CN105504227B - A kind of synthetic method of environmental protection chlorine-resistant color fixing agent - Google Patents
A kind of synthetic method of environmental protection chlorine-resistant color fixing agent Download PDFInfo
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- CN105504227B CN105504227B CN201610002041.3A CN201610002041A CN105504227B CN 105504227 B CN105504227 B CN 105504227B CN 201610002041 A CN201610002041 A CN 201610002041A CN 105504227 B CN105504227 B CN 105504227B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/02—Polycondensates containing more than one epoxy group per molecule
- C08G59/10—Polycondensates containing more than one epoxy group per molecule of polyamines with epihalohydrins or precursors thereof
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
- D06P5/02—After-treatment
- D06P5/04—After-treatment with organic compounds
- D06P5/08—After-treatment with organic compounds macromolecular
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P5/00—Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
- D06P5/22—Effecting variation of dye affinity on textile material by chemical means that react with the fibre
- D06P5/225—Aminalization of cellulose; introducing aminogroups into cellulose
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Abstract
The invention discloses a kind of synthetic methods of novel environment friendly chlorine-resistant color fixing agent, and with epoxychloropropane, diethylenetriamine, diallylamine is raw material, reacted obtained novel environment friendly chlorine-resistant color fixing agent.Color fixing agent of the invention has hydroxyl and imino group, not only can be in conjunction with dyestuff, but also can close the chloride ion on dyestuff, moreover it is possible to form thin polymer film in fiber surface.
Description
Technical field
The present invention relates to the color fixing agent of textile fabric, more particularly it relates to a kind of novel environment friendly chlorine-resistant color fixing agent
Synthetic method.
Background technique
The dyeing of the cellulose base fiber fabrics such as cotton can be such that dyed fabric obtains fresh usually using direct dyes and acid dyes
Gorgeous color, but its color processing fastness is poor, i.e., and the direct dyes and acid dyes on dyed fabric surface are easy in washing process
In falling off, dyed fabric colour fading is not only resulted in, but also can be infected with other fabrics, bring fiber crops to the consumption and arrangement of textile
It is tired.In addition, the sweat of human body and saliva and oxygen in environment and ultraviolet light can all make in the use process of dyed fabric
Covalent bond between reactive dye and cellulose fibre occurs fracture and fastness variation phenomenon occurs, leads to fabric fading.To mention
High dyestuff resists erosion of the environmental factor to dyestuff in the stability of fiber surface, usually carries out fixation to fabric after dyeing
It handles, auxiliary agent used in this processing is color fixing agent.
It comes out so far from early 1950s first generation polymer electrolyte color fixing agent, various countries develop variety classes not in succession
Isostructural color fixing agent.In cotton color fixing agent, according to Oeko-Tex standard, the index of textile color stability include it is resistance to soap,
Water-fastness, rub resistance, perspiration resistance, sun-resistant and chlorine-resistant, environmental protection are free of formaldehyde, promote sensitive color fastness, influence on coloured light small etc.
Index request, wherein chlorine-resistant, significantly improves the dyefastness of sensitive colors while reaching this formaldehydeless index study of environmental protection
It is in progress slower.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of synthetic method of novel environment friendly chlorine-resistant color fixing agent, this method is closed
At color fixing agent there is environmental protection, chlorine-resistant and the performance for improving sensitive color fastness, and be able to satisfy the primary demand of conventional color fixing agent.
To solve the above-mentioned problems, the present invention provides a kind of synthetic methods of novel environment friendly chlorine-resistant color fixing agent.
