CN101130642A - Method of producing high-strength active yellow 3R - Google Patents
Method of producing high-strength active yellow 3R Download PDFInfo
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- CN101130642A CN101130642A CNA2007100587326A CN200710058732A CN101130642A CN 101130642 A CN101130642 A CN 101130642A CN A2007100587326 A CNA2007100587326 A CN A2007100587326A CN 200710058732 A CN200710058732 A CN 200710058732A CN 101130642 A CN101130642 A CN 101130642A
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- soda ash
- urea
- anilide
- yellow soda
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Abstract
The invention discloses a preparing method of high-intensity active yellow 3R (190%), which comprises the following steps: adopting raw material desalinization; adding into sodium carbonate with pH value at 6. 0-8. 0; filtering; reclaiming filter liquor; using repeatedly; diazotizing without muriatic acid; adding ice grinding aids into one-step condensation step; controlling temperature of the two-step condensation step at 50 deg. c; controlling pH value of sodium carbonate at 4. 0-5. 0; using 2-naphthylamine-3, 6, 8-triple sulfonic acid self acidity; proceeding diazotization without acid; decreasing the added quantity of inorganic acid. This invention possesses low cost and simple craft, which is fit for cotton, silk, leather and polyamide-ester fiber.
Description
Technical field
The present invention relates to active dye technical field, particularly be high-strength active yellow 3 R (190%) preparation method.
Background technology
Reactive dyestuffs have lovely luster, application performance excellence, distinguishing feature such as easy to use, practical.Along with the enhancing of people's environmental consciousness, country is to the raising of environmental requirement, and ecotope is compeled especially, reduces wastewater discharge and qualified discharge, has been the top priority of Chemical Manufacture.
A kind of high strength yellow dyes is arranged at present, and its molecular structure is:
Molecular formula: C
28H
20Cl
1N
9Na
4O
16S
5Molecular weight: 1026.25, dye industry is referred to as active yellow 3 R.The intensity of this dyestuff can reach 190%.High strength colorant dissolubility height, without heat temperature raising both solubilized, and temperature raises and easily to make the active group hydrolysis during use.Use high-strength active yellow 3 R both to save the energy, protected active group again, avoided the disadvantage that causes the dye fixing rate to descend because of the active group hydrolysis.
The preparation method of active yellow 3 R is as follows now:
1, the preparation of a urea anilide: urea anilide hydrochloride between in water, adding, stir, normal temperature is used sodium carbonate regulating solution pH=6-8 down, prepares coupling.
2, diazotization: add 2-amino naphthalenes-3.6.8-trisulfonic acid in water, making beating adds ice, and controlled temperature＜5 ℃ add hydrochloric acid and Sodium Nitrite, react 2 hours, and it is little excessive that Sodium Nitrite keeps.
3, coupling: the diazonium salt reaction solution of step 2 is joined in the soup compound of step 1, and coupled reaction is standby more than 1 hour.
4, a step condensation: in mixture of ice and water, add cyanuric chloride, add the good para-ester solution of dissolving in advance then,, control pH=2.0-5.0, reacted 4--5 hour with yellow soda ash with 0-5 ℃ of ice controlled temperature.
5, two step condensations: in the condenses of step 4, add step 3 coupling solution, finish.55 ℃ of intensification are controlled pH=6.0-7.0 with yellow soda ash simultaneously, react 6--8 hour.
6, in the reaction solution of step 5, add the Repone K of cumulative volume 20%, saltoutd 2 hours, filter.Filter cake drying, pulverizing, stdn make finished product.Filtrate need be administered as waste water.
7, do not adopt step 6, then the reaction solution of step 5 is handled and carried out desalination with receiving membrane filtration, this process need constantly adds clear water, thereby produces saliferous dialyzate waste water.Wastewater flow rate equates approximately that with total liquor capacity colourity still needs to administer more than 1000.
Existing technology exists not enough: adopt the filtration process of saltouing to make, or adopt the nanofiltration membrane desalting treatment.The wastewater discharge of these two kinds of technologies is bigger, and the colourity height is unfavorable for environment protection treating, and preparation cost is higher.
