours under the conditions of 0～10 DEG C, then pH value is adjusted to 6.5 with 30% sodium hydrate aqueous solution, coupling reaction is complete
Into.
A certain amount of salt is added to make dyestuff saltout, vacuum filtration obtains filter cake, and 70 DEG C of drying obtain the acid dyes
Former powder --- acid xanthan powder.
Embodiment 2
First, acid dyes original powder --- the factory formula (weight portion) of acid xanthan powder：
2nd, the preparation method of acid dyes original powder：
Natrium nitrosum is dissolved in 80 DEG C of hot water in advance, is made into the sodium nitrite in aqueous solution that mass fraction is 30%, treated
With；G salt certified products is dissolved in a certain amount of 80 DEG C of hot water, pH value is adjusted to 6.0～6.5 with 30% sodium hydrate aqueous solution,
The G saline solutions that mass fraction is 30% are made into, it is stand-by.
(1) in the reactor, the CLT acid waste water of the various isomers of the acid containing 18%CLT is added, 80 DEG C are heated to, is stirred,
30% aqueous hydrochloric acid solution is slowly added dropwise in 0.5 hour, completion of dropping is stirred for 1.0 hours.Then ice bath is changed into, 0～5
Sodium nitrite in aqueous solution was slowly added dropwise in 0.5 hour under the conditions of DEG C, completion of dropping continues insulation and stirs under the conditions of 0～5 DEG C
Mix 2.5 hours, diazo-reaction is completed, and obtains diazol.
(2) G saline solutions are slowly added dropwise in 0.5 hour, in the diazol that step (1) is obtained, completion of dropping,
Continue insulated and stirred 2.5 hours under the conditions of 0～10 DEG C, then pH value is adjusted to 6.5 with 30% sodium hydrate aqueous solution, coupling reaction
Complete.
A certain amount of salt is added to make dyestuff saltout, vacuum filtration obtains filter cake, and 70 DEG C of drying obtain the acid dyes
Former powder --- acid xanthan powder.
Embodiment 3
First, acid dyes original powder --- the factory formula (weight portion) of acid xanthan powder：
2nd, the preparation method of acid dyes original powder：
Natrium nitrosum is dissolved in 60 DEG C of hot water in advance, is made into the sodium nitrite in aqueous solution that mass fraction is 30%, treated
With；G salt certified products is dissolved in a certain amount of 60 DEG C of hot water, pH value is adjusted to 6.0～6.5 with 30% sodium hydrate aqueous solution,
The G saline solutions that mass fraction is 30% are made into, it is stand-by.
(1) in the reactor, the CLT acid waste water of the various isomers of the acid containing 25%CLT is added, 60 DEG C are heated to, is stirred,
30% aqueous hydrochloric acid solution is slowly added dropwise in 0.5 hour, completion of dropping is stirred for 1.0 hours.Then under the conditions of 5～10 DEG C
Sodium nitrite in aqueous solution was slowly added dropwise in 0.5 hour, completion of dropping continues insulated and stirred 1.5 little under the conditions of 5～10 DEG C
When, diazo-reaction is completed, and obtains diazol.
(2) G saline solutions are slowly added dropwise in 0.5 hour, in the diazol that step (1) is obtained, completion of dropping,
Continue insulated and stirred 1.5 hours under the conditions of 10～15 DEG C, then pH value is adjusted to 6.5 with 30% sodium hydrate aqueous solution, coupling is anti-
Should complete.
A certain amount of salt is added to make dyestuff saltout, vacuum filtration obtains filter cake, and 70 DEG C of drying obtain the acid dyes
Former powder --- acid xanthan powder.
Embodiment 4
First, acid dyes original powder --- the factory formula (weight portion) of acid xanthan powder：
2nd, the preparation method of acid dyes original powder：
Natrium nitrosum is dissolved in 90 DEG C of hot water in advance, is made into the sodium nitrite in aqueous solution that mass fraction is 30%, treated
With；G salt certified products is dissolved in a certain amount of 90 DEG C of hot water, pH value is adjusted to 6.0～6.5 with 30% sodium hydrate aqueous solution,
The G saline solutions that mass fraction is 30% are made into, it is stand-by.