In order to achieve the above-mentioned object of the invention, this invention takes following technical schemes:
A kind of synthetic method of novel environment friendly chlorine-resistant color fixing agent, includes the following steps:
(1) epoxychloropropane of 50-80g, the diethylenetriamine of 80-110g, the addition of 80-110g diallylamine are equipped with
It is mixed in the round-bottomed flask of water segregator and condenser pipe and is heated to 45-55 DEG C, and water is not further added by water segregator；
(2) temperature is heated to 55-70 DEG C, 3.3-3.85g oxidizing agent solution and 3.3-3.85g is added into reaction system
Reducing agent solution, by 29.7-34.65g oxidizing agent solution and 29.7-34.65g reducing agent solution at 70-95 DEG C after 25-40min
Lower dropwise addition 2.5-3.5h, reaction terminate；
(3) after reaction, reaction product is bleached to get color fixing agent with hydrogenperoxide steam generator.
In one embodiment, the epoxychloropropane is 55-70g, diethylenetriamine 85-100g, diallyl
Amine is 85-100g.
In one embodiment, the oxidizing agent solution is ammonium persulfate solution.
In one embodiment, in the oxidizing agent solution, the quality of ammonium persulfate accounts for oxidizing agent solution gross mass
8.8-10.5%。
In one embodiment, in the oxidizing agent solution, the quality of ammonium persulfate accounts for oxidizing agent solution gross mass
9.09%。
In one embodiment, the reducing agent solution is sodium metabisulfite solution.
In one embodiment, in the reducing agent solution, the quality of sodium pyrosulfite accounts for reducing agent solution gross mass
8.8-10.5%.
In one embodiment, in the reducing agent solution, the quality of sodium pyrosulfite accounts for reducing agent solution gross mass
9.09%.
In one embodiment, in the hydrogenperoxide steam generator, the quality of hydrogen peroxide accounts for the total matter of hydrogenperoxide steam generator
The 30% of amount.
In one embodiment, the hydrogenperoxide steam generator dosage is 10g.
Compared with prior art, the invention has the following beneficial effects:
1. color fixing agent of the invention is cationic compound, color lake can be generated with the anionic reactive in dyestuff, be deposited on
Fiber surface.
2. the cross-linking reaction group of color fixing agent of the invention can not only be reacted with certain groups in dye molecule, but also
Energy and fibrin reaction can effectively improve the soaping fastness of dyestuff by forming polynary interconnected system.In addition, in product
Imino group enclose chloride ion on dyestuff, greatly improve the chlorine resistance of product dyed thereby.
3. after fixation bakes processing, various group crosslinking condensations in resin form solid netted in fiber surface
Thin polymer film, can effectively organizational environment influence, promote the properties of product dyed thereby.
The above-mentioned of the application and other features, aspects and advantages are more readily understood with reference to following detailed description.
Specific embodiment
Unless otherwise defined, all technologies used herein and scientific term have and the common skill of fields of the present invention
The normally understood identical meaning of art personnel.When there is a conflict, the definition in this specification shall prevail.
As used herein term " by ... preparation " it is synonymous with "comprising".Term "comprising" used herein, " comprising ",
" having ", " containing " or its any other deformation, it is intended that cover non-exclusionism includes.For example, the combination comprising listed elements
Object, step, method, product or device are not necessarily limited to those elements, but may include not expressly listed other elements or
Such composition, step, method, product or the intrinsic element of device.
Conjunction " Consists of " excludes any element that do not point out, step or component.If in claim, this
Phrase will make claim closed, so that it is not included the material in addition to the material of those descriptions, but relative normal
Except rule impurity.When being rather than immediately following after theme in the clause that phrase " Consists of " appears in claim main body,
It is only limited to element described in the clause；Other elements are not excluded except the claim as a whole.
Equivalent, concentration or other values or parameter are excellent with range, preferred scope or a series of upper limit preferred values and lower limit
When the Range Representation that choosing value limits, this should be understood as specifically disclosing by any range limit or preferred value and any range
Any pairing of lower limit or preferred value is formed by all ranges, regardless of whether the range separately discloses.For example, when open
When range " 1 to 5 ", described range should be interpreted as including range " 1 to 4 ", " 1 to 3 ", " 1-2 ", " 1-2 and 4-5 ",
" 1-3 and 5 " etc..When numberical range is described herein, unless otherwise stated, otherwise the range be intended to include its end value and
All integers and score in the range.