Summary of the invention
At defective such as side reaction in stock yard urea aniline saltiness height and the building-up reactions in the prior art processes is more, the present invention proposes to adopt raw material desalination method bonded synthetic method, realize the magma spray-drying process, reach active yellow 3 R 190% specification of quality, and do not have the purpose of processing wastewater or micro-waste water.
The present invention realizes by following measure, method of producing high-strength active yellow 3 R, comprise that a preparation of urea anilide, diazotization, a step condensation, two step condensations, the wet assembly mix drying step, wherein: a urea anilide preparation in, adopt the raw material desalination, add yellow soda ash, pH=6.0～8.0, filter, the filtrate recovery set is used; In the diazotation step: do not add hydrochloric acid, direct diazotization; In the one step condensation step: add the ice milling aid; In the two step condensation steps: controlled temperature 48--55 ℃, control pH=4.0～5.0 with yellow soda ash.
Technology concrete steps of the present invention are as follows:
1. the preparation of a urea anilide: urea anilide hydrochloride between in water, adding, stir, with sodium carbonate regulating solution pH=6～8, this time urea anilide is separates out shape to normal temperature down.After filtering, NaCl is removed with the aqueous solution.It is standby that filter cake adds the water making beating.Filtrate contain input amount 4～6% between the urea anilide, can be directly used in the synthetic of conventional active yellow 3 R, need not handle.
2. diazotization: add 2-amino naphthalenes-3.6.8-trisulfonic acid in water, making beating adds ice and Sodium Nitrite, and 0～5 ℃ of controlled temperature react 1～2 hour, and the maintenance Sodium Nitrite is little excessive.
3. coupling: the diazonium salt reaction solution of step 2 is joined in the soup compound of step 1, control pH=6.0～7.0 with yellow soda ash, coupled reaction is standby more than 1 hour.
4. a step condensation: in mixture of ice and water, add ice milling aid and cyanuric chloride, add the good para-ester solution of dissolving in advance then, finish,, control pH=2.0～5.0, reacted 4～5 hours with yellow soda ash with 0～5 ℃ of ice controlled temperature.
5. two step condensations: in the condenses of step 4, add step 3 coupling solution, finish.50 ℃ of intensification are controlled pH=4.0～5.0 with yellow soda ash simultaneously, react 6～8 hours.
6. wet the assembly mixes: add dispersing agent NNO in the reaction solution of step 5, adjust intensity to 190%, and with hydrochloric acid or yellow soda ash control pH=5.0～6.0, to be dried.
7. spraying drying: send the spray-drying tower spraying drying with the dye solution behind the above-mentioned wet assembly mixing lattice, temperature out is controlled at 90～100 ℃.Dry back is packing directly, promptly gets desired product.
The present invention adopts the raw material desalination method, and the aqueous solution that will contain a small amount of raw material reclaim to use, and utilizes self acidity of 2-amino naphthalenes-3.6.8-trisulfonic acid to carry out diazotization simultaneously, no longer adds acid, has reduced the add-on of mineral acid.By taking these measures, improve dye strength, lower isomer content, can not reach the standard substance requirement thereby need not make with extra care.The direct spraying drying of dye solution magma has been eliminated processing wastewater.The novel process low cost of manufacture, technology is simple, and does not have processing wastewater.The present invention is applicable to the dyeing and the stamp of cotton, hair, silk, leather, polyesteramide fibre and other mixed fibres.Has good dissemination.
