CN101260245B - Medium black 2B technique - Google Patents
Medium black 2B technique Download PDFInfo
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- CN101260245B CN101260245B CN2008100110699A CN200810011069A CN101260245B CN 101260245 B CN101260245 B CN 101260245B CN 2008100110699 A CN2008100110699 A CN 2008100110699A CN 200810011069 A CN200810011069 A CN 200810011069A CN 101260245 B CN101260245 B CN 101260245B
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Abstract
The invention relates to a technical method of dye, wherein during the technical process of mordant black 2B, neutralization pH value is adjusted from 2 to 3 and temperature is adjusted from the original 3 to 5 DEG C to the prior 8 to 10 DEG C; during salifying reaction, temperature is adjusted from the original 80 to 85 DEG C to the prior 90 to 95 DEG C; during coupling reaction, the molar ratio of saltpeter body and alpha-naphthol is adjusted from 1:1.10 to 1:1, and reaction temperature is adjusted from the original 20 to 25 DEG C to the prior 30 to 35 DEG C; moreover, salt is added during coupling to ensure that coupled dye molecule is formed into hydrate. Because the hydrated dye can not be dissolved in water, water-washing operation can be carried out after acidification to remove impurities, thereby increasing the purity of dye without influencing product yield; moreover, because technical control conditions are improved, product norm of consumption is reduced, which effectively increases market competitiveness and the economic benefits of an enterprise.
Description
Technical field
The present invention relates to a kind of dyestuff synthetic method, relate to the synthetic process of Mordant Black dyestuff specifically.
Background technology
Mordant Black 2B is that a kind of good hair is used dyestuff, and nearly 70 years production history is arranged.China began in Shanghai to produce in the 1950's, and stop production the sixties, had the eighties face south chemical plant and celebrating chemical plant, river, Chongqing, Tianjin to begin to produce again.
The nearly various schools of thinkers of manufacturer is the best with German vapour Ba-Jia Ji company Eriochrome Black T quality both at home and abroad.
Domestic have the tens of families of factory at present, all carry out HG/T 2589-2004 standard, national standard has nothing different with the CIBA product on quality index, but the CIBA product has strict application indexes, home products has a long way to go on the printing and dyeing application performance, and quality is not on a class.Wherein on coupling process, coupled reaction generates coupling unit molecule dyestuff, as wash, coupling unit molecule dyestuff is dissolved in water, the yield of product is reduced, and cost improves, and therefore common coupling process is not washed, owing to do not wash, the foreign matter content height causes quality product inferior in the dyestuff.The report of removing impurity method in the conjugates is not arranged at present as yet.
Summary of the invention
The present invention is directed to the quality problems that existing Mordant Black 2B exists, the present invention proposes a kind of synthetic process that reduces resistates.
The concrete technical measures that solve the problems of the technologies described above are:
The synthetic process of Mordant Black 2B can be divided into neutralization, salify, coupling, acidifying washing, and its reaction principle and processing method are as follows:
Structural formula:
Molecular formula: C
20H
14O
7N
2S
C.I.：Mordant Black 11
CAS NO.：1787-61-7
1 neutralization
Reaction formula:
Operation: in and add the H of 45～50mol in the still
2O stirs and to add nitre body 1mol down, and is then under 8～10 ℃ of conditions, with the NaOH pH=3 that neutralizes, standby.
2 salifies
Reaction formula:
Operation: the H that in becoming salt oven, adds 14～17mol
2O stirs and to add calculated amount NaOH down, is warmed up to 95 ℃, adds first-naphthols 1mol, complete molten after, cool to 50～55 ℃, standby.
3 couplings
Operation: in the coupling still, add the neutralization material earlier, open stirring, add the salify material again, stir 25～30min, add a certain amount of salt, restir 30～35min, coupling is finished, and process control temp is 30～35 ℃.
4 acidifyings, washing
Reaction formula (acidifying):
Operation: after the coupling time arrives, add dilute sulphuric acid, material pH value is transferred to 1～2, then the acidifying material is put into the washing pot that 2～3 times of water are housed, stir 10～15min, squeeze into pressure filter with pump and filter, filter cake removes expansion drying.