In addition, indefinite article "an" before element of the present invention or component and "one" quantitative requirement to element or component
(i.e. frequency of occurrence) unrestriction.Therefore "one" or "an" should be read as including one or at least one, and odd number
The element or component of form also include plural form, unless the obvious purport of the quantity refers to singular.
The present invention is specifically described below by embodiment.It is necessarily pointed out that following embodiment is only used
In the invention will be further described, it should not be understood as limiting the scope of the invention, professional and technical personnel in the field
The some nonessential modifications and adaptations made according to the content of foregoing invention, still fall within protection scope of the present invention.
In addition, if illustrated without other, it is raw materials used to be all commercially available.
In the examples below, in the oxidizing agent solution, the quality of ammonium persulfate accounts for oxidizing agent solution gross mass
9.09%；In the reducing agent solution, the quality of sodium pyrosulfite accounts for the 9.09% of reducing agent solution gross mass.
Embodiment 1
The synthetic method of novel environment friendly chlorine-resistant color fixing agent, includes the following steps:
(1) epoxychloropropane of 50g, the diethylenetriamine of 80g, 80g diallylamine are added equipped with water segregator and cold
It is mixed in the round-bottomed flask of solidifying pipe and is heated to 50 DEG C, and water is not further added by water segregator；
(2) 3g oxidant is weighed, is that 1:10 dissolved oxidant is molten to get oxidant according to the mass ratio of oxidant and water
Liquid；3g reducing agent is weighed, is the agent of 1:10 dissolving and reducing to get reducing agent solution according to the mass ratio of reducing agent and water；
(3) temperature is heated to 60 DEG C, the reducing agent solution of 3.3g oxidizing agent solution and 3.3g is added into reaction system,
3h is added dropwise at 70 DEG C in the reducing agent solution of the oxidizing agent solution of 29.7g and 29.7g after 0.5h, reaction terminates；
(4) after reaction, the hydrogenperoxide steam generator for being cooled to the 30wt% of 50 DEG C of addition 10g floats reaction product
It is white, it is cooled to room temperature finally to get color fixing agent.
Embodiment 2
The synthetic method of novel environment friendly chlorine-resistant color fixing agent, includes the following steps:
(1) epoxychloropropane of 60g, the diethylenetriamine of 100g, 100g diallylamine be added equipped with water segregator and
It is mixed in the round-bottomed flask of condenser pipe and is heated to 50 DEG C, and water is not further added by water segregator；
(2) 3g oxidant is weighed, is that 1:10 dissolved oxidant is molten to get oxidant according to the mass ratio of oxidant and water
Liquid；3g reducing agent is weighed, is the agent of 1:10 dissolving and reducing to get reducing agent solution according to the mass ratio of reducing agent and water；
(3) temperature is heated to 60 DEG C, the reducing agent solution of 3.3g oxidizing agent solution and 3.3g is added into reaction system,
3h is added dropwise at 70 DEG C in the reducing agent solution of the oxidizing agent solution of 29.7g and 29.7g after 0.5h, reaction terminates；
(4) after reaction, the hydrogenperoxide steam generator for being cooled to the 30wt% of 50 DEG C of addition 10g floats reaction product
It is white, it is cooled to room temperature finally to get color fixing agent.
