CN1286920C - Active red SBE, synthetic method and its composite active red dye - Google Patents

Active red SBE, synthetic method and its composite active red dye Download PDF

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Publication number
CN1286920C
CN1286920C CN 200410014844 CN200410014844A CN1286920C CN 1286920 C CN1286920 C CN 1286920C CN 200410014844 CN200410014844 CN 200410014844 CN 200410014844 A CN200410014844 A CN 200410014844A CN 1286920 C CN1286920 C CN 1286920C
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China
Prior art keywords
dry product
sbe
reaction
coupling
red
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Expired - Fee Related
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CN 200410014844
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CN1569967A (en
Inventor
史锦锋
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Wuxi Runxin Dye Co.,Ltd.
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SHENXIN DYE CHEMICAL CO Ltd JIANGSU
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Abstract

The present invention relates to active red SBE monomer which belongs to the field of dye. Cyanuric chloride and a dispersing agent are pulped into a powder shape under the existence of crushed ice, a dry product, p (beta-sulfuric ester ethyl sulfone)aniline, of which the proportion is from 1 to 1.5 is added in for one-time condensation, a pH value is controlled to be from 2 to 4, a temperature is from 6 to 12 DEG C, a dry product, H acid is added in for secondary condensation after reaction is finished, the temperature is controlled to be from 25 to 35 DEG C, the pH value is controlled to be from 3 to 5, the temperature is dropped to 20 to 30 DEG C after the reaction is finished, and the reaction substance is in the diazonium salt coupling with a dry product, 1, 5-disulfonate-2-naphthylamine; after the coupling is finished, the coupling substance is directly sprayed dryly. The process of the present invention reduces production cost, improves production efficiency, and reaches the production requirements of cleanness; simultaneously, the quality of the product fully approaches to that of red M-3BE., and the force proportion and the dissolvability are better than those of the red M-3BE.

Description

Reactive red SBE and synthetic method thereof
Technical field
The present invention relates to dye field, be meant a kind of reactive red monomer and synthetic this reactive red monomer methods, the composite active red dye that to provide with this reactive red monomer simultaneously be major ingredient.
Technical background
The H acid solution and the cyanuric chloride one of existing red M-3BE employing 10~20% contract, with solution 1,5-disulfonic acid-2-naphthylamines carries out the diazonium salt coupling then, and the sodium-chlor of adding 10~20% is saltoutd, filtering separation, filter cake is pulled an oar into solution, again and content be that 20~30% position ester solutions carry out the secondary condensation, saltout drying and get, this unit cost height that mixes the technology acquisition by synthetic, press filtration, oven dry, pulverizing, assembly, Dry Sack is dark inadequately, and the whole production process complexity, and sewage is many.
Summary of the invention
The invention provides a kind of with position ester synthetic reactive red monomer between the para-ester replacement, by adopting the dry product synthesis technique, reach cleaner production, the product of acquisition has lovely luster, gets color depth, solubleness height, advantages such as substantivity is low, compatibleness good, favorable reproducibility, excellent levelling property, enhancing rate height, degree of fixation height, easily washing property is good, colour fastness is good.The monomeric structural formula of this reactive red SBE is:
Synthetic this reactive red SBE monomer methods is: cyanuric chloride and dispersion agent are pulled an oar in the presence of trash ice to Powdered, the dry product that adds proportioning and be 1-1.05 is to (beta-sulfuric ester ethyl sulfonyl) aniline primary condensation, control pH value 2~4,6~12 ℃ of temperature add the condensation of dry product H acid secondary, 25~35 ℃ of controlled temperature again after reaction is finished, control pH value 3~5, reaction finishes to be cooled to 20~30 ℃ and dry product 1, and 5-disulfonic acid-2-naphthylamines carries out the diazonium salt coupling, and coupling finishes directly spray and does.
Position ester between replacing with para-ester in this synthetic method, other raw materials are constant, and reduce its proportioning, adopt dry product to feed intake simultaneously, and the hydrochloric acid that consume when having reduced used liquid caustic soda of material dissolution and reaction reduce unit cost and reach 40~50% more; Dry product feeds intake, and has also reduced the consumption of water, has improved the solid content of material, has improved spray-dired efficient, has reduced the consumption of heat energy and electric energy.This technology has reduced production cost, has improved production efficiency, reaches to clean production requirement, and quality product near red M-3BE, also is better than red M-3BE comprehensively on power part and solubleness simultaneously.
Composite active red dye, it is a major ingredient with above-mentioned reactive red SBE monomer, weight consists of: reactive red SBE monomer 80~95%, dust-proofing agent 1~5%, solubility promoter 1~15%.
The SBE reactive red is brought up to about 180% through this explained hereafter intensity, and solubleness reaches 180 grams per liters, and light fastness reaches 5 grades, 4 grades of soaping fastnesses, crock fastness 4-5 level, ironing fastness 4-5 level; Simple and the cleaning of synthesis technique, sewage reduces more than 99.5%, feeds intake by dry product; the directly dried yield that increases product of spray of not saltouing, unit must be measured by 100 kilograms and bring up to 170 kilograms, compare with traditional technology; reach the joint consumption and fallen this, improved the purpose of dyestuff quality and environment protection.
Specific implementation method
Embodiment 1,100 parts of cyanuric chlorides and 2 parts of dispersion agents are pulled an oar in the presence of trash ice to Powdered, add 100 parts of dry products (beta-sulfuric ester ethyl sulfonyl) aniline is carried out primary condensation, control pH value 3~4,8~12 ℃ of temperature, when unhindered amina adds the condensation of 100 parts of dry product H acid secondaries less than 1.5% the time again, 25~35 ℃ of controlled temperature, between the control pH value 3~5, reaction finishes to be cooled to 20~26 ℃ and 100 parts of dry products 1 behind the back, 5-disulfonic acid-2-naphthylamines diazonium salt carries out coupling, and coupling finishes directly spray and does.
Embodiment 2,100 parts of cyanuric chlorides and 5 parts of dispersion agents are pulled an oar in the presence of trash ice to Powdered, add 104 parts of dry products (beta-sulfuric ester ethyl sulfonyl) aniline is carried out primary condensation, control pH value 2.5~3.5,6~10 ℃ of temperature, when unhindered amina less than 1.5% the time, add the condensation of 100 parts of dry product H acid secondaries again, 25~35 ℃ of controlled temperature, control pH value 4~5, be cooled to 25~30 ℃ and 100 parts of dry products 1 after reaction finishes, 5-disulfonic acid-2-naphthylamines diazonium salt carries out coupling, and coupling finishes directly spray and does.
Embodiment 3, and composite active red dye is made up of 90 parts of reactive red SBE monomers, 2 parts of dust-proofing agents, 8 parts of Sodium sulfate anhydrous.min(99).
Embodiment 4, and composite active red dye is made up of 95 parts of reactive red SBE monomers, 1 part of dust-proofing agent, 4 parts of Sodium sulfate anhydrous.min(99).
Embodiment 5, and composite active red dye is made up of 85 parts of reactive red SBE monomers, 3 parts of dust-proofing agents, 12 parts of Sodium sulfate anhydrous.min(99).