The inventive method is compared with the common process method and is made following change:
Neutralization reaction: the pH value is adjusted into 3 by 2, and temperature is transferred to 8～10 ℃ by 3～5 ℃.
Salt-forming reaction: temperature is adjusted to 90～95 ℃ by 80～85 ℃.
Coupled reaction: nitre body and first-naphthols mol ratio was adjusted into 1: 1 by 1: 1.10.
Temperature of reaction is adjusted into 30～35 ℃ by 20～25 ℃.
Increased coupling with salt and filter cake washing step.
Temperature of reaction in the technical solution of the present invention, time are reaction span of control number.
Formed hydrate is C after the coupling
20H
11O
7N
3SNa
2NH
2O, (wherein n 〉=1), this hydrate is removed the bonded water molecules through washing and drying becomes monomolecular product.
Beneficial effect of the present invention: the present invention is because in technological process, in and the pH value be adjusted into 3 by 2, temperature is transferred to 8～10 ℃ by 3～5 ℃.Salt-forming reaction: temperature is adjusted to 90～95 ℃ by 80～85 ℃.Coupled reaction: nitre body and first-naphthols mol ratio was adjusted into 1: 1 by 1: 1.10.Temperature of reaction is adjusted into 30～35 ℃ and add salt in the coupling process by 20～25 ℃, make the dye molecule of coupling form hydrate, this hydration dyestuff is not dissolved in water, therefore can after acidifying, carry out washing operation, remove impurity, improve dyestuffs purity, the yield of product is unaffected, and owing to improve process control condition, the product norm quota of consumption reduces, and effectively improves the market competitiveness and business economic benefit.
Embodiment
Raw material
| Title | Specification (%) | Operative norm | The place of production |
| The nitre body | ≥70 | HG/T 3752-2004 | Dandong |
| First-naphthols | ≥96 | HG/T 3410-1989 | Changzhou |
| Sheet alkali | ≥96 | GB 6009-92 | Shenyang |
| Sulfuric acid | ≥98 | GB 11198-89 | Dalian |
| Refined salt | ≥99.5 | GB 209-93 | Hubei |
Embodiment 1
1 neutralization
Operation: add water 600L in 2000L He in the still, add nitre body 286kg (0.6775mol) under the stirring, then under 8～10 ℃ of conditions, with the liquid caustic soda pH=3 that neutralizes, finishing temperature is 8 ℃, and is standby.
2 salifies
Operation: in becoming salt oven, add water 200L, stir down and add sheet alkali 28kg, be warmed up to 95 ℃, processing industry first-naphthols 98kg (0.6775mol), molten entirely after, cool to 55 ℃, standby.
3 couplings
Operation: in 2000L coupling still, add the neutralization material earlier, open stirring, add the salify material again, stirred 30 minutes, with salt 350kg, restir 30 minutes, coupling is finished, and process control temp is 30～35 ℃.
4 acidifyings, washing
Operation: after the coupling time arrives, add dilute sulphuric acid, material pH value is transferred to 1～2, then the acidifying material is put into the washing pot that 2000L water is housed, stirred 10 minutes, squeeze into pressure filter with pump and filter, filter cake removes expansion drying.
The statistics that the product quality indicator and the product of production detect
The inventive method raw material consumption descends significantly, and comparing result is as follows:
| Material name | Specification | The inventive method (kg/t) | Ordinary method (kg/t) |
| The nitre body | ≥100％ | 392 | 460 |
| First-naphthols | ≥96％ | 196 | 230 |
| Sheet alkali | ≥96％ | 165 | 186 |
| Sulfuric acid | ≥98％ | 67 | 188 |
| Refined salt | ≥99.5％ | 550 | 820 |
Residue compares: ordinary method is:＜1 grade, gained result of the present invention is: 〉=3 grades.