(1) in the reactor, the CLT acid waste water of the various isomers of the acid containing 15%CLT is added, 90 DEG C are heated to, is stirred,
30% aqueous hydrochloric acid solution is slowly added dropwise in 0.5 hour, completion of dropping is stirred for 0.5 hour.Then under the conditions of -5～0 DEG C
Sodium nitrite in aqueous solution was slowly added dropwise in 0.5 hour, completion of dropping continues insulated and stirred 3.5 little under the conditions of -5～0 DEG C
When, diazo-reaction is completed, and obtains diazol.
(2) G saline solutions are slowly added dropwise in 0.5 hour, in the diazol that step (1) is obtained, completion of dropping,
Continue insulated and stirred 0.5 hour under the conditions of 15～20 DEG C, then pH value is adjusted to 6.5 with 30% sodium hydrate aqueous solution, coupling is anti-
Should complete.
A certain amount of salt is added to make dyestuff saltout, vacuum filtration obtains filter cake, and 70 DEG C of drying obtain the acid dyes
Former powder --- acid xanthan powder.
Embodiment 5
First, acid dyes original powder --- the factory formula (weight portion) of acid orange original powder：
2nd, the preparation method of acid dyes original powder：
Natrium nitrosum is dissolved in 80 DEG C of hot water in advance, is made into the sodium nitrite in aqueous solution that mass fraction is 30%, treated
With.
(1) in the reactor, the CLT acid waste water of the various isomers of the acid containing 18%CLT is added, 80 DEG C are heated to, is stirred,
30% aqueous hydrochloric acid solution is slowly added dropwise in 0.5 hour, completion of dropping is stirred for 1.0 hours.Then ice bath is changed into, 0～5
Sodium nitrite in aqueous solution was slowly added dropwise in 0.5 hour under the conditions of DEG C, completion of dropping continues insulation and stirs under the conditions of 0～5 DEG C
Mix 2.0 hours, diazo-reaction is completed, and obtains diazol.
(2) in 0.5 hour, the G of the various isomers of salt containing 6%G is slowly added dropwise in the diazol that step (1) is obtained
Salt waste water, completion of dropping continues insulated and stirred 2 hours under the conditions of 5～15 DEG C, then adjusts pH with 30% sodium hydrate aqueous solution
It is worth to 6.5, coupling reaction is completed.
A certain amount of salt is added to make dyestuff saltout, vacuum filtration obtains filter cake, and 70 DEG C of drying obtain described acid dye
The former powder of material --- acid orange original powder.
Embodiment 6
First, acid dyes original powder --- the factory formula (weight portion) of acid orange original powder：
2nd, the preparation method of acid dyes original powder：
Natrium nitrosum is dissolved in 80 DEG C of hot water in advance, is made into the sodium nitrite in aqueous solution that mass fraction is 30%, treated
With.
(1) in the reactor, the CLT acid waste water of the various isomers of the acid containing 18%CLT is added, 80 DEG C are heated to, is stirred,
30% aqueous hydrochloric acid solution is slowly added dropwise in 0.5 hour, completion of dropping is stirred for 1.0 hours.Then ice bath is changed into, 0～5
Sodium nitrite in aqueous solution was slowly added dropwise in 0.5 hour under the conditions of DEG C, completion of dropping continues insulation and stirs under the conditions of 0～5 DEG C
Mix 2.5 hours, diazo-reaction is completed, and obtains diazol.
(2) in 0.5 hour, the G of the various isomers of salt containing 6%G is slowly added dropwise in the diazol that step (1) is obtained
Salt waste water, completion of dropping continues insulated and stirred 2.5 hours under the conditions of 5～10 DEG C, then is adjusted with 30% sodium hydrate aqueous solution
To 6.5, coupling reaction is completed pH value.
