CN104710812B - Preparation method of disperse dye capable of alkaline dyeing - Google Patents
Preparation method of disperse dye capable of alkaline dyeing Download PDFInfo
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Abstract
The invention discloses a preparation method of a disperse dye capable of alkaline dyeing. The preparation method comprises the following step of carrying out a substitution reaction of a compound VI and a compound X-R2, wherein R1 is -H, -CH3, -C2H5, -OCH3 or -OC2H5, and R2 is C1-C4 straight-chain or branched-chain alkyl or benzyl, R8 is C1-C4 straight-chain or branched-chain alkyl, nitro, -NHCOCH3 or -NHCOC2H5, R9 and R10 are independently -H, halogen or nitro, and X is halogen. The disperse dye obtained by the preparation method shows a bright yellow color, can be used individually, also can be in combination use with alkali-resisting disperse dyes having other colors, and has excellent alkali resistance and hydrogen peroxide oxidization resistance stability.
Description
Technical field
The present invention relates to a kind of preparation method of the disperse dyes of alkali dyeing.
Background technology
Polyester fiber and its blend fabric have important application in current high-grade fabric, and the dyestuff that it is suitable for is dispersion
Dyestuff.Disperse dyes are applied to during the dyeing of polyester fiber product be usually using acid dye bath dyeing, but acid dyeing is easy
Produce and stain the disadvantages such as the specking causing, color dot, dyeing flower because of oligomer.Disperse dyes basic dyeing technique can effectively remove dyeing
During the oligomer that produces, be expected to shorten the technological process of production, have low consumption, efficiently, energy-conservation and timesaving feature.In recent years
Come, the pressure of energy-saving and emission-reduction and cost promotes printing and dyeing enterprise and color additive manufacturer to make joint efforts, and develops multiple alkali resistances and divides
Scattered dyestuff and its supporting dyeing assistant, the alkaline concise one-pass bath method for dyeing technique of new development also on basic dyeing Process ba- sis.
Alkaline-resisting series disperse dyes in the market, applicable pH value is generally 4-9, and portioned product is 4- up to pH value
10 or 4-11 scope.It is clear that for concise one-pass bath method for dyeing technique, the alkali resistance of part disperse dyes and oxytolerant
The property changed still is apparent not enough, and is especially the absence of a kind of alkali resistance and the good bright yellow disperse dyes of oxidative resistance.
Patent CN102250485 discloses a kind of Yellow disperse dye of acid-alkaline dyeing, can be in the dye bath of pH=4-14
Middle dyeing, but do not refer to its resistance to oxidation stability.This dye shade is that HONGGUANG is yellow, and because of material purity and reacts into stroke
The reason spend, this dyestuff yet suffers from the exceeded risk of carcinogen aromatic amine.
Content of the invention
Technical problem solved by the invention is to overcome existing disperse dyes alkali resistance difference and resistance to oxidation stable
Property difference defect, there is provided a kind of bright yellow disperse dyes of alkali dyeing.The Yellow disperse dye of the present invention presents light yellow
Color, can be used as monochromatic using it is also possible to be applied in combination with the alkaline-proof disperse dyes of other colors, it have excellent alkali resistance and
Resistance to hydrogen peroxide oxidation stability, this feature makes it can be applied not only to the general basic printing and dyeing processing of Polyester Fibers,
Can be applicable to concise one-pass bath method for dyeing technique or bleaching and dyeing single bath process technique and the active Graft versus host disease technique of dispersion, and can meet
Environmental requirement.
The present invention is to solve above-mentioned technical problem by the following technical programs：
The invention provides a kind of bright yellow disperse dyes A of alkali dyeing,
Wherein, R1For-H ,-CH3、-C2H5、-OCH3Or-OC2H5, R2For C1-C4Straight or branched alkyl or benzyl.
Wherein, R1Preferably-H or-CH3, more preferably for-H.
Wherein, R2Preferably n-pro-pyl, isopropyl, normal-butyl, isobutyl group, the tert-butyl group or benzyl, more preferably for positive third
Base.
In the present invention, the bright yellow disperse dyes A of described alkali dyeing is preferably as formula A ' or A " shown in compound,
Wherein, the definition of each substituent group is all same as above.