Embodiment 2
1 neutralization
Operation: add water 550L in 2000L He in the still, add nitre body 286kg (0.6775mol) under the stirring, then under 8～10 ℃ of conditions, with the liquid caustic soda pH=3 that neutralizes, finishing temperature is 8 ℃, and is standby.
2 salifies
Operation: in becoming salt oven, add water 180L, stir down and add sheet alkali 28kg, be warmed up to 95 ℃, processing industry first-naphthols 98kg (0.6775mol), molten entirely after, cool to 55 ℃, standby.
3 couplings
Operation: in 2000L coupling still, add the neutralization material earlier, open stirring, add the salify material again, stirred 30 minutes, with salt 350kg, restir 30 minutes, coupling is finished, and process control temp is 30～35 ℃.
4 acidifyings, washing
Operation: after the coupling time arrives, add dilute sulphuric acid, material pH value is transferred to 1～2, then the acidifying material is put into the washing pot that 2100L water is housed, stirred 10 minutes, squeeze into pressure filter with pump and filter, filter cake removes expansion drying, and the residue of gained commercial dye is 2～3 grades.
Embodiment 3
1 neutralization
Operation: add water 580L in 2000L He in the still, add nitre body 286kg (0.6775mol) under the stirring, then under 8～10 ℃ of conditions, with the liquid caustic soda pH=3 that neutralizes, finishing temperature is 10 ℃, and is standby.
2 salifies
Operation: in becoming salt oven, add water 200L, stir down and add sheet alkali 28kg, be warmed up to 95 ℃, processing industry first-naphthols 98kg (0.6775mol), molten entirely after, cool to 53 ℃, standby.
3 couplings
Operation: the material that will neutralize adds in the coupling still, stirs down to add the salify material, continue to stir 30 minutes, and with salt 350kg, restir 30 minutes, coupling is finished, and process control temp is 30～33 ℃, is controlled to be pH=2.
4 acidifyings, washing
Operation: after the coupling time arrives, add dilute sulphuric acid, material pH value is transferred to 1～2, then the acidifying material is put into the washing pot that 1900L water is housed, stirred 10 minutes, squeeze into pressure filter with pump and filter, filter cake removes expansion drying.The residue of commercial dye is the 3-level.
Claims (1)
1. Mordant Black 2B processing method of the present invention is characterized in that:
(1) neutralization: in and add the H of 45～50mol in the still
2O stirs and to add nitre body 1mol down, and is then under 8～10 ℃ of conditions, with the NaOH pH=3 that neutralizes, standby;
(2) salify: the H that in becoming salt oven, adds 14～17mol
2O stirs and to add calculated amount NaOH down, is warmed up to 95 ℃, adds first-naphthols 1mol, complete molten after, cool to 50～55 ℃, standby;
(3) coupling: in the coupling still, add the neutralization material earlier, open stirring, add the salify material again, stir 25～30min, add and press 1: 6.2 refined salt of nitre body mol ratio, restir 30～35min, coupling is finished, and process control temp is 30～35 ℃;
(4) acidifying, washing: after the coupling time arrives, add dilute sulphuric acid, material pH value is transferred to 1～2, then the acidifying material is put into the washing pot that 2～3 times of water are housed, stir 10～15min, squeeze into pressure filter with pump and filter, filter cake removes expansion drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100110699A CN101260245B (en) | 2008-04-18 | 2008-04-18 | Medium black 2B technique |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100110699A CN101260245B (en) | 2008-04-18 | 2008-04-18 | Medium black 2B technique |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101260245A CN101260245A (en) | 2008-09-10 |
| CN101260245B true CN101260245B (en) | 2010-06-02 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008100110699A Active CN101260245B (en) | 2008-04-18 | 2008-04-18 | Medium black 2B technique |
Country Status (1)
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|---|---|
| CN (1) | CN101260245B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109593382A (en) * | 2018-11-20 | 2019-04-09 | 恒升化工有限公司 | A kind of preparation method of red complexing type dye |
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| CN101260245A (en) | 2008-09-10 |
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