A certain amount of salt is added to make dyestuff saltout, vacuum filtration obtains filter cake, and 70 DEG C of drying obtain described acid dye
The former powder of material --- acid orange original powder.
Embodiment 7
First, acid dyes original powder --- the factory formula (weight portion) of acid orange original powder：
2nd, the preparation method of acid dyes original powder：
Natrium nitrosum is dissolved in 70 DEG C of hot water in advance, is made into the sodium nitrite in aqueous solution that mass fraction is 30%, treated
With.
(1) in the reactor, the CLT acid waste water of the various isomers of the acid containing 26%CLT is added, 70 DEG C are heated to, is stirred,
30% aqueous hydrochloric acid solution is slowly added dropwise in 0.5 hour, completion of dropping is stirred for 1.0 hours.Then ice bath is changed into, 0～5
Sodium nitrite in aqueous solution was slowly added dropwise in 0.5 hour under the conditions of DEG C, completion of dropping continues insulation and stirs under the conditions of 0～5 DEG C
Mix 2.5 hours, diazo-reaction is completed, and obtains diazol.
(2) in 0.5 hour, the G of the various isomers of salt containing 8%G is slowly added dropwise in the diazol that step (1) is obtained
Salt waste water, completion of dropping continues insulated and stirred 1.5 hours under the conditions of 5～10 DEG C, then is adjusted with 30% sodium hydrate aqueous solution
To 6.5, coupling reaction is completed pH value.
A certain amount of salt is added to make dyestuff saltout, vacuum filtration obtains filter cake, and 70 DEG C of drying obtain described acid dye
The former powder of material --- acid orange original powder.
Embodiment 8
First, acid dyes original powder --- the factory formula (weight portion) of acid orange original powder：
2nd, the preparation method of acid dyes original powder：
Natrium nitrosum is dissolved in 85 DEG C of hot water in advance, is made into the sodium nitrite in aqueous solution that mass fraction is 30%, treated
With.
(1) in the reactor, the CLT acid waste water of the various isomers of the acid containing 15%CLT is added, 85 DEG C are heated to, is stirred,
30% aqueous hydrochloric acid solution is slowly added dropwise in 0.5 hour, completion of dropping is stirred for 1.0 hours.Then under the conditions of -5～0 DEG C
Sodium nitrite in aqueous solution was slowly added dropwise in 0.5 hour, completion of dropping continues insulated and stirred 3.5 little under the conditions of -5～0 DEG C
When, diazo-reaction is completed, and obtains diazol.
(2) in 0.5 hour, the various isomers of salt containing 10%G are slowly added dropwise in the diazol that step (1) is obtained
G salt waste water, completion of dropping continues insulated and stirred 0.5 hour under the conditions of 15～20 DEG C, then is adjusted with 30% sodium hydrate aqueous solution
To 6.5, coupling reaction is completed section pH value.
A certain amount of salt is added to make dyestuff saltout, vacuum filtration obtains filter cake, and 70 DEG C of drying obtain described acid dye
The former powder of material --- acid orange original powder.
Embodiment 9
Acid orange original powder prepared by acid xanthan powder or embodiment 5～8 prepared by embodiment 1～4 is to dyeing nylon
And its washing fastness test：
First, prepared acid xanthan powder or acid orange original powder are to nylon dye methods
Colouring method：Contaminate
2nd, prepared acid xanthan powder or acid orange original powder dyeing prescription
1st, 3g/ blocks nylon cloth
2nd, dye strength (o.w.f) 4%
3rd, glacial acetic acid concentration (o.w.f) 4%
4th, glauber salt concentration (o.w.f) 10%
Bath raio：30：1
3rd, prepared acid xanthan powder or acid orange original powder dyeing flow process and process conditions
Dyeing curve is as shown in figure 1, specifically include：Technology preparation is pressed at room temperature and adds dyestuff and auxiliary agent, adopt
Temperature-gradient method is dyeed, with the ramp of 1.5 DEG C/min to 70 DEG C, then with the ramp of 1.0 DEG C/min to 100 DEG C,
After insulation 30min, room temperature is cooled to by 100 DEG C with the speed of 2.0 DEG C/min, finally washes, iron dry, be i.e. dyeing is finished.
