CN100595236C - Preparation process for directly blended spinning navy D-R dye - Google Patents
Preparation process for directly blended spinning navy D-R dye Download PDFInfo
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- CN100595236C CN100595236C CN200810107102A CN200810107102A CN100595236C CN 100595236 C CN100595236 C CN 100595236C CN 200810107102 A CN200810107102 A CN 200810107102A CN 200810107102 A CN200810107102 A CN 200810107102A CN 100595236 C CN100595236 C CN 100595236C
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Abstract
The invention relates to a process for preparing a directly blended atroceruleous D-R dye, mainly comprising a diazo reaction, a primary coupling reaction, a secondary diazo reaction and a secondary coupling reaction. Compared with the prior process, the process has no intermediate purification step, which means the solution of the first coupling reaction undergoes the secondary diazo reaction directly. As the purification step is not required, the process greatly reduces the discharge of dyeing waste water, saves energy and man hour, and has the advantages of saving money, creating practicaleffect, along with simpleness and safety.
Description
Technical field
The present invention relates to a kind of preparation technology's of direct blending dark blue dye, particularly a kind of direct blended spinning navy D-R preparation technology.
Background technology
Directly blended spinning navy D-R is to support to wash/cotton, the new dye of washing/glue mixed fibre " goes on foot single bath process " dyeing, by washing of supporting of direct blended spinning navy D-R/cotton, wash/glue mixed fibre " goes on foot single bath process " dyeing, can significantly reduce the dyeing waste water quantity discharged, energy efficient, save man-hour, have advantages such as technology is easy, safe, economical, actual effect.In addition, it still is one of direct blend dye three-primary colours, not only can solid shade dyeing but also can piece together the union dyeing look with other direct blend dyes, and wide application, usage quantity is big.
Directly the structural formula of blended spinning navy D-R is as follows:
In the prior art, directly the preparation of blended spinning navy D-R mainly comprises the steps:
(1), diazotization reaction, 4, diazotization reaction takes place and generates diazonium salt in 4 '-diamino-2 '-sulfonic acid pentanoic under the effect of hydrochloric acid and Sodium Nitrite;
(2), a linked reaction, mix 1-naphthlamine-6-sulfonic acid sodium salt generation linked reaction with 1.6 and 1.7 by the diazonium salt of step (1) gained and generate a coupled product, wherein, diazonium salt mixes the 1-naphthlamine-6-sulfonic acid sodium salt with 1.6 and 1.7 mol ratio is 1: 2;
(3), purification process, remove do not react 1.6 and 1.7 mix the 1-naphthlamine-6-sulfonic acid sodium salts;
(4), the secondary diazotization reaction, coupled product generation diazotization reaction generates secondary diazonium product;
(5), the secondary linked reaction, the reaction of described secondary diazonium product and J acid sodium-salt generates and has the as above secondary coupled product of structural formula, this secondary coupled product through heat up, 5～8% sodium-chlor separate out, filter, filter cake dry finished product
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation technology of direct blended spinning navy D-R, and this preparation technology does not have the intermediate purification operation, can significantly reduce the dyeing waste water quantity discharged.
For solving above technical problem, the technical solution used in the present invention is:
A kind of preparation technology of direct blended spinning navy D-R dye, described direct blended spinning navy D-R has following structural formula:
This technology is made up of following steps:
(1), diazotization reaction: 4,4 '-diamino-2 '-sulfonic acid pentanoic generation diazotization reaction generates diazonium salt;
(2), linked reaction: mix 1-naphthlamine-6-sulfonic acid sodium salt generation linked reaction with 1.6 and 1.7 by the diazonium salt of step (1) gained and make coupled product solution one time, wherein, 1.6 with 1.7 mixing 1-naphthlamine-6-sulfonic acid sodium salts and 4,4 '-diamino-2 '-sulfonic acid pentanoic mol ratio is 1.96～1.98: 1;
(3), secondary diazotization reaction: add hydrochloric acid, Sodium Nitrite in coupled product solution of step (2) gained, under 12～15 ℃ of temperature, insulation reaction made secondary diazonium product solution in 3～5 hours;
(4), the secondary linked reaction: the reaction of described secondary diazonium product solution and J acid sodium-salt, make and have the as above solution of the secondary coupled product of structural formula, this solution saltouts, filters, dry described direct blended spinning navy D-R dye.