Embodiment
1, technical recipe:
| Material name | Molecular weight | Molecular ratio | 100% consumption | Content | Actual amount | Water at the bottom of the change material |
| Kg | % | Kg | Kg | |||
| Between urea anilide hydrochloride | 187.5 | 1.05 | 724.8 | 84.00% | 862.9 | 2,500.0 |
| 2-amino-benzene-3.6.8-trisulfonic acid | 383.0 | 1.00 | 1,410.0 | 73.00% | 1,931.5 | 2,800.0 |
| Cyanuric chloride | 184.5 | 1.01 | 686.0 | 98.00% | 700.0 | 1,500.0 |
| Para-ester | 281.0 | 1.03 | 1,065.5 | 96.00% | 1,109.9 | 2,800.0 |
| Sodium Nitrite | 69.0 | 1.00 | 254.0 | 96.00% | 264.6 | |
| Yellow soda ash | 106.0 | Consumption is as the criterion so that the pH value is qualified | ||||
| Diffusant | Consumption is as the criterion so that product strength is qualified. | |||||
2, the preparation of a urea anilide: urea anilide hydrochloride between in water, adding, stir, with sodium carbonate regulating solution pH=6～8, this time urea anilide is separates out shape to normal temperature down.After filtering, NaCl is removed with the aqueous solution.It is standby that filter cake adds the water making beating.Filtrate contain input amount about 4～6% between the urea anilide, this part filtrate can not need be handled, direct reuse is synthetic in conventional active yellow 3 R.
3, diazotization: add 2-amino naphthalenes-3.6.8-trisulfonic acid in water, making beating adds ice and Sodium Nitrite, and 0～5 ℃ of controlled temperature reacted 1～2 hour, keeps Sodium Nitrite little excessive.
4, coupling: the diazonium salt reaction solution of step 2 is joined in the soup compound of step 1, control pH=6.0～7.0 with yellow soda ash, coupled reaction 1--2 hour standby.
5, a step condensation: in mixture of ice and water, add ice milling aid and cyanuric chloride, add the good para-ester solution of dissolving in advance then, finish,, control pH=2.0～5.0, reacted 4～5 hours with yellow soda ash with 0～5 ℃ of ice controlled temperature.
6, two step condensations: in the condenses of step 4, add step 3 coupling solution, finish.The 48--55 of intensification ℃, control pH=4.0～5.0 with yellow soda ash simultaneously, reacted 6～8 hours.
7, the wet assembly mixes: add dispersing agent NNO in the reaction solution of step 5, adjust intensity to 190%, and with hydrochloric acid or yellow soda ash control pH=5.0～6.0, to be dried.
8, spraying drying: send the spray-drying tower spraying drying with the dye solution behind the above-mentioned wet assembly mixing lattice, temperature out is controlled at 90～100 ℃.Dry back is packing directly, promptly gets desired product.
Experimental result: this magma spray art result that compares with saltout technology or membrane filtration process is as follows:
| The technology title | Wastewater discharge M 3/ ton product | The wastewater treatment expense is compared | Can reclaim use after the waste water simple process | Product coloured light and intensity |
| The technology of saltouing | 4.0 | High | Not | Qualified |
| Membrane filtration process | 3.2 | Lower slightly | Not | Qualified |
| The magma spray art | 0 | 0 | Can | Coloured light is bright-coloured |
Conclusion: this magma drying process with atomizing with saltout or membrane filtration process is compared, have following advantage: the yellow 3R190% coloured light that present technique is produced is bright-coloured, and cost is low, no processing wastewater discharges.A small amount of colorful wastewater that washing equipment produces in the production can be recycled through flocculation sediment.
Open and high-strength active yellow 3 R (190%) preparation method that proposes of the present invention, those skilled in the art can be by using for reference this paper content, and links such as appropriate change raw material, processing parameter, processing step realize.Method of the present invention and technology are described by preferred embodiment, person skilled obviously can be in not breaking away from content of the present invention, spirit and scope to method as herein described with technology is changed or suitably change and combination, realize the technology of the present invention.Special needs to be pointed out is, the replacement that all are similar and change apparent to those skilled in the artly, they are regarded as being included in spirit of the present invention, scope and the content.
Claims (2)
1. method of producing high-strength active yellow 3 R, comprise that a preparation of urea anilide, diazotization, a step condensation, two step condensations, the wet assembly mix drying step, it is characterized in that: A) the urea anilide preparation in, adopt the raw material desalination, add yellow soda ash, filter pH=6.0～8.0, and the filtrate recovery set is used; B) in the diazotation step: do not add hydrochloric acid, direct diazotization; C) in the step condensation step: add the ice milling aid; D) in the two step condensation steps: controlled temperature 48--55 ℃, control pH=4.0～5.0 with yellow soda ash.
