- ECO-FRIENDLY METHOD FOR PREPARING HIGHLY PURE 2-CHLORO-4-AMINOTOLUENE-5-SULFONIC ACID
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The present invention relates to an eco-friendly method for preparing highly pure 2-chloro-4-aminotoluene-5-sulfonic acid, which includes efficient reaction processes to provide highly pure 2-chloro-4-aminotoluene-5-sulfonic acid without a purification process, and minimizes generation of contaminants by reusing a waste solvent after distillation. The method comprises the steps of: 1) adding 2-chloro-4-aminotoluene, a solvent and sulfuric acid to a reactor; 2) carrying out sulfonation of the reaction materials added to the reactor; 3) filtering and washing the compound produced from the step 2) with a solvent to provide wet cake; 4) vacuum drying the wet cake obtained from the step 3) to provide 2-chloro-4-aminotoluene-5-sulfonic acid; and 5) carrying out distillation of the waste solvent generated from the steps 3) and 4).(AA) Start(BB) End(S10) Add 2-chloro-4-aminotoluene, solvent and sulfuric acid to a reactor(S20) Carry out sulfonation on additive added to the reactor(S30) Filter and wash compound subjected to sulfonation with solvent to obtain wet cake(S40) Vacuum dry wet cake to obtain 2-chloro-4-aminotoluene-5-sulfonic acid(S50) Carry out distillation of waste solvent generated during filtering, washing and vacuum dryingCOPYRIGHT KIPO 2016
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Paragraph 0151-0159
(2017/06/02)
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- ECO-FRIENDLY METHOD FOR PREPARING HIGHLY PURE 2-CHLORO-4-AMINOTOLUENE-5-SULFONIC ACID
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The present invention relates to a manufacturing method of high-purity 2-chloro-4-aminotoluene-5-sulfonic acid of eco-friendly process, more specifically, the present invention may provide a high-purity 2-chloro-4-aminotoluene-5-sulfonic acid without having a purification process by having an efficient reaction process, and minimize a generation of pollutant by reusing a waste solvent through distillation. The present invention comprises the following steps: a first step of adding 2-chloro-4-aminotoluene, solvent, and sulfuric acid to a reactor; a second step of performing a sulfonating reaction to an additive added in the reactor; a third step of manufacturing a wet cake by filtering and cleaning a compound generated in the second step with the solvent; a fourth step of manufacturing the 2-chloro-4-aminotoluene-5-sulfonic acid by vacuum drying the wet cake manufactured in the third step; a fifth step of distilling the waste solvent generated from the third and fourth step.(AA) Start(BB) End(S10) Adding 2-chloro-4-aminotoluene, solvent, and sulfuric acid to a reactor(S20) Performing a sulfonating reaction to an additive added in the reactor(S30) Manufacturing a wet cake by filtering and cleaning a compound generated in the second step with the solvent(S40) Manufacturing the 2-chloro-4-aminotoluene-5-sulfonic acid by vacuum drying the wet cake(S50) Distilling the waste solvent generated during filtering, cleaning, and vacuum drying processCOPYRIGHT KIPO 2015
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Paragraph 0161-0165
(2016/10/20)
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- The influence of different solvents on 2-ammonio-4-chloro-5- methylbenzenesulfonate, including its De- and resulfonation
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The title compound (2-ammonio-4-chloro-5-methylbenzenesulfonate), C 7H8ClNO3S, 1, is an intermediate in the synthesis of laked red and yellow azo pigments. Heating 1 in 2-picoline, quinoline and N,N′-dimethylacetamide (DMAc) [or N-methyl-2-pyrrolidone (NMP)] resulted in the formation of three different compounds: a 2-picolinium hydrate (2), a quinolinium quinoline solvate (3), and a sulfate of the desulfonated title compound (4). The three new compounds were structurally characterised using single-crystal diffraction data and chemically using thermal analysis (DTA/TGA), elemental analysis and spectroscopic methods (IR and NMR). By heating 2, 3 and 4 in the solid state, compound 1 is obtained again. In the case of 4, this corresponds to a desulfonation-resulfonation reaction in subsequent steps, which is rarely observed as such. Graphical Abstract: The title compound 2-ammonio-4-chloro-5-methylbenzenesulfonate was heated in 2-picoline, quinoline and N,N′-dimethylacetamide (DMAc) resulting in the formation of three different compounds: a 2-picolinium hydrate (2), a quinolinium quinoline solvate (3), and a sulfate of the desulfonated title compound (4 see Figure). Heating 2, 3 and 4 in the solid state, compound 1 is obtained again. In the case of 4, this corresponds to a desulfonation- resulfonation reaction in subsequent steps, which is rarely observed as such.[Figure not available: see fulltext.]