Because the technique scheme utilization, the present invention compared with prior art has following advantage:
The present invention is on the basis of the traditional technology of the direct blended spinning navy D-R dye of preparation, condition to each step reaction is optimized, particularly the proportioning between the reaction raw materials is improved, got rid of the purification process of original technology intermediate steps, improved the production yield.This technology has been owing to got rid of the intermediate purification operation, can significantly reduce dyeing waste water quantity discharged, energy efficient, saving man-hour, has advantages such as technology is easy, safe, economical, actual effect.
Embodiment
Below the specific embodiment of the present invention is described:
Preparation technology according to the direct blended spinning navy D-R of present embodiment is made up of following four steps successively:
(1), diazotization reaction: with 0.05mol 4, the hydrochloric acid of 4 '-diamino-2 '-sulfonic acid pentanoic and water, 0.25mol is mixed, become suspensoid after 30 minutes, add ice-cooled after 0～5 ℃, add the 0.05mol sodium nitrite solution, carry out diazotization reaction, control reaction temperature is between 0～5 ℃, and 2 hours reaction times got a diazonium product.
(2), linked reaction: 0.098mol 1.6 and 1.7 mixes 1-naphthlamine-6-sulfonic acids and dissolve in alkaline aqueous solution and form mixing 1-naphthlamine-6-sulfonic acid solution.To join by the diazonium product that (1) obtains and mix in the 1-naphthlamine-6-sulfonic acid solution, 10～15 ℃ of temperature, pH 6.8, material is the reddish-brown suspensoid, reacts to get a coupled product solution in 6～8 hours;
(3), secondary diazotization reaction: in by coupled product solution of step (2) gained, add ice-cooled, add the hydrochloric acid of 0.329mol, the Sodium Nitrite of 0.101mol, under 13～15 ℃, carry out diazotization reaction, reacted 3 hours to such an extent that Dark grey suspension is secondary diazonium liquid;
(4), secondary linked reaction: the J acid of getting 0.1mol, water and soda ash are dissolved into liquid, on the rocks and add coupling soda ash 0.394mol and form the J acid solution, to slowly join by the secondary diazonium liquid of step (3) gained then and carry out linked reaction in the J acid solution, keep being reflected under 5～8 ℃ of the pH 8.5～9.0, temperature and carry out, react after 2 hours, adding 5～8% sodium-chlor by cumulative volume saltouts, filters, after filter cake oven dry, the markization, get 100% intensity finished product 238g, quality conformance with standard product.
For the present invention and traditional technology are compared, carried out the contrast experiment, the contrast experiment is as follows:
A kind of technology according to the direct blended spinning navy D-R of traditional preparation process comprises the steps:
(1), diazotization reaction
With 0.05mol 4, the hydrochloric acid of 4 '-diamino-2 '-sulfonic acid pentanoic and water, 0.25mol is mixed, become suspensoid after 30 minutes, add ice-cooled after 0～5 ℃, add the 0.05mol sodium nitrite solution, carry out diazotization reaction, control reaction temperature is between 0～5 ℃, and 2 hours reaction times got a diazonium product.
(2), linked reaction:
In alkaline aqueous solution, dissolve formation mixing 1-naphthlamine-6-sulfonic acid solution 0.11mol 1.6 and 1.7 mix 1-naphthlamine-6-sulfonic acid, to join by a diazonium product of step (1) gained then and mix in the 1-naphthlamine-6-sulfonic acid solution, 10～15 ℃ of controlled temperature, pH7～7.5, material becomes the reddish-brown suspensoid, reacts to get a coupled product solution in 10 hours;
(3), purify:
To be warming up to 60 ℃ by a coupled product solution of step (2) gained, and add 18% then and salt out filtration, and keep filter cake and be coupled product one time;
(4), secondary diazotization reaction:
Described coupled product successively in the step (3) is mixed with water, regulate pH 7.5～8.0 with liquid caustic soda and make its dissolving, add ice-cooledly, add hydrochloric acid, the 0.1mol Sodium Nitrite of 0.33mol then, carry out the diazotization reaction second time at 8～12 ℃, react 3 hours secondary diazonium liquid;
(5), secondary linked reaction:
J acid with 0.1mol, water and soda ash are dissolved into liquid, add ice-cooled, the described secondary diazonium liquid that adds 0.394mol soda ash then, obtains by step (4), at 5～8 ℃, pH 8.5～9.0, react after 2 hours, add 5～8% sodium-chlor and saltout, filter, the filter cake oven dry, piece together mixed, markization, get 100% intensity finished product 202g and be direct blended spinning navy D-R, quality conformance with standard product.