In the present invention, the bright yellow disperse dyes A of described alkali dyeing is further preferably as shown in formula A1, A2 or A3
Compound,
Present invention also offers the preparation method of the bright yellow disperse dyes A of described alkali dyeing, it includes following
Step：By compound I and compounds X-R2Carry out substitution reaction, you can；
Wherein, R1For-H ,-CH3、-C2H5、-OCH3Or-OC2H5, R2For C1-C4Straight or branched alkyl or benzyl, X is halogen
Element.
Wherein, the preparation method of described bright yellow disperse dyes A preferably includes following step：In water, in hydroxide
In the presence of sodium and tetrabutyl ammonium bromide, compound I and compounds X-R2Carry out substitution reaction, you can.
Wherein, described compound I and described compounds X-R2Mol ratio be preferably（1:1）~（1:1.5）.
Wherein, described sodium hydroxide and the mol ratio of described compound I are preferably（1:1）~（1.6:1）.
Wherein, described tetrabutyl ammonium bromide and the mol ratio of described compound I are preferably（0.002:1）~
（0.05:1）.
Wherein, preferably 65～100 DEG C of the temperature of described substitution reaction.
Wherein, the described process obtaining reaction can be monitored by HPLC or GC, makees when typically being disappeared with compound I
Terminal for reaction.The time of described substitution reaction is preferably 3～15h.
In the preparation method of bright yellow disperse dyes A, described compound I can be obtained by following methods：In nitrous acid
In the presence of sodium, compound II and compound III carries out diazo coupling reaction, you can；
The preparation method of described compound I preferably includes following step：In hydrochloric acid, in the presence of sodium nitrite,
There is diazo-reaction in compound II, then in the presence of sodium carbonate and sodium hydroxide, carry out coupling reaction with compound III,
?.
Wherein, described sodium nitrite and the mol ratio of described compound II are preferably（1.01:1）~（1.3:1）.
Described sodium nitrite is preferably fed intake in the form of sodium nitrite solution, and the percent mass of described sodium nitrite solution compares
It is 20%～30% goodly.
Wherein, the mass percent concentration of described hydrochloric acid preferably 30%～36%, described hydrochloric acid and described change
The mol ratio of compound II is preferably（2.5:1）~（4.5:1）.
Wherein, preferably 0～5 DEG C of the temperature of described diazo-reaction.The time of described diazo-reaction is preferable
Ground is 3～5h.
Wherein, described compound III is preferably with the mol ratio of described compound II（1.01:1）~（1.15:
1）.
Wherein, described sodium carbonate and the mol ratio of described compound II are preferably（1:1）~（1.2:1）.
Wherein, described sodium hydroxide and the mol ratio of described compound II are preferably（1.5:1）~（2.0:1）.
Wherein, preferably 0～10 DEG C of the temperature of described coupling reaction.The time of described coupling reaction is preferably
3～5h.
Present invention also offers the bright yellow disperse dyes A of described alkali dyeing is in dyeing polyester fibre material or print
Application in spending.
Wherein, the technique of described dyeing is preferably concise one-pass bath method for dyeing technique or bleachinges and dyeing single bath process technique.Described
The technique of stamp be preferably and disperse active Graft versus host disease technique.
The invention provides bright yellow disperse dyes B,
Wherein, R3For C1-C4Straight or branched alkyl ,-OCH3Or-OC2H5, R4And R5Alone for H, halogen or nitro, but
It is asynchronously-H or nitro, R6And R7Alone for methyl, ethyl ,-C2H4CN、-C2H4OCH3、-C2H4OC2H5Or benzyl.
Wherein, R3Preferably methyl or ethyl, more preferably for methyl.
Wherein, R4Preferably-H ,-Cl ,-Br or nitro, more preferably for-Br.
Wherein, R5Preferably-H ,-Cl ,-Br or nitro, more preferably for-Br.
Wherein, R6Preferably-C2H4CN、-C2H4OCH3Or benzyl, more preferably for-C2H4CN or benzyl.
Wherein, R7Preferably-C2H4CN、-C2H4OCH3Or benzyl, more preferably for-C2H4CN or benzyl.
In the present invention, described bright yellow disperse dyes B is preferably as formula B ', B " or B " ' shown in compound,
Wherein, the definition of each substituent group is all same as above.