- Bekoe, Sandor L.,Bats, Jan W.,Alig, Edith,Schmidt, Martin U.
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p. 655 - 663
(2014/01/06)
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- Mixed coupled azo pigments
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(1) A mixed coupled azo pigment prepared from: (A) 30% to 70% of two or more diazonium components, at least one derived from a monoaryl amine and (B) an organic coupled component, said pigment containing one or more COOH or .?.SO H.!. .Iadd.SO3 H .Iaddend.groups or esters, amides, alkali metal or alkali earth metal salts thereof or (2) A mixed coupled azo pigment prepared from: (A) 5% to 95% of two or more bis, tris or tetrakis diazonium components, at least one derived from a monoaryl amine and meeting certain specific critria and (B) an organic coupling component, said pigment comprising the same acid or salt groups of pigment (1).
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- Mixed coupled azo pigments
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(1) A mixed coupled azo pigment prepared from: (A) 30% to 70% of two or more diazonium components, at least one derived from a monoaryl amine and (B) an organic coupling component, said pigment containing one or more COOH or SO H groups or esters, amides, alkali metal or alkali earth metal salts thereof or (2) A mixed coupled azo pigment prepared from: (A) 5% to 95% of two or more bis, tris or tetrakis diazonium components, at least one derived from a monoaryl amine and meeting certain specific critria and (B) an organic coupling component, said pigment comprising the same acid or salt groups of pigment (1).
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- Azo pigment compositions and process for their preparation
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This invention is that of an azo pigment composition containing about 1 to 10 percent by weight of a nonionic alkyl polyglycoside dispersing agent. The polyglycosides useful in the invention have the general formulae: wherein: M is an oxygen, sulfur, nitrogen phosphorous or silicon atom; n is an integer from 8 to 18, preferably 8 to 11 and X represents the number average degree of polymerization having a numerical value from about 1 to about 2. These azo pigment compositions are prepared by conducting the azo pigment coupling reaction in the presence of said alkyl polyglycoside. The resulting pigment exhibit superior application properties in water based ink systems.
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- Bisazo brown reactive dye
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A brown reactive dye represented by a free acid of the formula, STR1 wherein R is a hydrogen atom or a C1 to C4 alkyl group, X is --SO2 CH2 CH2 Cl, --SO2 CH=CH2, --SO2 CH2 CH2 OSO3 H or --SO2 CH2 CH2 OPO3 H2, rings A, B and C are each a benzene or naphthalene ring which may have other substituent, m is 0 to 3 and n is 0 to 1. This dye is suitable for dyeing cellulose fibers brown to afford dyeings superior in fastnesses, acid stability, build-up property and level dyeing property.
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- Process for the preparation of aminoarylsulphonic acids in sulfolene solvent
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Aromatic aminosulphonic acids which have a reduced content of discoloring by-products are obtained when aromatic amines are reacted with a sulphonating agent in a reaction medium at least some of which consists of tetramethylene sulphone.
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- Azo dyestuffs
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Azo dyestuffs, which in the acid form, are represented by the formula: wherein A is an aromatic radical, M is a 1,4-benzene radical which may be substituted, E is the residue of a coupling component which is free from azo groups, At least one of A and M containing a phosphonic acid group, and the metal complexes of those having a metallisable group are reactive dyes suitable for use in the process of German OLS No. 2324809.
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