CN106590017A - Technology for preparing direct fast yellow RS dye - Google Patents
Technology for preparing direct fast yellow RS dye Download PDFInfo
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- CN106590017A CN106590017A CN201611115826.8A CN201611115826A CN106590017A CN 106590017 A CN106590017 A CN 106590017A CN 201611115826 A CN201611115826 A CN 201611115826A CN 106590017 A CN106590017 A CN 106590017A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B43/00—Preparation of azo dyes from other azo compounds
- C09B43/12—Preparation of azo dyes from other azo compounds by acylation of amino groups
- C09B43/136—Preparation of azo dyes from other azo compounds by acylation of amino groups with polyfunctional acylating agents
- C09B43/14—Preparation of azo dyes from other azo compounds by acylation of amino groups with polyfunctional acylating agents with phosgene or thiophosgene
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a technology for preparing a direct fast yellow RS dye. Compared with the prior art, the technology omits the procedures of salting out, filtration, press filtration, drying, and crushing; primary pulp is employed for direct spray drying, an original auxiliary material is saved, 10-20% of sodium chloride added in proportion in a traditional method is omitted, the products processed by a spray drying tower have good consistency, and have the advantages of time saving, coal saving, electricity saving, and steam saving. The technology has the advantages of clean production and energy saving without waste water discharge in the production technology, and changes the condition of traditional production technology for the direct fast yellow RS dye. the production technology is simplified, production cost is reduced, product quality is effectively increased, product yield is increased, loading and unloading capacity is enlarged, the environment pollution problem due to waste water can be solved, the technology has large business value, and accords with continuous development of environmental protection.
Description
Technical field
The invention belongs to dyestuff preparing technical field, is related to the preparation technology of dyestuff, a kind of especially direct fast yellow RS
Dyestuff preparation technology, the international standard number of direct fast yellow RS is C.I.50.
Background technology
It is bright-coloured HONGGUANG yellow that direct fast yellow RS is used to contaminate cotton or viscose, has good level-dyeing property and migration property, upper dye
Rate is fair, and it is 60 DEG C that temperature is contaminated in highest, and temperature is low, obtains color depth.Can be with direct printing, also can background color discharge.It is mainly used in sticking
The dyeing of collodion silk fabric and stamp.The weightening that silk is resistant to for silk fabrics dyeing is processed, and coloured light is unaffected.Can be additionally used in skin
The coloring of leather, paper and anodized aluminium.
In the traditional processing technology of direct fast yellow RS dyestuffs, usually amido-G-acid is entered with meta-aminotoluene through diazotising
The yellow bass of row coupling synthesis, then be condensed with triphosgene and to form direct fast yellow RS.The synthesis of wherein yellow bass and yellow bass and three
The condensation of phosgene such as is required for saltouing, filter and concentrate at the technical process；Purpose is desalination, removes unreacted raw material, intermediate
And secondary dyestuff, slough moisture, to obtain the dyestuff of desired concn and purity, then carry out oven drying, make powder dye or
Directly preparing becomes liquid dyes.But there is a problem of certain：
1st, in synthesis and salting-out process, the impurity that brings, salinity are summarized and a large amount of affect dyestuffs purities, intensity and dissolubility
Composition, the impurity being only reduced in dyestuff, salinity could improve tinctorial strength and dyestuffs purity of dyestuff etc..
2nd, adopt and saltout or acid out separation dye component, product purity is not high, and the product quality of different batches is consistent
Property is also poor, makes product quality be very limited.
3rd, due to a large amount of Sodium Chloride having been used in salting-out process, can produce substantial amounts of waste water, the discharge of waste water not only makes again
The utility such as the industrial chemicals for wherein containing and intermediate is slatterned, and greatly pollution can be also caused to environment, serious to restrict
The sustainable development of dye industry.
The content of the invention
It is an object of the invention in place of overcoming the deficiencies in the prior art, there is provided a kind of simplified production technology, dyestuff is improved
Quality, direct fast yellow RS dyestuff preparation technologies that are energy-saving, reducing pollution.
