CN105951483B - A kind of color fixing agent for reactive dyeing and preparation method thereof - Google Patents
A kind of color fixing agent for reactive dyeing and preparation method thereof Download PDFInfo
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- CN105951483B CN105951483B CN201610339306.9A CN201610339306A CN105951483B CN 105951483 B CN105951483 B CN 105951483B CN 201610339306 A CN201610339306 A CN 201610339306A CN 105951483 B CN105951483 B CN 105951483B
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- fixing agent
- color fixing
- allyl
- reactive dyeing
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- 238000004045 reactive dyeing Methods 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000010992 reflux Methods 0.000 claims abstract description 20
- 239000003999 initiator Substances 0.000 claims abstract description 18
- 150000002460 imidazoles Chemical class 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 239000002253 acid Substances 0.000 claims abstract description 10
- 238000009833 condensation Methods 0.000 claims abstract description 10
- 230000005494 condensation Effects 0.000 claims abstract description 10
- -1 dihydroxy ethyl diallyl ammonium chloride Chemical compound 0.000 claims abstract description 10
- 238000009413 insulation Methods 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- 239000000178 monomer Substances 0.000 claims abstract description 7
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 24
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 18
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 16
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 13
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 10
- 235000019394 potassium persulphate Nutrition 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 6
- 239000011975 tartaric acid Substances 0.000 claims description 6
- 235000002906 tartaric acid Nutrition 0.000 claims description 6
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 2
- 150000003851 azoles Chemical class 0.000 claims 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 125000004205 trifluoroethyl group Chemical group [H]C([H])(*)C(F)(F)F 0.000 claims 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 abstract description 9
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 abstract description 9
- 238000010438 heat treatment Methods 0.000 abstract description 9
- 239000000975 dye Substances 0.000 description 9
- 239000004744 fabric Substances 0.000 description 8
- 239000003643 water by type Substances 0.000 description 8
- 235000019270 ammonium chloride Nutrition 0.000 description 7
- 239000004753 textile Substances 0.000 description 7
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 6
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 6
- 239000000985 reactive dye Substances 0.000 description 6
- 235000015165 citric acid Nutrition 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- 238000004043 dyeing Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000013112 stability test Methods 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 229920000742 Cotton Polymers 0.000 description 2
- 235000011054 acetic acid Nutrition 0.000 description 2
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 2
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 2
- 235000011130 ammonium sulphate Nutrition 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- WBZKQQHYRPRKNJ-UHFFFAOYSA-L disulfite Chemical compound [O-]S(=O)S([O-])(=O)=O WBZKQQHYRPRKNJ-UHFFFAOYSA-L 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013068 control sample Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 125000002883 imidazolyl group Chemical group 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000001151 other effect Effects 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical group 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 210000004243 sweat Anatomy 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F226/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen
- C08F226/06—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen by a heterocyclic ring containing nitrogen
-
- 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
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/38—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using reactive dyes
-
- 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
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/58—Material containing hydroxyl groups
- D06P3/60—Natural or regenerated cellulose
- D06P3/66—Natural or regenerated cellulose using reactive dyes
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Coloring (AREA)
Abstract
The present invention provides a kind of color fixing agent for reactive dyeing and preparation method thereof, and its step is as follows：(1) equipped with thermometer, agitator, reflux condenser reactor in sequentially add the imidazoles villaumite monomer, acrylic acid trifluoro second fat, dihydroxy ethyl diallyl ammonium chloride, acid regulator, deionized water after open reflux condensation mode, stirring, and begin to warm up heating；(2) when temperature rises to 85~100 DEG C, then start that the initiator solution that mass percent concentration is 1~10% is added dropwise, this initiator solution is formulated by the initiator and the part deionized water；Time for adding control at 0.5~3 hour, dropwise addition temperature control at 85~100 DEG C；(3) insulation reaction 1~5 hour again after adding, the water of surplus is subsequently added into, stirring discharges after 0.5 hour, produces the color fixing agent.
Description
Technical field
The invention belongs to field of fine chemical, more particularly to a kind of color fixing agent and its preparation side for reactive dyeing
Method.
Background technology
Reactive dye are cheap, chromatogram is complete, bright in colour, are widely used in cotton fabric dyeing process.Although reactive dye
Reactive group in molecule is easily with fiber with Covalent bonding together, but color fastness is unsatisfactory.It is in dyeing course, particularly
When contaminating dark, often occur to make the reactive dye that a large amount of non-sets on dyed fabric be present because dye strength is too high, these
The dyestuff of non-set is difficult to be removed from dyed fabric, and this some dyes will fade in washing process；Meanwhile some activity
The chemical bond facile hydrolysis formed between base and fiber, causes wet colour fastness relatively low.And the color fixing agent of early stage such as color fixing agent Y is first
The product of the reactions such as aldehyde, dicyandiamide and ammonium chloride, although every fastness of product dyed thereby can be improved, exist content of formaldehyde compared with
Height, the problems such as being detrimental to health, International Textile requirement is not met.With the continuous expansion of World Textile trade and people
The continuous improvement of people's living standard, environmental consciousness, higher requirement is proposed to indexs such as the comfortable of textile, cleaning, safety.