4th, washing color fastness test
To the nylon after dyeing according to GB/T 3921-2008《Textile color stability tests fastness to soaping》In (2)
Test method carries out washing color fastness test.It is water-fast to pass judgment on according to the grade of sample discoloration and the grade of adjacent fabric staining
Wash color fastness.Washing color fastness test result is as shown in table 1：
The washing color fastness test result of table 1
| Colour fading fastness | Staining fastness | |
| Embodiment 1 | 3 grades | 3.5 level |
| Embodiment 2 | 3.5 level | 3.5 level |
| Embodiment 3 | 3 grades | 3 grades |
| Embodiment 4 | 3.5 level | 3 grades |
| Embodiment 5 | 3 grades | 3 grades |
| Embodiment 6 | 3.5 level | 3.5 level |
| Embodiment 7 | 3 grades | 3.5 level |
| Embodiment 8 | 3.5 level | 3 grades |
From above-mentioned washing color fastness test result, the present invention is prepared using the isomer mixture of CLT acid
Acid dyes original powder there is preferable colour fading fastness and staining fastness.Acid dyes original powder prepared by the present invention is actually used
When, consumption is similar to the usage amount of existing acid dyes original powder, can be adjusted according to actual needs.The present invention both can be prepared
Go out the cheap and good-quality acid dyes that can be used for dyeing nylon, accessory substance produced in intermediate production process is reduced again can
Energy pollution on the environment, makes industrialized production obtain the development of synthesis, sustainability.
Claims (10)
1. a kind of method that isomer mixture of CLT acid prepares acid dyes original powder, it is characterised in that include：
(1) in acid condition, the isomer mixture of CLT acid carries out diazo-reaction with natrium nitrosum, obtains diazol；
(2) there is coupling reaction in the isomer mixture of the diazol that step (1) is obtained and G salt or G salt, after reaction completely through
Post processing obtains described acid dyes original powder.
2. the method that the isomer mixture of CLT acid according to claim 1 prepares acid dyes original powder, its feature exists
In the isomer mixture of the CLT acid is at least one in formula (1)-compound shown in (6)：
3. the method that the isomer mixture of CLT acid according to claim 1 prepares acid dyes original powder, its feature exists
In the isomer mixture of the G salt is at least one in formula (7)-compound shown in (8)：
4. the method that the isomer mixture of CLT acid according to claim 1 prepares acid dyes original powder, its feature exists
In, in step (1), as active ingredients, the isomer mixture of the CLT acid and the mass ratio of natrium nitrosum be 110～
310：48～110.
5. the method that the isomer mixture of CLT acid according to claim 1 prepares acid dyes original powder, its feature exists
In, in step (1), the acidity of system is controlled by hydrochloric acid, as active ingredients, the isomer mixture of the CLT acid
It is 110～310 with the mass ratio of hydrochloric acid：51～113.
6. the method that the isomer mixture of CLT acid according to claim 1 prepares acid dyes original powder, its feature exists
In in step (1), the temperature of the diazo-reaction is 0～5 DEG C.
7. the method that the isomer mixture of CLT acid according to claim 1 prepares acid dyes original powder, its feature exists
In in step (1), the time of the diazo-reaction is 0.5～4h.
8. the method that the isomer mixture of CLT acid according to claim 1 prepares acid dyes original powder, its feature exists
In in step (2), as active ingredients, the input amount of the isomer mixture of G salt or G salt is different with the CLT acid of initial input
The mass ratio of structure body mixture is 98～522：110～310.
9. the method that the isomer mixture of CLT acid according to claim 1 prepares acid dyes original powder, its feature exists
In the time of the coupling reaction is 0.5～4h.
10. a kind of acid dyes original powder product, it is characterised in that described acid dyes original powder product is by claim 1～9 times
Preparation method described in one is prepared.
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