The present invention solves its technical problem and takes technical scheme below to realize：
Direct fast yellow RS dyestuff preparation technologies, step are as follows：
(1) amido-G-acid diazotising
Add water in C-acid diazonium pot 3000L, stirring to pulp 30 minutes, then adjusts pH=6-6.5 with soda, and solution is in
Transparency liquid, adds water and is cooled to t=5 DEG C, adds the sodium nitrite solution of hydrochloric acid and 30wt%, with just after reaction 10-15 minutes
Arnotto, sodium iodide detection paper are blue, are acted on 1 hour, and temperature t=16 DEG C ± 2, volume v=6000L, reaction are reached home
Afterwards, adjusted with sulfamic acid and lose excessive nitrous acid, prepare coupling；
(2) meta-aminotoluene material
Add water 2000L in coupling pot, stirring adds sodium bicarbonate, meta-aminotoluene, stir 40 minutes, then on the rocks be cooled to t
=8 DEG C standby；
(3) meta-aminotoluene coupling
The diazo liquid of step (1) is added in meta-aminotoluene mixed liquor, whole process 60 minutes, and it is every during charging
5 minutes pH value of monitoring and temperature, finally require pH=5.5-6, temperature t=10-20 DEG C, volume v=8300L, effect 90
After minute, pH=2.7-3.3 is adjusted back with hydrochloric acid, be stirred overnight, final pH=2.7-3.3 volumes=8500L；
Next day, with t=90 DEG C of intensification in 90 minutes, act on 2 hours at 90 DEG C, be warming up to t=50-55 DEG C of foaming, it is overall
Product V=11200L, adjusts pH=8 with liquid caustic soda, adds activated carbon 5-15kg, is warming up to 80 DEG C, and stirring was filtered after 30 minutes, collects female
Liquid and filtrate wait to be condensed；
(4) triphosgene condensation
Solid phosgene, pH=6 is added to adjust pH=6-6.5 with cold dilute alkali liquid during reaction in the mother solution collected, reaction 3 is little
When after add pyridine, reaction adjusted pH=8-8.5 with liquid caustic soda after 2 hours, and outlet temperature controls 60-70 DEG C, stirs 1-2 hours,
Destroy responseless phosgene, volume v=12000L；
The amido-G-acid：Hydrochloric acid：Sodium nitrite：Meta-aminotoluene：The mol ratio of phosgene is 1:2.4:1.03:0.98:
0.24；
(5) mist projection granulating
The solution that step (4) reaches condensation reaction terminal is directly carried out into mist projection granulating, drying tower setting inlet temperature：
180 DEG C, 80 DEG C of outlet temperature；
(6) finished product.
And, in step (3), hydrochloric acid is 30wt% hydrochloric acid.
The advantages of the present invention are：
1st, the present invention adds 5-15kg activated carbons in the next day of meta-aminotoluene coupling, as excellent adsorbent, significantly increases
Plus dye solubility, purity is improved, accelerates coupling speed, promote coupling effect, it is to avoid the impurity of the generation of saltouing in old technology,
Improve production efficiency, increases production capacity.
2nd, the present invention saves the step saltoutd in the building-up process and follow-up condensation course of yellow bass compared with old technology
Suddenly, in old technology, in yellow bass building-up process, need refined salt to be added by volume 8%, stir 30 minutes, temperature t=18 DEG C ±
2, after acting on 90 minutes, PH=2.7-3.3 (being checked with Congored test paper) is slowly adjusted back with 30% hydrochloric acid, be stirred overnight temperature t
=25--27 DEG C, volume=8500L.Next day was first warming up to t=90 DEG C with 90 minutes, 90 DEG C act on 2 hours, during intensification
50-55 DEG C of foaming cumulative volume V=11200L, adds refined salt by volume V=13%, stirs 40 minutes at 90 DEG C, filter.And it is new
Above-mentioned steps are saved by technique, reduces cost, less operation, and can reach more preferable synthetic effect.
3rd, need refined salt to be added by volume 15-20% in yellow bass and triphosgene condensation course in old technology, saltout 30 points
Clock, filters, and dries 1 hour, increases production cost and processing step, and produces substantial amounts of impurity；And the new technology of the present invention, subtract
The impurity produced in few salting-out process and salinity, further improve purity, intensity and the dissolubility of dyestuff, are avoiding producing impurity
While improve dyestuff degree of staining.
4th, the present invention it is main remove saltout, filter, filter pressing, the operation dried, crushes, using the drying of oleo stock Direct spraying,
Former auxiliary material is saved, saves the 10%-20% Sodium Chloride that traditional method is proportionally added into, spray-dried tower is produced after processing
The concordance of product is good, both saved time, and saved coal, power saving, saves steam etc..