In the present invention, the described bright yellow disperse dyes B chemical combination further preferably as shown in formula B1, B2, B3, B4 or B5
Thing,
Present invention also offers the preparation method of described bright yellow disperse dyes B, it comprises the steps：In nitrous acid
In the presence of sodium, compound IV and compound V carries out diazo coupling reaction, you can；
Wherein, R3For C1-C4Straight or branched alkyl ,-OCH3Or-OC2H5, R4And R5Alone for H, halogen or nitro, but
It is asynchronously-H or nitro, R6And R7Alone for methyl, ethyl ,-C2H4CN、-C2H4OCH3、-C2H4OC2H5Or benzyl.
The preparation method of described bright yellow disperse dyes B preferably includes following step：In hydrochloric acid, in sodium nitrite
Under effect, there is diazo-reaction in compound IV, then in the presence of concentrated sulphuric acid, carry out coupling reaction with compound V, you can.
Wherein, described sodium nitrite and the mol ratio of described compound IV are preferably（1.01:1）~（1.15:
1）.Described sodium nitrite is preferably fed intake in the form of sodium nitrite solution, the percent mass of described sodium nitrite solution
Ratio preferably 20%～30%.
Wherein, the mass percent concentration of described hydrochloric acid preferably 30%～36%, described hydrochloric acid and described change
The mol ratio of compound IV is preferably（2.5:1）~（4.5:1）.
Wherein, preferably 0～5 DEG C of the temperature of described diazo-reaction.The time of described diazo-reaction is preferable
Ground is 3～5h.
Wherein, described compound IV is preferably with the mol ratio of described compound V（1.01:1）~（1.15:1）.
Wherein, described concentrated sulphuric acid and the mass ratio of described compound IV are preferably（0.3:1）~（0.6:1）.Institute
The mass percent concentration of the concentrated sulphuric acid stated preferably 93%～98%.
Wherein, preferably 0～10 DEG C of the temperature of described coupling reaction.The time of described coupling reaction is preferably
3～5h.
Present invention also offers application in dyeing polyester fibre material or stamp for the described bright yellow disperse dyes B.
Wherein, the technique of described dyeing is preferably concise one-pass bath method for dyeing technique or bleachinges and dyeing single bath process technique.Described
The technique of stamp be preferably and disperse active Graft versus host disease technique.
The invention provides disperse dyes C,
Wherein, R1For-H ,-CH3、-C2H5、-OCH3Or-OC2H5, R2For C1-C4Straight or branched alkyl or benzyl, R8For
C1-C4Straight or branched alkyl, nitro ,-NHCOCH3Or-NHCOC2H5, R9And R10Alone for-H, halogen or nitro.
Wherein, R1Preferably-H or-CH3, more preferably for-H.
Wherein, R2Preferably propyl group, butyl or benzyl, more preferably for propyl group.
Wherein, R8Preferably methyl, ethyl, nitro or-NHCOCH3, more preferably for nitro or-NHCOCH3.
Wherein, R9Preferably-H ,-Br or nitro, more preferably for-H or-Br.
Wherein, R10Preferably-H ,-Br or nitro, more preferably for-H or-Br.
In the present invention, described disperse dyes C is preferably as formula C ', C ", C " ' or C " " shown in compound,
Wherein, the definition of each substituent group is all same as above.
In the present invention, the described disperse dyes C compound further preferably as shown in formula C1, C2, C3, C4, C5 or C6,
Present invention also offers the preparation method of described disperse dyes C, it comprises the steps：By compound VI and change
Compound X-R2Carry out substitution reaction, you can；
Wherein, R1For-H ,-CH3、-C2H5、-OCH3Or-OC2H5, R2For C1-C4Straight or branched alkyl or benzyl, R8For
C1-C4Straight or branched alkyl, nitro ,-NHCOCH3Or-NHCOC2H5, R9And R10Alone for-H, halogen or nitro, X is halogen
Element.
Wherein, the preparation method of described disperse dyes C preferably includes following step：In water, in sodium hydroxide and four
In the presence of butylammonium bromide, compound VI and compounds X-R2Carry out substitution reaction, you can.
Wherein, described compound VI and described compounds X-R2Mol ratio be preferably（1:1）~（1:1.5）.
Wherein, described sodium hydroxide and the mol ratio of described compound VI are preferably（1:1）~（1.6:1）.
Wherein, described tetrabutyl ammonium bromide and the mol ratio of described compound VI are preferably（0.002:1）~
（0.05:1）.
Wherein, preferably 65～100 DEG C of the temperature of described substitution reaction.