2. method of producing high-strength active yellow 3 R as claimed in claim 1 is characterized in that the method for institute's art is:
1) preparation of urea anilide between: urea anilide hydrochloride between in water, adding, stir, with sodium carbonate regulating solution pH=6～8, this time urea anilide is separates out shape to normal temperature down, and after filtering, NaCl is removed with the aqueous solution, and it is standby that filter cake adds the water making beating;
2) diazotization: add 2-amino naphthalenes-3.6.8-trisulfonic acid in water, making beating adds ice and Sodium Nitrite, and 0～5 ℃ of controlled temperature reacted 1～2 hour, keeps Sodium Nitrite little excessive;
3) coupling: the diazonium salt reaction solution of step 2 is joined in the soup compound of step 1, control pH=6.0～7.0 with yellow soda ash, coupled reaction 1--2 hour standby;
4) a step condensation: in mixture of ice and water, add ice milling aid and cyanuric chloride, add the good para-ester solution of dissolving in advance then, finish,, control pH=2.0～5.0, reacted 4～5 hours with yellow soda ash with 0～5 ℃ of ice controlled temperature;
5) two step condensations: in the condenses of step 4, add step 3 coupling solution, finish.Be warming up to 48--55 ℃, control pH=4.0～5.0 with yellow soda ash simultaneously, reacted 6～8 hours;
6) the wet assembly mixes: add dispersing agent NNO in the reaction solution of step 5, adjust intensity to 190%, and with hydrochloric acid or yellow soda ash control pH=5.0～6.0, to be dried;
7) dye solution after qualified send the spray-drying tower spraying drying, and temperature out is controlled at 90～100 ℃.Dry back is packing directly, promptly gets desired product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100587326A CN100537671C (en) | 2007-08-14 | 2007-08-14 | Method of producing high-strength active yellow 3R |
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|---|---|---|---|
| CNB2007100587326A CN100537671C (en) | 2007-08-14 | 2007-08-14 | Method of producing high-strength active yellow 3R |
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| CN101130642A true CN101130642A (en) | 2008-02-27 |
| CN100537671C CN100537671C (en) | 2009-09-09 |
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| CNB2007100587326A Expired - Fee Related CN100537671C (en) | 2007-08-14 | 2007-08-14 | Method of producing high-strength active yellow 3R |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101481525B (en) * | 2008-12-12 | 2013-01-16 | 天津德凯化工股份有限公司 | Preparation of reactive red GN dye for fur |
| CN101481522B (en) * | 2008-12-12 | 2013-01-16 | 天津德凯化工股份有限公司 | Preparation of red reactive dye for fur |
| CN102898857A (en) * | 2012-09-27 | 2013-01-30 | 汤宝祥 | Circulation applying process for mother liquor waste water of coupling reaction |
-
2007
- 2007-08-14 CN CNB2007100587326A patent/CN100537671C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101481525B (en) * | 2008-12-12 | 2013-01-16 | 天津德凯化工股份有限公司 | Preparation of reactive red GN dye for fur |
| CN101481522B (en) * | 2008-12-12 | 2013-01-16 | 天津德凯化工股份有限公司 | Preparation of red reactive dye for fur |
| CN102898857A (en) * | 2012-09-27 | 2013-01-30 | 汤宝祥 | Circulation applying process for mother liquor waste water of coupling reaction |
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| Publication number | Publication date |
|---|---|
| CN100537671C (en) | 2009-09-09 |
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Address after: 300163 Tianjin city Dongli District ZhangGuiZhuang road Ji'an Road Patentee after: Tianjin Dekai Chemical Industry Co., Ltd. Address before: 300163 Tianjin city Dongli District ZhangGuiZhuang road Ji'an Road Patentee before: Tianjin Dekai Chemical Co., Ltd. |
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Denomination of invention: Method of producing high-strength active yellow 3R Effective date of registration: 20120711 Granted publication date: 20090909 Pledgee: Bank of Dalian Co Tianjin branch Pledgor: Tianjin Dekai Chemical Industry Co., Ltd. Registration number: 2012990000366 |
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