5th, the prominent cleanly production and the advantage of energy saving for embodying non-wastewater discharge in production technology of the present invention, changes
Direct resistance to yellow RS dyestuffs traditional processing technology condition.Typically directly DYE PRODUCTION 300kg/h, the inventive method production 500kg/h-
800kg/h.Simplify production technology, reduce production cost, effectively increase product quality, increased product yield, expand life
Production capacity power, and contaminated wastewater environment is fundamentally solved the problems, such as, with larger commercial value, and meet holding for environmental protection
Supervention exhibition.
Description of the drawings
Fig. 1 is the process chart of the present invention.
Specific embodiment
Below by specific embodiment, the invention will be further described, and following examples are descriptive, is not limit
Qualitatively, it is impossible to which protection scope of the present invention is limited with this.
Technological process such as Fig. 1 of the present invention, dispensing are as follows：
3rd, direct fast yellow RS dyestuffs preparation technology, step are as follows：
(1) amido-G-acid diazotising
Add water in C-acid diazonium pot 3000L, stirring to pulp 30 minutes, then adjusts pH=6-6.5 with soda, and solution is in
Transparency liquid, adds water and is cooled to t=5 DEG C, adds the sodium nitrite solution of hydrochloric acid and 30wt%, with just after reaction 10-15 minutes
Arnotto, sodium iodide detection paper are blue, are acted on 1 hour, and temperature t=16 DEG C ± 2, volume v=6000L, reaction are reached home
Afterwards, adjusted with sulfamic acid and lose excessive nitrous acid, prepare coupling；
(2) meta-aminotoluene material
Add water 2000L in coupling pot, stirring adds sodium bicarbonate, meta-aminotoluene, stir 40 minutes, then on the rocks be cooled to t
=8 DEG C standby；
(3) meta-aminotoluene coupling
The diazo liquid of step (1) is added in meta-aminotoluene mixed liquor, whole process 60 minutes, and it is every during charging
5 minutes pH value of monitoring and temperature, finally require pH=5.5-6, temperature t=10-20 DEG C, volume v=8300L, effect 90
After minute, pH=2.7-3.3 is adjusted back with hydrochloric acid, be stirred overnight, final pH=2.7-3.3 volumes=8500L；
Next day, with t=90 DEG C of intensification in 90 minutes, act on 2 hours at 90 DEG C, be warming up to t=50-55 DEG C of foaming, it is overall
Product V=11200L, adjusts pH=8 with liquid caustic soda, adds activated carbon 5-15kg, is warming up to 80 DEG C, and stirring was filtered after 30 minutes, collects female
Liquid and filtrate wait to be condensed；
(4) triphosgene condensation
Solid phosgene, pH=6 is added to adjust pH=6-6.5 with cold dilute alkali liquid during reaction in the mother solution collected, reaction 3 is little
When after add pyridine, reaction adjusted pH=8-8.5 with liquid caustic soda after 2 hours, and outlet temperature controls 60-70 DEG C, stirs 1-2 hours,
Destroy responseless phosgene, volume v=12000L；
The amido-G-acid：Hydrochloric acid：Sodium nitrite：Meta-aminotoluene：The mol ratio of phosgene is 1:2.4:1.03:0.98:
0.24；
(5) mist projection granulating
The solution that step (4) reaches condensation reaction terminal is directly carried out into mist projection granulating, drying tower setting inlet temperature：
180 DEG C, 80 DEG C of outlet temperature；
(6) finished product.
And, in step (3), hydrochloric acid is 30wt% hydrochloric acid.