Wherein, the described process obtaining reaction can be monitored by HPLC or GC, when typically being disappeared with compound VI
Terminal as reaction.The time of described substitution reaction is preferably 3～15h.
In the preparation method of disperse dyes C, described compound VI can be obtained by following methods：Work in sodium nitrite
With under, compound VII and compound III carry out diazo coupling reaction, you can；
Wherein, the definition of each substituent group is all same as above.
The preparation method of described compound VI preferably includes following step：In hydrochloric acid, in the presence of sodium nitrite,
There is diazo-reaction in compound VII, then in the presence of sodium carbonate and sodium hydroxide, carry out coupling reaction with compound III,
?.
Wherein, described sodium nitrite and the mol ratio of described compound VII are preferably（1.01:1）~（1.3:
1）.Described sodium nitrite is preferably fed intake in the form of sodium nitrite solution, the percent mass of described sodium nitrite solution
Ratio preferably 20%～30%.
Wherein, the mass percent concentration of described hydrochloric acid preferably 30%～36%, described hydrochloric acid and described change
The mol ratio of compound VII is preferably（2.5:1）~（4.5:1）.
Wherein, preferably 0～5 DEG C of the temperature of described diazo-reaction.The time of described diazo-reaction is preferable
Ground is 3～5h.
Wherein, described compound III is preferably with the mol ratio of described compound VII（1.01:1）~（1.15:
1）.
Wherein, described sodium carbonate and the mol ratio of described compound VII are preferably（1:1）~（1.2:1）.
Wherein, described sodium hydroxide and the mol ratio of described compound VII are preferably（1.5:1）~（2.0:1）.
Wherein, preferably 0～10 DEG C of the temperature of described coupling reaction.The time of described coupling reaction is preferably
3～5h.
Present invention also offers application in dyeing polyester fibre material or stamp for the described disperse dyes C.
Wherein, the technique of described dyeing is preferably concise one-pass bath method for dyeing technique or bleachinges and dyeing single bath process technique.Described
The technique of stamp be preferably and disperse active Graft versus host disease technique.
Present invention also offers a kind of admixture of disperse dyes, it includes following components by percentage to the quality：Dispersion
Dyestuff A0～100%, disperse dyes B0～100% and disperse dyes C0～100%, wherein disperse dyes A, disperse dyes B and dispersion
It is 0 when the content of dyestuff C is different.
Wherein, the content of described disperse dyes A preferably 5～90%, more preferably for 10～80%.
Wherein, the content of described disperse dyes B preferably 5～90%, more preferably for 10～80%.
Wherein, the content of described disperse dyes C preferably 5～90%, more preferably for 10～80%.
It is preferred that described admixture of disperse dyes can also include auxiliary agent, described auxiliary agent can disperse dye for this area
Conventional use of various auxiliary agents in material, are preferably comprised naphthalene sulfonic acid-formaldehyde condensation product, lignosulfonates and alkyl naphthalene sulfonic acid first
One or more of aldehyde condensate, more preferably includes condensation compound of methyl naphthalene sulfonic acid and formaldehyde（I.e. Dispersant MF）And/or lignin
Sodium sulfonate.
Described auxiliary agent is preferably with the mass ratio of disperse dyes in mixture（0.6～5）：1.
Present invention also offers the preparation method of above-mentioned admixture of disperse dyes, it is any one in following methods：
Method one：After all components are mixed with water by mass percentage, grinding distribution, it is spray-dried, you can；
Method two：After each component is mixed with water respectively, grinding distribution, it is spray-dried, then mix by mass percentage, that is,
Can.
When containing auxiliary agent in described admixture of disperse dyes, the preparation method of described admixture of disperse dyes is preferred
Any one in following methods：
Method one：After all components are mixed with auxiliary agent and water by mass percentage, grinding distribution, it is spray-dried, you can；
Method two：After each component is mixed with auxiliary agent and water respectively, grinding distribution, it is spray-dried, more by mass percentage
Mixing, you can.
Wherein, described grinding distribution is preferably carried out in grinder or sand mill.
Present invention also offers application in dyeing polyester fibre material or stamp for the above-mentioned admixture of disperse dyes.
Wherein, the technique of described dyeing is preferably concise one-pass bath method for dyeing technique or bleachinges and dyeing single bath process technique.Described
The technique of stamp be preferably and disperse active Graft versus host disease technique.
