CN114907703A - Method for reducing loss of dye in storage process - Google Patents
Method for reducing loss of dye in storage process Download PDFInfo
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- CN114907703A CN114907703A CN202210599420.0A CN202210599420A CN114907703A CN 114907703 A CN114907703 A CN 114907703A CN 202210599420 A CN202210599420 A CN 202210599420A CN 114907703 A CN114907703 A CN 114907703A
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- 238000000034 method Methods 0.000 title claims abstract description 37
- 238000003860 storage Methods 0.000 title claims abstract description 36
- 239000000985 reactive dye Substances 0.000 claims abstract description 73
- 239000000975 dye Substances 0.000 claims abstract description 67
- 239000002002 slurry Substances 0.000 claims abstract description 66
- 239000003381 stabilizer Substances 0.000 claims abstract description 18
- 239000003513 alkali Substances 0.000 claims abstract description 17
- 239000007921 spray Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000004806 packaging method and process Methods 0.000 claims abstract description 7
- INOIOAWTVPHTCJ-UHFFFAOYSA-N 6-acetamido-4-hydroxy-3-[[4-(2-sulfooxyethylsulfonyl)phenyl]diazenyl]naphthalene-2-sulfonic acid Chemical compound CC(=O)NC1=CC=C2C=C(C(N=NC3=CC=C(C=C3)S(=O)(=O)CCOS(O)(=O)=O)=C(O)C2=C1)S(O)(=O)=O INOIOAWTVPHTCJ-UHFFFAOYSA-N 0.000 claims description 13
- 239000006227 byproduct Substances 0.000 claims description 12
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- OMRXVBREYFZQHU-UHFFFAOYSA-N 2,4-dichloro-1,3,5-triazine Chemical compound ClC1=NC=NC(Cl)=N1 OMRXVBREYFZQHU-UHFFFAOYSA-N 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 6
- -1 reactive yellow 160 Chemical compound 0.000 claims description 5
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- 238000006460 hydrolysis reaction Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- 235000017550 sodium carbonate Nutrition 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 239000012752 auxiliary agent Substances 0.000 claims description 2
- 235000015165 citric acid Nutrition 0.000 claims description 2
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 2
- 229910000397 disodium phosphate Inorganic materials 0.000 claims description 2
- 235000019800 disodium phosphate Nutrition 0.000 claims description 2
- HQWKKEIVHQXCPI-UHFFFAOYSA-L disodium;phthalate Chemical compound [Na+].[Na+].[O-]C(=O)C1=CC=CC=C1C([O-])=O HQWKKEIVHQXCPI-UHFFFAOYSA-L 0.000 claims description 2
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 2
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 2
- GCFAQSYBSUQUPL-UHFFFAOYSA-I pentasodium 5-[[4-chloro-6-[3-(2-sulfonatooxyethylsulfonyl)anilino]-1,3,5-triazin-2-yl]amino]-3-[(1,5-disulfonatonaphthalen-2-yl)diazenyl]-4-hydroxynaphthalene-2,7-disulfonate Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].Oc1c(N=Nc2ccc3c(cccc3c2S([O-])(=O)=O)S([O-])(=O)=O)c(cc2cc(cc(Nc3nc(Cl)nc(Nc4cccc(c4)S(=O)(=O)CCOS([O-])(=O)=O)n3)c12)S([O-])(=O)=O)S([O-])(=O)=O GCFAQSYBSUQUPL-UHFFFAOYSA-I 0.000 claims description 2
- YYOYUTRZHZNCFZ-UHFFFAOYSA-I pentasodium 5-[[4-chloro-6-[4-(2-sulfooxyethylsulfonyl)anilino]-1,3,5-triazin-2-yl]amino]-3-[(1,5-disulfonatonaphthalen-2-yl)diazenyl]-4-oxidonaphthalene-2,7-disulfonate Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].Oc1c(N=Nc2ccc3c(cccc3c2S([O-])(=O)=O)S([O-])(=O)=O)c(cc2cc(cc(Nc3nc(Cl)nc(Nc4ccc(cc4)S(=O)(=O)CCOS([O-])(=O)=O)n3)c12)S([O-])(=O)=O)S([O-])(=O)=O YYOYUTRZHZNCFZ-UHFFFAOYSA-I 0.000 claims description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- 239000001509 sodium citrate Substances 0.000 claims description 2
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 2
- 235000011083 sodium citrates Nutrition 0.000 claims description 2
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 2
- 239000001488 sodium phosphate Substances 0.000 claims description 2