Embodiment 3
The synthetic method of novel environment friendly chlorine-resistant color fixing agent, includes the following steps:
(1) epoxychloropropane of 60g, the diethylenetriamine of 100g, 100g diallylamine be added equipped with water segregator and
It is mixed in the round-bottomed flask of condenser pipe and is heated to 50 DEG C, and water is not further added by water segregator；
(2) 3g oxidant is weighed, is that 1:10 dissolved oxidant is molten to get oxidant according to the mass ratio of oxidant and water
Liquid；3g reducing agent is weighed, is the agent of 1:10 dissolving and reducing to get reducing agent solution according to the mass ratio of reducing agent and water；
(3) temperature is heated to 60 DEG C, the reducing agent solution of 3.3g oxidizing agent solution and 3.3g is added into reaction system,
3h is added dropwise at 75 DEG C in the reducing agent solution of the oxidizing agent solution of 29.7g and 29.7g after 0.5h, reaction terminates；
(4) after reaction, the hydrogenperoxide steam generator for being cooled to the 30wt% of 50 DEG C of addition 10g floats reaction product
It is white, it is cooled to room temperature finally to get color fixing agent.
Embodiment 4
The synthetic method of novel environment friendly chlorine-resistant color fixing agent, includes the following steps:
(1) epoxychloropropane of 60g, the diethylenetriamine of 100g, 100g diallylamine be added equipped with water segregator and
It is mixed in the round-bottomed flask of condenser pipe and is heated to 50 DEG C, and water is not further added by water segregator；
(2) 3g oxidant is weighed, is that 1:10 dissolved oxidant is molten to get oxidant according to the mass ratio of oxidant and water
Liquid；3g reducing agent is weighed, is the agent of 1:10 dissolving and reducing to get reducing agent solution according to the mass ratio of reducing agent and water；
(3) temperature is heated to 60 DEG C, the reducing agent solution of 3.3g oxidizing agent solution and 3.3g is added into reaction system,
3h is added dropwise at 80 DEG C in the reducing agent solution of the oxidizing agent solution of 29.7g and 29.7g after 0.5h, reaction terminates；
(4) after reaction, the hydrogenperoxide steam generator for being cooled to the 30wt% of 50 DEG C of addition 10g floats reaction product
It is white, it is cooled to room temperature finally to get color fixing agent.
Embodiment 5
The synthetic method of novel environment friendly chlorine-resistant color fixing agent, includes the following steps:
(1) epoxychloropropane of 60g, the diethylenetriamine of 100g, 100g diallylamine be added equipped with water segregator and
It is mixed in the round-bottomed flask of condenser pipe and is heated to 50 DEG C, and water is not further added by water segregator；
(2) 3g oxidant is weighed, is that 1:10 dissolved oxidant is molten to get oxidant according to the mass ratio of oxidant and water
Liquid；3g reducing agent is weighed, is the agent of 1:10 dissolving and reducing to get reducing agent solution according to the mass ratio of reducing agent and water；
(3) temperature is heated to 60 DEG C, the reducing agent solution of 3.3g oxidizing agent solution and 3.3g is added into reaction system,
3h is added dropwise at 85 DEG C in the reducing agent solution of the oxidizing agent solution of 29.7g and 29.7g after 0.5h, reaction terminates；
(4) after reaction, the hydrogenperoxide steam generator for being cooled to the 30wt% of 50 DEG C of addition 10g floats reaction product
It is white, it is cooled to room temperature finally to get color fixing agent.
Embodiment 6
The synthetic method of novel environment friendly chlorine-resistant color fixing agent, includes the following steps:
(1) epoxychloropropane of 60g, the diethylenetriamine of 100g, 100g diallylamine be added equipped with water segregator and
It is mixed in the round-bottomed flask of condenser pipe and is heated to 50 DEG C, and water is not further added by water segregator；
(2) 3g oxidant is weighed, is that 1:10 dissolved oxidant is molten to get oxidant according to the mass ratio of oxidant and water
Liquid；3g reducing agent is weighed, is the agent of 1:10 dissolving and reducing to get reducing agent solution according to the mass ratio of reducing agent and water；
(3) temperature is heated to 60 DEG C, the reducing agent solution of 3.3g oxidizing agent solution and 3.3g is added into reaction system,
3h is added dropwise at 90 DEG C in the reducing agent solution of the oxidizing agent solution of 29.7g and 29.7g after 0.5h, reaction terminates；
(4) after reaction, the hydrogenperoxide steam generator for being cooled to the 30wt% of 50 DEG C of addition 10g floats reaction product
It is white, it is cooled to room temperature finally to get color fixing agent.