On the basis of meeting common sense in the field, above-mentioned each optimum condition, can combination in any, obtain final product each preferable reality of the present invention
Example.
Agents useful for same of the present invention and raw material are all commercially available.
The positive effect of the present invention is：Dyestuff of the present invention has extremely strong alkali stability and resistance to stabilized hydrogen peroxide
Property, this feature is concise one-pass bath method for dyeing technique or bleachinges and dyeing single bath process technique, and disperses answering of active Graft versus host disease technique
With providing feasibility；And dyestuff meets environmental protection and ecological requirements, there is preferably comprehensive dyefastness.
Specific embodiment
Further illustrate the present invention below by the mode of embodiment, but therefore do not limit the present invention to described reality
Apply among a scope.The experimental technique of unreceipted actual conditions in the following example, conventionally and condition, or according to business
Product description selects.
The preparation of compound A1：（1）Add 150 grams of water, N- (2,4- dinitro) phenyl -1 in 250mL there-necked flask,
13.7 grams of 3- diaminobenzene, adds 20 grams of the hydrochloric acid that mass percent concentration is 36%, continues after room temperature uniform stirring half an hour
Stirring 1.5 hours, on the rocks be cooled to 0-5 DEG C, Deca mass fraction is 20% 18.6 grams of sodium nitrite solution, then proceedes to
0-5 DEG C react 3 hours, add 0.5 gram of sulfamic acid, with starch potassium iodide paper test colourless after, that is, obtain diazol and treat idol
Close.
（2）1000mL beaker adds 7 grams of the sodium hydroxide that 200 grams of water, mass fraction are 30%, 8.7 grams of sodium carbonate,
4.8 grams of phenol, after stirring half is little, is maintained at 0-10 DEG C of Deca step（1）The diazol obtaining, keeps pH value little for 8-9 reaction 3
When, it is warming up to 65-70 DEG C and is incubated 2 hours, filter to obtain 18 grams of intermediate product filter cake.
（3）In 250mL there-necked flask, add 80 grams of water, above-mentioned intermediate product filter cake, after stirring, add 2 grams
Sodium hydroxide, 0.5 gram of tetrabutyl ammonium bromide, are warming up to 6.15 grams of 70-85 DEG C of Deca N-Propyl Bromide, insulation reaction disappears to intermediate product
Lose, cooling, filter and be washed to neutrality, dry, obtain 18.5 grams of dyestuff dry product.
By above-mentioned same synthetic method, you can obtain dyestuff A2 and A3.
The preparation of compound B-11：（1）100 grams of water, 2- nitro -4- MEA 8.3 is added in 250mL there-necked flask
Gram, mass percent concentration be 36% 20 grams of hydrochloric acid, be stirred at room temperature 0.5 hour, on the rocks be cooled to 0-5 DEG C, Deca quality is divided
17.8 grams of the sodium nitrite solution for 20% for the number, then proceedes to react 2 hours at 0-5 DEG C, is subsequently adding 0.5 gram of sulfamic acid,
With starch potassium iodide paper test colourless after, that is, obtain diazol and treat coupling.
（2）200 grams of water, 6 grams of concentrated sulphuric acid, N- cyanoethyl-N- methoxy ethyl aniline 10.5 is added in 1000mL beaker
Gram, after stirring and dissolving, it is maintained at 0-5 DEG C of Deca step（1）The diazol obtaining, and react 3 hours in this temperature, heat up
It is incubated 2 hours to 65-70 DEG C, filter to obtain intermediate product filter cake, 18 grams of product product filter cake of giving money as a gift.
By above-mentioned same synthetic method, you can obtain dyestuff B2, B3, B4 and B5.
The preparation of compound C1：（1）100 grams of water, 6.9 grams of 4- nitroaniline, quality hundred is added in 250mL there-necked flask
Point specific concentration is 36% 20 grams of hydrochloric acid, is heated to 60 DEG C and stirs 0.5 hour, on the rocks after being down to room temperature be cooled to 0-5 DEG C, Deca
Mass fraction is 20% 17.8 grams of sodium nitrite solution, then proceedes to react 2 hours at 0-5 DEG C, is subsequently adding 0.5 gram of amino
Sulfonic acid, with starch potassium iodide paper test colourless after, that is, obtain diazol and treat coupling.
