CN101230204A - Orange reactive dye and preparation method thereof - Google Patents
Orange reactive dye and preparation method thereof Download PDFInfo
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- CN101230204A CN101230204A CNA2007103024826A CN200710302482A CN101230204A CN 101230204 A CN101230204 A CN 101230204A CN A2007103024826 A CNA2007103024826 A CN A2007103024826A CN 200710302482 A CN200710302482 A CN 200710302482A CN 101230204 A CN101230204 A CN 101230204A
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Abstract
The invention discloses orange reactive dye and the preparation method thereof. The dye and the structural formula thereof are as follows: the preparation method comprises the following steps: after the unipolycondensation reaction of tricyanogen chloride and cyanamid, the copolycondensation reaction is performed with J acid; Beta sulfuric ester ethyl sulfone amino benzene is diazotized to obtain diazo salt, and then the diazo salt is added into copolycondensation compound to perform the coupling reaction, to obtain mono azo dye; 2amido ethyl-2(1) sulfonyl ethoxyl sulphone is added into mono azo dye solution to perform the tri-polycondensation reaction. The invention has the advantages of high color fixation rate, good building up property and level dyeing property, good sun-proof performance, sweat resistance and washing fastness, which is suitable for the cellulose fiber dying and simultaneously suitable for the fiber dying such as direct viscose and artificial amiray ramie, etc.
Description
Technical field
The present invention relates to a kind of orange active dye and preparation method thereof.
Background technology
The present reactive dyestuffs of producing are halo triazine type normally, and phenylethyl sulfone sulfate type or halo triazine and phenylethyl sulfone sulfate mixed type cause dyeing waste-water colourity big more greatly with the salt amount in dyeing course, and environmental pollution is heavy.Secondly dying when pitch black reactive black KN-B (reactive black 5) commonly used at present pieces together to mix with reactive orange KN-GR (REACTIVE ORANGE 12 9) and forms.It is often not ideal enough that yet this assembly mixes the dyestuff pitch black degree that forms, again because reactive orange KN-GR is the active group of dichlorotriazine and the avidity height of cellulosic fibre, be adsorbed on the fiber earlier, and reactive black KNB colouring is slow, so cause aberration, easily cause the look flower, particularly orange component is easily heavy when adding the alkali fixation carefully separates out, and causes color spot.
Reactive black KNB structure:
Reactive orange KN-GR structure
Summary of the invention:
For addressing the above problem, the present invention provides a kind of orange active dye and preparation method thereof.
Its structural formula of orange dye of the present invention is as follows:
Orange active dye of the present invention can prepare by following process:
Cyanuric chloride and cyanamide carry out two reactions of contracting with J acid again after the reaction of carrying out contracting; To β sulfuric ester ethyl sulfonyl aniline diazotization, diazonium salt, above-mentioned diazonium salt is joined two contracts and carry out coupled reaction in the thing, obtain monoazo-dyes; With 2 amino-ethyl-2 ' alkylsulfonyl hydroxyethyl sulfones join carry out in the monoazo-dyes solution three contract the reaction and get.
One temperature of reaction that contracts is 0-5 ℃, and two contract temperature of reaction 35-40 ℃.
Dyestuff of the present invention contains anionic group, as-SO
3H all represents with free H acid in specification sheets for simplicity, and usually with aqueous solution form, particularly alkali-metal aqueous solution form such as sodium salt, sylvite exist dyestuff of the present invention in producing and using.
The present invention compared with prior art has the following advantages:.
The present invention introduces new active group 2 amino-ethyl-2 ' alkylsulfonyl hydroxyethyl sulfone sulfates and the halo triazine is combined into halo triazine and aliphatics ethyl sulfonyl sulfate mixed type reactive dyestuffs; can improve the dye fixing rate; every fastness such as photostabilization, wash resistant, anti-daylight-sweat fastness are good; can carry out colorant match with reactive black KNB on the one hand; the performance that mixes improves; be difficult for causing the look flower, improve pitch black pitch black degree.
Embodiment:
One contracts: contract in one and put 150 parts of mixture of ice and water in the bucket, add 18.5 parts of 100% cyanuric chlorides, 0 ℃ of making beating 45-60 minute down, drip 4.2 parts of cyanamide solution of 100% then, add 0-5 ℃ of back controlled temperature, it is 7-9 that the NaOH solution with 10% is regulated PH, conditioned reaction 10-40 minute.