Embodiment 7
The synthetic method of novel environment friendly chlorine-resistant color fixing agent, includes the following steps:
(1) epoxychloropropane of 60g, the diethylenetriamine of 100g, 100g diallylamine be added equipped with water segregator and
It is mixed in the round-bottomed flask of condenser pipe and is heated to 50 DEG C, and water is not further added by water segregator；
(2) 3g oxidant is weighed, is that 1:10 dissolved oxidant is molten to get oxidant according to the mass ratio of oxidant and water
Liquid；3g reducing agent is weighed, is the agent of 1:10 dissolving and reducing to get reducing agent solution according to the mass ratio of reducing agent and water；
(3) temperature is heated to 60 DEG C, the reducing agent solution of 3.3g oxidizing agent solution and 3.3g is added into reaction system,
3h is added dropwise at 95 DEG C in the reducing agent solution of the oxidizing agent solution of 29.7g and 29.7g after 0.5h, reaction terminates；
(4) after reaction, the hydrogenperoxide steam generator for being cooled to the 30wt% of 50 DEG C of addition 10g floats reaction product
It is white, it is cooled to room temperature finally to get color fixing agent.
Embodiment 8
The synthetic method of novel environment friendly chlorine-resistant color fixing agent, includes the following steps:
(1) epoxychloropropane of 80g, the diethylenetriamine of 100g, 100g diallylamine be added equipped with water segregator and
It is mixed in the round-bottomed flask of condenser pipe and is heated to 50 DEG C, and water is not further added by water segregator；
(2) 3g oxidant is weighed, is that 1:10 dissolved oxidant is molten to get oxidant according to the mass ratio of oxidant and water
Liquid；3g reducing agent is weighed, is the agent of 1:10 dissolving and reducing to get reducing agent solution according to the mass ratio of reducing agent and water；
(3) temperature is heated to 60 DEG C, the reducing agent solution of 3.3g oxidizing agent solution and 3.3g is added into reaction system,
3h is added dropwise at 70 DEG C in the reducing agent solution of the oxidizing agent solution of 29.7g and 29.7g after 0.5h, reaction terminates；
(4) after reaction, the hydrogenperoxide steam generator for being cooled to the 30wt% of 50 DEG C of addition 10g floats reaction product
It is white, it is cooled to room temperature finally to get color fixing agent.
Embodiment 9
The synthetic method of novel environment friendly chlorine-resistant color fixing agent, includes the following steps:
(1) epoxychloropropane of 60g, the diethylenetriamine of 80g, 80g diallylamine are added equipped with water segregator and cold
It is mixed in the round-bottomed flask of solidifying pipe and is heated to 50 DEG C, and water is not further added by water segregator；
(2) 3g oxidant is weighed, is that 1:10 dissolved oxidant is molten to get oxidant according to the mass ratio of oxidant and water
Liquid；3g reducing agent is weighed, is the agent of 1:10 dissolving and reducing to get reducing agent solution according to the mass ratio of reducing agent and water；
(3) temperature is heated to 60 DEG C, the reducing agent solution of 3.3g oxidizing agent solution and 3.3g is added into reaction system,
3h is added dropwise at 80 DEG C in the reducing agent solution of the oxidizing agent solution of 29.7g and 29.7g after 0.5h, reaction terminates；
(4) after reaction, the hydrogenperoxide steam generator for being cooled to the 30wt% of 50 DEG C of addition 10g floats reaction product
It is white, it is cooled to room temperature finally to get color fixing agent.