（2）1000mL beaker adds 7 grams of the sodium hydroxide that 200 grams of water, mass fraction are 30%, 8.7 grams of sodium carbonate,
4.8 grams of phenol, after stirring half an hour, is maintained at 0-10 DEG C of Deca step（1）The diazol obtaining, keeps pH value to react 3 for 8-9
Hour, it is warming up to 65-70 DEG C and is incubated 2 hours, filter to obtain 11 grams of intermediate product filter cake.
（3）In 250mL there-necked flask, add 80 grams of water, above-mentioned intermediate product filter cake, after stirring, add 2 grams
Sodium hydroxide, 0.5 gram of tetrabutyl ammonium bromide, are warming up to 6.8 grams of 80-95 DEG C of Deca benzyl chloride, insulation reaction disappears to intermediate product
Lose, cooling, filter and be washed to neutrality, dry, obtain 14 grams of dyestuff dry product.
By above-mentioned same synthetic method, you can obtain dyestuff C2, C3, C4, C5 and C6.
Embodiment 1
By 20 grams of the former dyestuff shown in 20 grams of the former dyestuff shown in 10 grams of the former dyestuff shown in formula A1, formula B4, formula C3, dispersion
MF60 gram of agent, 15 grams of sodium lignin sulfonate, 153 gram one of water are reinstated sand mill and are carried out decentralized processing, then is spray-dried, and obtain final product this
Bright bright yellow dye mixture.
Embodiment 2～30
According to the preparation method of embodiment 1, the compound shown in formula A, B, C is ground by the data as shown in table 1 below
Mill dispersion, spray drying.
Table 1
Effect example 1
Respectively taking the disperse dyes that 0.5 gram of embodiment 1-30 is obtained to be dispersed in 500 milliliters of water becomes dye suspensions, draws
25 milliliters of suspensions are mixed with 25 milliliters of water, adjust Value in Dyeing Process for 4 with acetic acid, are warming up to 60 DEG C, are respectively put into 2.5 grams of polyester
Fiber cloth, was warming up to 130 DEG C in 30 minutes, was incubated 50 minutes, and cooling is fully washed, dried up.
By above-mentioned colouring method, it is right that the disperse dyes that embodiment 1-30 is obtained are carried out respectively in the dye bath of different pH value
Than dyeing.Value in Dyeing Process is respectively 5.5,9,11,12,13（When pH value is 14, polyester fiber cloth is damaged after high-temperature pressure dyeing
Seriously, thus do not choose pH value and tested for 14）, and respectively added with 6g/L30% hydrogen peroxide.
Above-mentioned dyeing cloth specimen is tested respectively by GB/T3921-2008, GB/T3920-2008, GB/T5718-1997 standard
Its water-fastness, rub resistance and sub-limation fastness.Test result is shown in Table 2, is 4 wherein all with Value in Dyeing Process and is not added with hydrogen peroxide
Dyeing cloth specimen is as standard.
Comparative example
Take the disperse dyes of preparation example 2 described in 0.5 gram of CN102250485A, test its alkali resistance and resistance to by ibid method
Oxidation susceptibility, and water-fastness, rub resistance and sub-limation fastness.Result is also shown in Table 2 below.
Table 2
（Numerical value in wash durability, crocking resistance and sub-limation fastness in upper table is series）
As can be seen from the above table, the disperse dyes of the present invention can use in the basic conditions, and resistance to hydrogen peroxide oxidation
Stability also fine, its wash durability, crocking resistance and sub-limation fastness are all preferable, and the dyestuff of comparative example is strong
Resistance to oxidation stability under alkalescence condition is not ideal enough, is worse than the disperse dyes of the present invention.
Effect example 2
The conventional printing technology of dispersion：Respectively take the disperse dyes that 1.5 grams of embodiments 1-30 are obtained, respectively with 1 gram of reservehao S
（M-nitrobenzene sulfonic acid）, 2 grams of carbamide, 70 gram mass fractions be 8% sodium alginate former paste mixing, add water to total amount and be 100 grams,
And pH value is adjusted to as 5-6 with proper amount of acetic acid, after stirring, to polyester cotton（T65/C35）Carry out stamp, dry
After 170 DEG C of decatizes 7 minutes, washing, soap, dry.