Claims (2)
1. direct fast yellow RS dyestuffs preparation technology, it is characterised in that：Step is as follows：
(1) amido-G-acid diazotising
Add water in C-acid diazonium pot 3000L, stirring to pulp 30 minutes, then adjusts pH=6-6.5 with soda, and solution is transparent
Liquid, adds water and is cooled to t=5 DEG C, adds the sodium nitrite solution of hydrochloric acid and 30wt%, after reaction 10-15 minutes with Congo red,
Sodium iodide detection paper is blue, is acted on 1 hour, temperature t=16 DEG C ± 2, volume v=6000L, after reaction is reached home, is used
Sulfamic acid is adjusted and loses excessive nitrous acid, prepares coupling；
(2) meta-aminotoluene material
Add water 2000L in coupling pot, stirring adds sodium bicarbonate, meta-aminotoluene, stir 40 minutes, then on the rocks be cooled to t=8 DEG C
It is standby；
(3) meta-aminotoluene coupling
The diazo liquid of step (1) is added in meta-aminotoluene mixed liquor, whole process 60 minutes, and per 5 points during charging
Clock monitors a pH value and temperature, finally requires pH=5.5-6, and temperature t=10-20 DEG C, volume v=8300L are acted on 90 minutes
Afterwards, pH=2.7-3.3 is adjusted back with hydrochloric acid, be stirred overnight, final pH=2.7-3.3 volumes=8500L；
Next day, with t=90 DEG C of intensification in 90 minutes, act on 2 hours at 90 DEG C, be warming up to t=50-55 DEG C of foaming, cumulative volume V=
11200L, with liquid caustic soda adjust pH=8, add activated carbon 5-15kg, be warming up to 80 DEG C, stirring 30 minutes after filter, collect mother solution and
Filtrate waits to be condensed；
(4) triphosgene condensation
The mother solution collected is added into solid phosgene, pH=6 adjusts pH=6-6.5 with cold dilute alkali liquid during reaction, after reacting 3 hours
Pyridine, reaction is added to adjust pH=8-8.5 with liquid caustic soda after 2 hours, outlet temperature controls 60-70 DEG C, stirs 1-2 hours, destruction
Responseless phosgene, volume v=12000L；
The amido-G-acid：Hydrochloric acid：Sodium nitrite：Meta-aminotoluene：The mol ratio of phosgene is 1：2.4：1.03：0.98：0.24；
(5) mist projection granulating
The solution that step (4) reaches condensation reaction terminal is directly carried out into mist projection granulating, drying tower setting inlet temperature：180 DEG C,
80 DEG C of outlet temperature；
(6) finished product.
2. direct fast yellow RS dyestuff preparation technologies according to claim 1, it is characterised in that：In step (3), hydrochloric acid is
30wt% hydrochloric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611115826.8A CN106590017A (en) | 2016-12-07 | 2016-12-07 | Technology for preparing direct fast yellow RS dye |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611115826.8A CN106590017A (en) | 2016-12-07 | 2016-12-07 | Technology for preparing direct fast yellow RS dye |
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| Publication Number | Publication Date |
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| CN106590017A true CN106590017A (en) | 2017-04-26 |
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ID=58595180
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611115826.8A Pending CN106590017A (en) | 2016-12-07 | 2016-12-07 | Technology for preparing direct fast yellow RS dye |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113104865A (en) * | 2019-12-12 | 2021-07-13 | 林齐坤 | Method for treating refined mother liquor of vat blue RSN |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1125239A (en) * | 1995-07-11 | 1996-06-26 | 大连理工大学吉化集团公司 | Phosgenation method in course of production of dye and intermediate |
| CN101580643A (en) * | 2009-03-31 | 2009-11-18 | 天津市亚东化工染料厂 | Pollution-free production technology of direct fast black G |
| CN101580644A (en) * | 2009-03-31 | 2009-11-18 | 天津市亚东化工染料厂 | Pollution-free preparation technology of direct fast yellow D-RL |
| CN103788680A (en) * | 2013-12-25 | 2014-05-14 | 连云港锐华化工有限公司 | Preparation method of covering green-light benzimidazolone yellow HGRW for solvent treatment |
-
2016
- 2016-12-07 CN CN201611115826.8A patent/CN106590017A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1125239A (en) * | 1995-07-11 | 1996-06-26 | 大连理工大学吉化集团公司 | Phosgenation method in course of production of dye and intermediate |
| CN101580643A (en) * | 2009-03-31 | 2009-11-18 | 天津市亚东化工染料厂 | Pollution-free production technology of direct fast black G |
| CN101580644A (en) * | 2009-03-31 | 2009-11-18 | 天津市亚东化工染料厂 | Pollution-free preparation technology of direct fast yellow D-RL |
| CN103788680A (en) * | 2013-12-25 | 2014-05-14 | 连云港锐华化工有限公司 | Preparation method of covering green-light benzimidazolone yellow HGRW for solvent treatment |
Non-Patent Citations (1)
| Title |
|---|
| 化工部科技情报研究所主编: "《世界精细化工手册续编》", 31 May 1986, 化学工业部科学技术情报研究所出版 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113104865A (en) * | 2019-12-12 | 2021-07-13 | 林齐坤 | Method for treating refined mother liquor of vat blue RSN |
| CN113104865B (en) * | 2019-12-12 | 2023-08-22 | 酒泉宇鹏化工科技有限公司 | Treatment method of vat blue RSN refining mother liquor |
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Application publication date: 20170426 |
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