Embodiment 10
The synthetic method of novel environment friendly chlorine-resistant color fixing agent, includes the following steps:
(1) epoxychloropropane of 60g, the diethylenetriamine of 90g, 90g diallylamine are added equipped with water segregator and cold
It is mixed in the round-bottomed flask of solidifying pipe and is heated to 50 DEG C, and water is not further added by water segregator；
(2) 3g oxidant is weighed, is that 1:10 dissolved oxidant is molten to get oxidant according to the mass ratio of oxidant and water
Liquid；3g reducing agent is weighed, is the agent of 1:10 dissolving and reducing to get reducing agent solution according to the mass ratio of reducing agent and water；
(3) temperature is heated to 60 DEG C, the reducing agent solution of 3.3g oxidizing agent solution and 3.3g is added into reaction system,
3h is added dropwise at 70 DEG C in the reducing agent solution of the oxidizing agent solution of 29.7g and 29.7g after 0.5h, reaction terminates；
(4) after reaction, the hydrogenperoxide steam generator for being cooled to the 30wt% of 50 DEG C of addition 10g floats reaction product
It is white, it is cooled to room temperature finally to get color fixing agent.
Test method:
Red cotton looped fabric (dye strength 7%) is padded, rolling chlorine residue is 85%, then uses 120-160 DEG C of temperature
Drying.Red cotton looped fabric after drying crosses 1%-3%(with respect to cloth weight) color fixing agent, tested according to following standard:
1. soaping fastness is tested (1-5 grades, 5 grades best) by GB/T420-90；
2. chlorine fastness is tested by AATCC61-4A-2010 standard.
Example above-mentioned is merely illustrative, some features of feature for explaining the present invention.The attached claims
It is intended to the range as wide as possible for requiring to be contemplated that, and embodiments as presented herein is only according to all possible embodiment
Combined selection embodiment explanation.Therefore, the purpose of applicant is that the attached claims are not illustrated the present invention
Feature exemplary selectional restriction.And the progress in science and technology will be formed language express it is inaccurate due to and not
The possible equivalent being presently considered or son replacement, and these variations should also be interpreted in the conceived case by appended
Claim covering.
Claims (1)
1. a kind of synthetic method of environmental protection chlorine-resistant color fixing agent, which comprises the steps of:
(1) epoxychloropropane of 60g, the diethylenetriamine of 100g, 100g diallylamine are added and water segregator and condensation is housed
It is mixed in the round-bottomed flask of pipe and is heated to 50 DEG C, and water is not further added by water segregator；
(2) temperature is heated to 60 DEG C, 3.3g oxidizing agent solution and 3.3g reducing agent solution, 30min is added into reaction system
3h is added dropwise in 29.7g oxidizing agent solution and 29.7g reducing agent solution at 75 DEG C afterwards, reaction terminates；
(3) after reaction, the hydrogenperoxide steam generator for being cooled to the 30wt% of 50 DEG C of addition 10g bleaches reaction product,
It is cooled to room temperature finally to get color fixing agent；
The oxidizing agent solution is ammonium persulfate solution, and the quality of ammonium persulfate accounts for the 9.09% of oxidizing agent solution gross mass；Institute
Stating reducing agent solution is sodium metabisulfite solution, and the quality of sodium pyrosulfite accounts for the 9.09% of reducing agent solution gross mass；It is described
In hydrogenperoxide steam generator, the quality of hydrogen peroxide accounts for the 30% of hydrogenperoxide steam generator gross mass.
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| CN201610002041.3A CN105504227B (en) | 2016-01-06 | 2016-01-06 | A kind of synthetic method of environmental protection chlorine-resistant color fixing agent |
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| CN201610002041.3A CN105504227B (en) | 2016-01-06 | 2016-01-06 | A kind of synthetic method of environmental protection chlorine-resistant color fixing agent |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1077936C (en) * | 1995-03-18 | 2002-01-16 | 克莱里安特财务(Bvi)有限公司 | Textile dye-fixing agents |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1077936C (en) * | 1995-03-18 | 2002-01-16 | 克莱里安特财务(Bvi)有限公司 | Textile dye-fixing agents |
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