The active Graft versus host disease technique of dispersion：Respectively take the disperse dyes that 1.5 grams of embodiments 1-30 are obtained, respectively with 2 grams of carbonic acid
Hydrogen sodium, 1 gram of reservehao S（M-nitrobenzene sulfonic acid）, 2 grams of carbamide, 70 gram mass fractions be 8% sodium alginate former paste mixing, add water
It is 100 grams to total amount, after stirring, to polyester cotton（T65/C35）Carry out stamp, dry after 102 DEG C of vapour
Steam 8 minutes, then bake 2 minutes in 190 DEG C, washing, soap, dry.
With the cloth specimen of conventional printing technology gained as standard, the disperse dyes Graft versus host disease cloth that testing example 1-30 is obtained
The coloured light of sample and intensity.Test its fastness to rubbing by GB/T3920-2008 respectively, the results are shown in Table 3.
Table 3
As can be seen here, the disperse dyes of the present invention, because having excellent alkali resistance and resistance to oxidation stability, are lived using dispersion
Property Graft versus host disease technique the effect consistent with conventional printing technology be can reach on coloured light, intensity and fastness.
Claims (9)
1. a kind of preparation method of the disperse dyes C of alkali dyeing, it comprises the steps：By compound VI and compounds X-
R2Carry out substitution reaction, you can；
Wherein, R1For-H ,-CH3、-C2H5、-OCH3Or-OC2H5, R2For C1-C4Straight or branched alkyl or benzyl, R8For C1-C4Directly
Chain or branched alkyl, nitro ,-NHCOCH3Or-NHCOC2H5, R9And R10Alone for-H, halogen or nitro, X is halogen；
Described disperse dyes C does not include following compound：
2. preparation method as claimed in claim 1 is it is characterised in that described R1For-H or-CH3；Described R2For propyl group,
Butyl or benzyl；Described R8For methyl, ethyl, nitro or-NHCOCH3；Described R9For-H ,-Br or nitro；Described R10
For-H ,-Br or nitro.
3. preparation method as claimed in claim 1 is it is characterised in that described disperse dyes C is as formula C ', C ", C " ' or
Compound shown in C " ",
Wherein, the definition of each substituent group is all with described in claim 1 or 2.
4. preparation method as claimed in claim 3 it is characterised in that described disperse dyes C be as formula C1, C3, C4, C5 or
Compound shown in C6,
5. preparation method as claimed in claim 1 is it is characterised in that described preparation method comprises the steps：In water,
In the presence of sodium hydroxide and tetrabutyl ammonium bromide, compound VI and compounds X-R2Carry out substitution reaction, you can.
6. preparation method as claimed in claim 5 is it is characterised in that described compound VI and described compounds X-R2's
Mol ratio is (1:1)～(1:1.5)；Described sodium hydroxide is (1 with the mol ratio of described compound VI:1)～(1.6:
1)；Described tetrabutyl ammonium bromide is (0.002 with the mol ratio of described compound VI:1)～(0.05:1)；Described replacement
The temperature of reaction is 65～100 DEG C.
7. preparation method as claimed in claim 1 is it is characterised in that described compound VI is obtained by following methods：In Asia
In the presence of sodium nitrate, compound VII and compound III carries out diazo coupling reaction, that is, obtain compound VI；
8. preparation method as claimed in claim 7 is it is characterised in that described compound VI is obtained by following methods：In salt
In acid, in the presence of sodium nitrite, there is diazo-reaction in compound VII, then in the presence of sodium carbonate and sodium hydroxide,
Carry out coupling reaction with compound III, that is, obtain compound VI.
9. preparation method as claimed in claim 8 is it is characterised in that in the method for prepare compound VI, described nitrous
Sour sodium is (1.01 with the mol ratio of described compound VII:1)～(1.3:1)；The mass percent concentration of described hydrochloric acid is
30%～36%, described hydrochloric acid is (2.5 with the mol ratio of described compound VII:1)～(4.5:1)；Described diazotising
The temperature of reaction is 0～5 DEG C；The time of described diazo-reaction is 3～5h；Described compound III and described chemical combination
The mol ratio of thing VII is (1.01:1)～(1.15:1)；Described sodium carbonate is (1 with the mol ratio of described compound VII:
1)～(1.2:1)；Described sodium hydroxide is (1.5 with the mol ratio of described compound VII:1)～(2.0:1)；Described
The temperature of coupling reaction is 0～10 DEG C.
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