- RGGWIBHAZTZHMR-UHFFFAOYSA-J tetrasodium 5-[[4-chloro-6-[4-(2-sulfooxyethylsulfonyl)anilino]-1,3,5-triazin-2-yl]amino]-4-oxido-3-[(2-sulfonatophenyl)diazenyl]naphthalene-2,7-disulfonate Chemical compound C1=CC=C(C(=C1)N=NC2=C(C3=C(C=C(C=C3C=C2S(=O)(=O)[O-])S(=O)(=O)[O-])NC4=NC(=NC(=N4)NC5=CC=C(C=C5)S(=O)(=O)CCOS(=O)(=O)O)Cl)[O-])S(=O)(=O)[O-].[Na+].[Na+].[Na+].[Na+] RGGWIBHAZTZHMR-UHFFFAOYSA-J 0.000 claims description 2
- UIEBGVDTKLYGTN-UHFFFAOYSA-J tetrasodium;7-[[2-(carbamoylamino)-4-[[4-chloro-6-[3-(2-sulfonatooxyethylsulfonyl)anilino]-1,3,5-triazin-2-yl]amino]phenyl]diazenyl]naphthalene-1,3,6-trisulfonate Chemical compound [Na+].[Na+].[Na+].[Na+].C=1C=C(N=NC=2C(=CC3=CC(=CC(=C3C=2)S([O-])(=O)=O)S([O-])(=O)=O)S([O-])(=O)=O)C(NC(=O)N)=CC=1NC(N=1)=NC(Cl)=NC=1NC1=CC=CC(S(=O)(=O)CCOS([O-])(=O)=O)=C1 UIEBGVDTKLYGTN-UHFFFAOYSA-J 0.000 claims description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 2
- 229910000406 trisodium phosphate Inorganic materials 0.000 claims description 2
- 235000019801 trisodium phosphate Nutrition 0.000 claims description 2
- 238000004043 dyeing Methods 0.000 abstract description 13
- 238000005406 washing Methods 0.000 abstract description 9
- 238000004040 coloring Methods 0.000 abstract description 3
- 238000001694 spray drying Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 16
- 238000012795 verification Methods 0.000 description 12
- 239000000047 product Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 150000004982 aromatic amines Chemical class 0.000 description 5
- 239000004744 fabric Substances 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000006482 condensation reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- ORLGPUVJERIKLW-UHFFFAOYSA-N 5-chlorotriazine Chemical group ClC1=CN=NN=C1 ORLGPUVJERIKLW-UHFFFAOYSA-N 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 230000003301 hydrolyzing effect Effects 0.000 description 2
- 239000000543 intermediate Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 150000002790 naphthalenes Chemical class 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012954 diazonium Substances 0.000 description 1
- 150000001989 diazonium salts Chemical class 0.000 description 1
- AFOSIXZFDONLBT-UHFFFAOYSA-N divinyl sulfone Chemical group C=CS(=O)(=O)C=C AFOSIXZFDONLBT-UHFFFAOYSA-N 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
Classifications
-
- 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
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0071—Process features in the making of dyestuff preparations; Dehydrating agents; Dispersing agents; Dustfree compositions
- C09B67/0072—Preparations with anionic dyes or reactive dyes
-
- 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
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0001—Post-treatment of organic pigments or dyes
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Coloring (AREA)
Abstract
The invention discloses a method for reducing loss of a dye in a storage process, and belongs to the technical field of dyes. A method of reducing loss of dye during storage comprising the steps of: step 1: heating the reactive dye which normally reacts to the end point to 15-50 ℃, and measuring the pH value in the reactive dye slurry in real time; step 2: when the pH value of the active dye slurry is less than 5.5, adding a pH stabilizer and alkali into the active dye slurry, measuring the pH value of the active dye slurry to be increased to 5.5-6.5 in real time, stopping adding the stabilizer into the active dye slurry when the pH value of the active dye slurry does not change or is stabilized in a certain interval to float, transferring the active dye slurry into a spray tower storage tank, standardizing, and spray-drying and packaging. The method can reduce the reduction of the hundred fold amount of the reactive dye in the storage process, improve the shelf life of the reactive dye, avoid the reduction of the coloring capability of the reactive dye, avoid the reduction of the dyeing strength and improve the washing fastness of the reactive dye.