By more as can be known, preparation technology of the present invention compares with traditional handicraft, the purification in the middle of having reduced Step, and production yield of the present invention is than the traditional handicraft height. Because getting rid of of purification process will certainly be fallen Low discharge of wastewater, energy savings are conducive to environmental protection.
Claims (1)
1, a kind of preparation technology of direct blended spinning navy D-R dye, described direct blended spinning navy D-R has following structural formula:
It is characterized in that: this technology is made up of following steps:
(1), diazotization reaction: 4,4 '-diamino-2 '-sulfonic acid pentanoic generation diazotization reaction generates diazonium salt;
(2), linked reaction: mix 1-naphthlamine-6-sulfonic acid sodium salt generation linked reaction with 1.6 and 1.7 by the diazonium salt of step (1) gained and make coupled product solution one time, wherein, 1.6 with 1.7 mixing 1-naphthlamine-6-sulfonic acid sodium salts and 4,4 '-diamino-2 '-sulfonic acid pentanoic mol ratio is 1.96～1.98: 1;
(3), secondary diazotization reaction: add hydrochloric acid, Sodium Nitrite in coupled product solution of step (2) gained, under 12～15 ℃ of temperature, insulation reaction made secondary diazonium product solution in 3～5 hours;
(4), the secondary linked reaction: the reaction of described secondary diazonium product solution and J acid sodium-salt, make and have the as above solution of the secondary coupled product of structural formula, this solution saltouts, filters, dry described direct blended spinning navy D-R dye.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN200810107102A CN100595236C (en) | 2008-07-09 | 2008-07-09 | Preparation process for directly blended spinning navy D-R dye |
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| CN200810107102A CN100595236C (en) | 2008-07-09 | 2008-07-09 | Preparation process for directly blended spinning navy D-R dye |
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| CN100595236C true CN100595236C (en) | 2010-03-24 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101531831B (en) * | 2009-04-07 | 2012-05-30 | 吴江梅堰三友染料化工有限公司 | Production method of direct blended brown D-RS dye |
| CN102408743B (en) * | 2011-08-10 | 2013-04-17 | 吴江梅堰三友染料化工有限公司 | Production process of direct blending navy blue D-R dye |
| CN109233324A (en) * | 2018-09-17 | 2019-01-18 | 宣城凯欧纺织有限公司 | A kind of dyestuff processing technology for anticorrosion fabric |
| CN112358740B (en) * | 2020-11-06 | 2022-09-20 | 浙江闰土染料有限公司 | Navy blue direct dye and its preparation method and use |
| CN113502067B (en) * | 2021-08-16 | 2023-05-16 | 浙江闰土染料有限公司 | Preparation method of direct blending dye |
| CN115612308B (en) * | 2022-09-08 | 2023-11-17 | 浙江闰土染料有限公司 | Preparation method and application of yellow direct blending dye |
| CN116102898A (en) * | 2023-02-22 | 2023-05-12 | 内蒙古新亚化工有限公司 | Preparation method of direct blending dark blue |
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Address after: 215225 Wujiang City, Jiangsu Province Ping Wang Zhen Mei Yan Shuangqiao Village Patentee after: Suzhou Meiyan Sanyou dye chemical (Group) Co.,Ltd. Address before: 215225 Wujiang City, Jiangsu Province Ping Wang Zhen Mei Yan Shuangqiao Village Patentee before: WUJIANG MEIYAN SANYOU DYESTUFF CHEMICAL Co.,Ltd. |
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Effective date of registration: 20230322 Address after: 017000 Yellow River Road East, Jianshe Road West, municipal road south, Mengxi Town, Etuoke Banner, Ordos City, Inner Mongolia Autonomous Region Patentee after: INNER MONGOLIA MEILIJIAN TECHNOLOGY CHEMICAL CO.,LTD. Address before: 215225 Wujiang City, Jiangsu Province Ping Wang Zhen Mei Yan Shuangqiao Village Patentee before: Suzhou Meiyan Sanyou dye chemical (Group) Co.,Ltd. |