Claims (2)

1. reactive red SBE monomer is characterized in that structural formula is:
2. the monomeric synthetic method of reactive red SBE, cyanuric chloride and dispersion agent are pulled an oar in the presence of trash ice to Powdered, carry out condensation reaction then, it is characterized in that cyanuric chloride is that the dry product of 1-1.05 carries out primary condensation to (beta-sulfuric ester ethyl sulfonyl) aniline with proportioning earlier, control pH value 2-4, temperature 6-12 ℃, after finishing, reaction adds the condensation of dry product H acid secondary again, controlled temperature 25-35 ℃, control pH value 3-5, reaction finishes to be cooled to 20-30 ℃ and dry product 1, and 5-disulfonic acid-2-naphthylamines carries out the diazonium salt coupling, and coupling finishes directly spray and does.
CN 200410014844 2004-04-30 2004-04-30 Active red SBE, synthetic method and its composite active red dye Expired - Fee Related CN1286920C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 200410014844 CN1286920C (en) 2004-04-30 2004-04-30 Active red SBE, synthetic method and its composite active red dye

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Application Number Priority Date Filing Date Title
CN 200410014844 CN1286920C (en) 2004-04-30 2004-04-30 Active red SBE, synthetic method and its composite active red dye

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CN1569967A CN1569967A (en) 2005-01-26
CN1286920C true CN1286920C (en) 2006-11-29

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Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100424136C (en) * 2006-10-31 2008-10-08 姜堰市东风染料化工厂 Preparation method of active red DF-3BS
CN102031019B (en) * 2010-11-19 2013-05-15 无锡润新染料有限公司 Novel compound activity printing red dye and cleaning production process
CN103497127B (en) * 2013-09-25 2015-01-21 浙江劲光化工有限公司 Synthesis method of para-beta-hydroxyethylsulfonyl sulfate aniline
CN104448921B (en) * 2014-11-28 2016-10-05 浙江劲光实业股份有限公司 A kind of synthetic method of active red dye
CN111100478B (en) * 2019-12-30 2021-03-05 浙江劲光实业股份有限公司 Preparation method and application of blue dye with three active groups

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Effective date of registration: 20081226

Address after: No. 107, Xinfeng Road, Xinjian Town, Jiangsu, Yixing

Patentee after: Wuxi Runxin Dye Co.,Ltd.

Address before: No. 107 middle Xinfeng Road, Xinjian Town, Jiangsu, Yixing

Patentee before: Shenxin Dye Chemical Co., Ltd., Jiangsu

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