Description
Technical Field
The invention relates to the technical field of dyes, in particular to a method for reducing loss of a dye in a storage process.
Background
Reactive dyes, also known as reactive dyes, are a class of dyes that chemically react with fibers during dyeing. The dye molecule contains a group which can react with the fiber chemically, and the dye and the fiber react during dyeing to form a covalent bond between the dye and the fiber into a whole, so that the fastness to washing and rubbing is improved.
The reactive dye is relatively stable under neutral and weakly acidic conditions, the reactive dye product contains 5-8% of water in the storage process, by-products generated in the synthesis of the reactive dye or some incompletely-reacted intermediates or raw materials carried into the product are far easier to hydrolyze than the reactive dye, and after the by-products, the intermediates or the raw materials are hydrolyzed, the pH value of the reactive dye product is reduced, the hydrolysis of the main reactive dye is accelerated, so that the structure of the main reactive dye in the reactive dye product is damaged, the dyeing rate of the reactive dye is low, the dyeing intensity is reduced, and in all the reactive dyes, the M-type reactive dye is most unstable and has short shelf life!
Synthesis of M-type reactive dye containing monochlorotriazine reactive group: usually, the compound is obtained by condensing aromatic amine containing vinylsulfonyl and trichloro-s-triazine, reacting with aromatic amine (or chromophore containing amino) to block a second active chlorine, and then reacting with diazonium salt. In the industrial production process, the aromatic amine containing the vinyl sulfone group and the trichloro-s-triazine are directly subjected to a second-step condensation reaction without separation and purification after reaction, and the nucleophilicity of a plurality of aromatic amines adopted in the second-step condensation reaction is not high, so that the aromatic amines cannot completely react with the first-step condensation reaction, and the target product often contains a small amount of by-products with a dichloro-s-triazine structure. The by-products can be continuously and slowly hydrolyzed in the storage of the liquid dye to reduce the pH value of the system, and become main factors influencing the stability of the monochlorotriazine type salt-free liquid reactive dye.
During the storage process of the M-type reactive dye, the hundred-fold reduction rate during one year is generally 2% -4%, if ten thousand tons of dye are stored every year, the reactive dye loses 200-400 tons before being sprayed and dried, the loss amount of the reactive dye during the storage process is not small, and the longer the storage time is, the more hydrolysis loss is generated.
In order to solve the problem of loss of reactive dye in the storage process of the reactive dye, the reactive dye is purified before preparing reactive dye slurry, and by-products of a dichloro-s-triazine structure in the reactive dye are reduced, so that the storage time of the reactive dye slurry is prolonged, and the loss of the reactive dye in the storage process of the reactive dye slurry is reduced.
Therefore, how to reduce the reduction of the hundred fold amount of the reactive dye in the storage process, improve the shelf life of the reactive dye, and avoid the reduction of the coloring capability and the dyeing strength of the reactive dye is a problem to be solved urgently.
Disclosure of Invention
1. Technical problem to be solved
Aiming at the problems in the prior art, the invention aims to provide a method for reducing the loss of the dye in the storage process, which can reduce the reduction of the folding amount of the reactive dye in the storage process, improve the shelf life of the reactive dye and avoid the problems of reduced coloring capability and reduced dyeing strength of the reactive dye due to the reduction of the folding amount.
2. Technical scheme
In order to solve the above problems, the present invention adopts the following technical solutions.
A method of reducing dye loss during storage comprising the steps of: step 1: heating the reactive dye which normally reacts to the end point to 15-50 ℃, and measuring the pH value in the reactive dye slurry in real time; step 2: when the pH value of the active dye slurry is less than 5.5, adding a pH stabilizer and alkali into the active dye slurry, measuring in real time that the pH value of the active dye slurry is increased to 5.5-6.5, stopping adding the stabilizer and the alkali into the active dye slurry when the pH value of the active dye slurry does not change or is stabilized in a certain interval and floats, transferring the active dye slurry into a spray tower storage tank, standardizing, and then spraying, drying and packaging.