Two contract: put into 200 parts in the dissolving bucket, 23.9 parts of the J acid of input 100%, pull an oar after one hour and to regulate PH5.8-6.5 with 10% NaOH liquid, molten clear, and adjust volume control J acid concentration 4-5%, join one then and contract in the thing, intensification 35-40 ℃, and to regulate PH with 15% soda ash liquid be 3-6, reacts 3-4 hour to terminal, and it is standby to reduce to normal temperature.
Diazonium: in the diazonium bucket, put 100 parts of mixture of ice and water, drop into right-(beta-sulfuric ester ethyl sulfonyl) aniline 100% 28.1 parts, pulled an oar 10 minutes, add 12 parts of industrial goods hydrochloric acid, add 6.9 parts of sodium nitrite solutions of 100% then, controlled temperature is 0-5 ℃ simultaneously, finish, excessive nitrous acid was eliminated with thionamic acid after 2 hours in controlled temperature≤10 ℃, the little blue colour response of starch potassium iodide paper.
Coupling: diazonium salt is joined two contract in the liquid, controlled temperature 0-15 ℃, regulating PH with 15% soda ash liquid then is 5.5-6.5, react diazonium salt disappearance in 3 hours.
Three contract: 2 amino-ethyl-2 ' alkylsulfonyl hydroxyethyl sulfone sulfates are joined in the above-mentioned coupling solution, and to regulate PH with 15% soda ash liquid be 6.5-8.5, be warming up to 60-80 ℃ then; controlled temperature and pH value; react 4-5 hour to terminal, and with the dye liquor drying, the theme dyestuff.
Claims (2)
1. orange active dye and preparation method thereof, its structural formula is as follows:
2. the preparation method that dyestuff according to claim 1 is determined, cyanuric chloride and cyanamide 0-5 ℃ carry out contracting react after, carry out two reactions of contracting with J acid in 35-40 ℃ again; To β sulfuric ester ethyl sulfonyl aniline diazotization, diazonium salt, above-mentioned diazonium salt is joined two contracts and carry out coupled reaction in the thing, obtain monoazo-dyes; With 2 amino-ethyl-2 ' alkylsulfonyl hydroxyethyl sulfones join carry out in the monoazo-dyes solution three contract the reaction and get.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007103024826A CN101230204A (en) | 2007-12-26 | 2007-12-26 | Orange reactive dye and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007103024826A CN101230204A (en) | 2007-12-26 | 2007-12-26 | Orange reactive dye and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
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| CN101230204A true CN101230204A (en) | 2008-07-30 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNA2007103024826A Pending CN101230204A (en) | 2007-12-26 | 2007-12-26 | Orange reactive dye and preparation method thereof |
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| CN (1) | CN101230204A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101942214A (en) * | 2010-08-20 | 2011-01-12 | 天津德凯化工股份有限公司 | Orange degreased reactive dye for wool and preparation method thereof |
| CN101942215A (en) * | 2010-08-20 | 2011-01-12 | 天津德凯化工股份有限公司 | Orange reactive dye for wool and preparation method thereof |
| CN102993771A (en) * | 2011-12-13 | 2013-03-27 | 褚平忠 | Preparation method of orange reactive dye |
| CN102993772A (en) * | 2011-12-14 | 2013-03-27 | 褚平忠 | Preparation method of orange reactive dye |
| CN107142753A (en) * | 2017-06-05 | 2017-09-08 | 西安工程大学 | Response type levelling agent and preparation method and application |
| CN109233332A (en) * | 2018-10-31 | 2019-01-18 | 泰兴锦云染料有限公司 | Ink-jet printed active orange of one kind and its preparation method and application |
-
2007
- 2007-12-26 CN CNA2007103024826A patent/CN101230204A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101942214A (en) * | 2010-08-20 | 2011-01-12 | 天津德凯化工股份有限公司 | Orange degreased reactive dye for wool and preparation method thereof |
| CN101942215A (en) * | 2010-08-20 | 2011-01-12 | 天津德凯化工股份有限公司 | Orange reactive dye for wool and preparation method thereof |
| CN102993771A (en) * | 2011-12-13 | 2013-03-27 | 褚平忠 | Preparation method of orange reactive dye |
| CN102993772A (en) * | 2011-12-14 | 2013-03-27 | 褚平忠 | Preparation method of orange reactive dye |
| CN107142753A (en) * | 2017-06-05 | 2017-09-08 | 西安工程大学 | Response type levelling agent and preparation method and application |
| CN107142753B (en) * | 2017-06-05 | 2019-12-10 | 西安工程大学 | Reactive leveling agent and preparation method and application thereof |
| CN109233332A (en) * | 2018-10-31 | 2019-01-18 | 泰兴锦云染料有限公司 | Ink-jet printed active orange of one kind and its preparation method and application |
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Open date: 20080730 |