Preferably, step 1: the reactive dye which normally reacts to the end point is heated to 20-50 ℃.
Further, the stabilizer is selected from one or more of trisodium phosphate, sodium hydrogen phosphate, sodium dihydrogen phosphate, citric acid, sodium citrate and sodium phthalate.
Further, the molar ratio of the stabilizer to the reactive dye is as follows: 0.005-0.03:1.
Further, the reactive dye is M type reactive dye.
Further, the structural formula of the reactive dye is shown in the specification
Wherein Ar is benzene series, naphthalene series and derivatives or chromophore thereof.
Further, the structural formula of the reactive dye is shown in the specification
Wherein Ar is benzene series, naphthalene series and derivatives or chromophore thereof, and X is-SO 3 M、—NHCH 3 、—OCH 3， M is H, Li, Na or K.
The chromophore is the chromophoric part of the dye, also called color developing agent, and is mostly amino azo compound containing water-soluble group and metal complex compound.
Further, the reactive dye is one or more of reactive yellow 145, reactive yellow 160, reactive orange 122, reactive red 194, reactive red 195, reactive red 240, reactive red 241, reactive blue 194 or reactive blue 222.
Further, in step 1, a dichloros-triazine by-product exists in the M-type active dye slurry, and the hydrolysis reaction equation of the dichloros-triazine by-product is as follows:
wherein R and R 2 Are each independently selected from-CH 3 、-OCH 3 、-SO 3 One of H and-H groups.
Further, in the step 2, after the pH value of the active dye slurry is stable, and before the active dye slurry is dried by spraying, a dye auxiliary agent is added for standardization.
Further, in step 2, the stabilizer and the alkali are added in sequence, namely, the stabilizer is added firstly, the pH of the solution is still lower than 5.5, and the alkali is added to adjust the pH of the active dye slurry.
Further, the alkali includes, but is not limited to, three of baking soda, soda ash and liquid alkali.
3. Advantageous effects
Compared with the prior art, the invention has the advantages that:
(1) according to the invention, the prepared reactive dye slurry is treated, so that byproducts in the reactive dye slurry are completely hydrolyzed, the reactive dye slurry is stored after being sprayed and dried in a standardized manner, the storage shelf life of the reactive dye is prolonged, the storage lasts for one year or more, and the color light and the intensity of the reactive dye product are basically unchanged.
(2) The method improves the washing color fastness of the obtained reactive dye product to a certain extent by treating the active dye slurry which is just prepared.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1: taking activated yellow 145 as an example:
the structural formula of activated yellow 145 is shown below:
step 1: firstly, measuring the pH value of the active yellow 145 slurry which normally reacts to the end point and the dye strength of the active yellow 145, then heating the active yellow 145 slurry to 15-50 ℃, measuring the pH value of the active dye slurry in real time, hydrolyzing the by-product for 2-4h, and gradually reducing the pH value of the active yellow 145 slurry;
step 2: when the pH value of the active yellow 145 slurry is less than 5.5, measuring the dye strength of the dye, firstly adding a pH stabilizer into the active dye slurry, then adding alkali, measuring the pH value of the active dye slurry in real time, stopping adding the stabilizer and the alkali into the active dye slurry when the pH value of the active dye slurry is raised to 5.5-6.5 and the pH value of the active dye slurry does not change or is stabilized in a certain interval to float, then transferring the active yellow 145 slurry into a storage tank of a spray tower, standardizing, and then spraying and drying for packaging.
Comparative example 1: taking activated yellow 145 as an example:
taking the activated yellow 145 slurry which normally reacts to the end point and is the same as the activated yellow 145 slurry in the example 1, transferring 100ml of the activated yellow 145 slurry into a storage tank of a spray tower, standardizing, and then spraying, drying and packaging.
Verification example 1: respectively taking the active yellow 145 stored for 10 months in example 1 and comparative example 1, dissolving in water to prepare standard solutions, respectively putting into cotton cloth for fully dyeing, carrying out bath ratio of 1:10, running for 10min, adding 60g/L sodium sulfate, and running for 10 min; heating to 60 ℃ at the speed of 1 ℃/min, running for 10min, adding 15g/L sodium carbonate, running for 45min, and then carrying out the treatment of water washing, soaping, water washing and drying to obtain dyed cloth.
| Dye material | Dyeing effect | Color fastness to washing | Dyeing mechanical properties |
| Example 1 | 4-5 stages | 4-5 stages | 4-5 stages |
| Comparative example 1 | Grade 3-4 | 2-3 stages | Grade 3-4 |
| Freshly prepared reactive dye solution | 4-5 stages | Grade 4 | 4-5 stages |
Example 2: taking reactive orange 122 as an example:
the structural formula of reactive orange 122 is shown below:
step 1: firstly, measuring the pH value of the reactive orange 122 slurry which normally reacts to the end point and the dye strength of the reactive orange 122, then heating the reactive orange 122 slurry to 20-50 ℃, measuring the pH value of the reactive dye slurry in real time, hydrolyzing the by-product for 2-4h, and gradually reducing the pH value of the reactive orange 122 slurry;
step 2: when the pH value of the reactive orange 122 slurry is less than 5.5, determining the dye strength of the dye, adding a pH stabilizer into the reactive dye slurry, then adding alkali, determining the pH value of the reactive dye slurry in real time, stopping adding the stabilizer and the alkali into the reactive dye slurry when the pH value of the reactive dye slurry is raised to 5.5-6.5 and the pH value of the reactive dye slurry is unchanged or stabilized to float in a certain interval, transferring the reactive orange 122 slurry into a spray tower storage tank, standardizing, and then spraying and drying for packaging.
Comparative example 2: taking reactive orange 122 as an example:
the same slurry of reactive orange 122, which normally reacts to the end point as in example 2, is taken, and the slurry of reactive orange 122 is transferred to a spray tower storage tank, standardized, and spray dried for packaging.
Verification example 2: dissolving the active orange 122 stored for 20 months in example 2 and comparative example 2 respectively in water to prepare standard solutions, respectively putting into cotton cloth for fully dyeing, wherein the bath ratio is 1:10, running for 10min, adding 60g/L sodium sulfate, and running for 10 min; heating to 60 ℃ at the speed of 1 ℃/min, running for 10min, adding 15g/L sodium carbonate, running for 45min, and then carrying out the treatment of water washing, soaping, water washing and drying to obtain dyed cloth.
| Dye material | Dyeing effect | Color fastness to washing | Dyeing mechanical properties |
| Example 2 | Grade 5 | Grade 5 | Grade 5 |
| Comparative example 2 | 4 stage | Grade 3 | Grade 3 |
| Freshly prepared reactive dye solution | Grade 5 | Grade 4 | Grade 5 |
The procedure of example 3, comparative example 3 and verification example 3 was the same as that of example 1 and comparative example 1 and verification example 1, and the data on example 3, comparative example 3 and verification example 3 are shown in table 3:
table 3:
the procedure of example 4, comparative example 4 and verification example 4 was the same as that of example 1 and comparative example 1 and verification example 1, and the data on example 4, comparative example 4 and verification example 4 are shown in table 4:
table 4:
the procedure of example 5, comparative example 5 and verification example 5 was the same as that of example 1, comparative example 1 and verification example 1, and the relevant data of example 5, comparative example 5 and verification example 5 are shown in table 5:
table 5:
through the implementation of 1-5, the comparative examples 1-5 and the verification examples 1-5, it can be seen that the reactive dye is easier to store after the prepared reactive dye slurry is treated by the method of the invention, the performance of the stored reactive dye is consistent with that of the prepared reactive dye slurry, and the reactive dye is easy to lose and is difficult to store after the prepared reactive dye slurry which is not treated by the method of the invention is directly and standardizedly sprayed and dried.
Claims (9)
1. A method of reducing dye loss during storage, comprising: the method comprises the following steps:
step 1: heating the reactive dye which normally reacts to the end point to 15-50 ℃, and measuring the pH value in the reactive dye slurry in real time;
step 2: when the pH value of the active dye slurry is less than 5.5, adding a pH stabilizer and alkali into the active dye slurry, measuring in real time that the pH value of the active dye slurry is increased to 5.5-6.5, stopping adding the stabilizer and the alkali into the active dye slurry when the pH value of the active dye slurry does not change or is stabilized in a certain interval and floats, transferring the active dye slurry into a spray tower storage tank, standardizing, and then spraying, drying and packaging.
2. A method of reducing dye loss during storage according to claim 1, wherein: the stabilizer is one or more selected from trisodium phosphate, sodium hydrogen phosphate, sodium dihydrogen phosphate, citric acid, sodium citrate and sodium phthalate.
3. A method of reducing dye loss during storage according to claim 1, wherein: the mol ratio of the stabilizer to the reactive dye is as follows: 0.005-0.03:1.
4. A method of reducing dye loss during storage according to claim 1, wherein: the reactive dye is M type reactive dye.
5. A method of reducing dye loss during storage according to claim 1, wherein: the reactive dye is one or more of reactive yellow 145, reactive yellow 160, reactive orange 122, reactive red 194, reactive red 195, reactive red 240, reactive red 241, reactive blue 194 or reactive blue 222.
6. A method of reducing dye loss during storage according to claim 1, wherein: in the step 1, a dichloros-triazine byproduct exists in M-type active dye slurry, and the hydrolysis reaction equation of the dichloros-triazine byproduct is as follows:
wherein R and R 2 Are each independently selected from-CH 3 、-OCH 3 、-SO 3 One of H and-H groups.
7. A method of reducing dye loss during storage according to claim 1, wherein: and 2, after the pH of the active dye slurry is stable and before the active dye slurry is sprayed to be dry, adding a dye auxiliary agent for standardization.
8. A method of reducing dye loss during storage according to claim 1, wherein: in the step 2, the stabilizer and the alkali are added in sequence, namely the stabilizer is added firstly, the pH of the solution is still lower than 5.5, and the alkali is added to adjust the pH of the active dye slurry.
9. A method of reducing dye loss during storage according to claim 6 or 8, wherein: the alkali includes but is not limited to three of baking soda, soda ash and liquid alkali.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210599420.0A CN114907703B (en) | 2022-05-30 | 2022-05-30 | Method for reducing loss of dye in storage process |
Applications Claiming Priority (1)
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| PT74159A (en) * | 1980-12-22 | 1982-01-01 | Sumitomo Chemical Co | Aqueous liquid dye composition |
| JPS6218474A (en) * | 1985-07-16 | 1987-01-27 | Sumitomo Chem Co Ltd | Aqueous liquid reactive dye composition |
| US5772699A (en) * | 1995-03-13 | 1998-06-30 | Crompton & Knowles Corporation | Stable aqueous reactive dye composition and method for stabilizing an aqueous reactive dye composition |
| CN1594447A (en) * | 2004-06-21 | 2005-03-16 | 东华大学 | Hydrolysis retardant for liquid active dye and method for making same |
| CN102352126A (en) * | 2011-08-25 | 2012-02-15 | 郑州大学 | Active red dye for digital ink-jet printing and preparation method thereof |
| CN111234561A (en) * | 2020-03-13 | 2020-06-05 | 浙江大学滨海产业技术研究院 | Preparation of storage-stable active liquid dye |
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Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| PT74159A (en) * | 1980-12-22 | 1982-01-01 | Sumitomo Chemical Co | Aqueous liquid dye composition |
| US4439205A (en) * | 1980-12-22 | 1984-03-27 | Sumitomo Chemical Company, Limited | Aqueous liquid dye composition: storage stable reactive dye with reduction inhibitor |
| JPS6218474A (en) * | 1985-07-16 | 1987-01-27 | Sumitomo Chem Co Ltd | Aqueous liquid reactive dye composition |
| US5772699A (en) * | 1995-03-13 | 1998-06-30 | Crompton & Knowles Corporation | Stable aqueous reactive dye composition and method for stabilizing an aqueous reactive dye composition |
| CN1594447A (en) * | 2004-06-21 | 2005-03-16 | 东华大学 | Hydrolysis retardant for liquid active dye and method for making same |
| CN102352126A (en) * | 2011-08-25 | 2012-02-15 | 郑州大学 | Active red dye for digital ink-jet printing and preparation method thereof |
| CN111234561A (en) * | 2020-03-13 | 2020-06-05 | 浙江大学滨海产业技术研究院 | Preparation of storage-stable active liquid dye |
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