Since 21 century, World Textile Market proposes higher requirement to product dyed thereby items fastness, through fixation
Product dyed thereby after agent processing, not only there is the jail such as the soaping, wash of certain grade, rub resistance, perspiration resistance, sun-resistant, chlorine-resistant drift
Degree, but also require without formaldehyde, it is nontoxic, do not influence fabric feeling and discoloration etc..Therefore, research meets ecological, environmental protective, Wu Jia
The new reactive dyes of aldehyde are a significant job with color fixing agent.
The content of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of color fixing agent for reactive dyeing and
Its preparation method, the color fixing agent can more preferably improve fabric fastness to wet rubbing and color fastness to washing.
To achieve these goals, the present invention uses following technical scheme：
A kind of color fixing agent for reactive dyeing, include the raw material components of following portions by weight proportioning：
The imidazoles villaumite is 1- pi-allyl -3- methylimidazole villaumites, 1- pi-allyl -3- ethyl imidazol(e)s villaumite, 1- allyls
In base -3- hexyl imidazoliums villaumite, 1- pi-allyl -3- octylimidazole villaumites any one or it is two or more with it is any than mixing
Mixture.
The acid regulator is that the acid regulator is any one or two kinds in citric acid, tartaric acid, acetic acid
Above with any mixture than mixing.
The initiator be in ammonium persulfate, sodium peroxydisulfate and potassium peroxydisulfate any one or it is two or more arbitrarily to compare
The mixture of mixing.
A kind of preparation method of color fixing agent for reactive dyeing and preparation method thereof, is achieved by the steps of：
(1) equipped with thermometer, agitator, reflux condenser reactor in sequentially add the imidazoles villaumite monomer,
Reflux condensation mode is opened after acrylic acid trifluoro second fat, dihydroxy ethyl diallyl ammonium chloride, acid regulator, deionized water, is stirred,
And begin to warm up heating；
(2) when temperature rises to 85~100 DEG C, it is molten then to start the initiator that dropwise addition mass percent concentration is 1~10%
Liquid, this initiator solution are formulated by the initiator and the part deionized water；Time for adding control is small 0.5~3
When, temperature control is at 85~100 DEG C during dropwise addition；
(3) insulation reaction 1~5 hour again after adding, the water of surplus is subsequently added into, stirring discharges after 0.5 hour, produces institute
State color fixing agent.
Compared with prior art, the present invention has following remarkable result：
1st, by introducing imidazole group, hydroxyl, aliphatic radical, halogen isoreactivity group so that the color fixing agent of preparation is using
During, fixation agent molecule is crosslinked with reference to production color lake with dyestuff, the active group (such as hydroxyl, amino) of fiber molecule
(fixation), reaching reduces dyestuff to the compatibility of water, improves wet colour fastnesses such as the soaping of dyed fabric, staining and other effects.This
Outside, there is quaternary ammonium salt cationic group in molecule, pass through cation base and the sulfonic group of reactive dye (including its hydrolised dye)
Deng anion, Coulomb attraction effect occurs, neutralizes its electric charge, reduces the water solubility of dyestuff, and is combined with dye anion, increases
Active force between dye molecule and fiber molecule, to improve wet fastness.
2nd, the formaldehydeless pollution of prepared color fixing agent, fabric formaldehyde content is effectively reduced, lifts the quality of fabric, meet
Environmental requirement and the health demand of the people, there are wide market prospects.
Embodiment
The present invention is further elaborated on reference to embodiments.
A kind of color fixing agent for reactive dyeing of the present invention, include the raw material components of following portions by weight proportioning：
The imidazoles villaumite is 1- pi-allyl -3- methylimidazole villaumites, 1- pi-allyl -3- ethyl imidazol(e)s villaumite, 1- allyls
In base -3- hexyl imidazoliums villaumite, 1- pi-allyl -3- octylimidazole villaumites any one or it is two or more with it is any than mixing
Mixture.
The acid regulator is that the acid regulator is any one or two kinds in citric acid, tartaric acid, acetic acid
Above with any mixture than mixing.
The initiator be in ammonium persulfate, sodium peroxydisulfate or potassium peroxydisulfate any one or it is two or more arbitrarily to compare
The mixture of mixing.
A kind of preparation method of formaldehyde-free color fixing agent for reactive dyes of the present invention, is achieved by the steps of：
(1) equipped with thermometer, agitator, reflux condenser reactor in sequentially add the imidazoles villaumite monomer,
Reflux condensation mode is opened after acrylic acid trifluoro second fat, dihydroxy ethyl diallyl ammonium chloride, acid regulator, deionized water, is stirred,
And begin to warm up heating；
(2) when temperature rises to 85~100 DEG C, it is molten then to start the initiator that dropwise addition mass percent concentration is 1~10%
Liquid, this initiator solution are formulated by the initiator and the part deionized water；Time for adding control is small 0.5~3
When, temperature control is at 85~100 DEG C during dropwise addition；
(3) insulation reaction 1~5 hour again after adding, the water of surplus is subsequently added into, stirring discharges after 0.5 hour, produces institute
State color fixing agent.
With specific embodiment, the present invention is described in detail below, but the present invention is not limited only to this.
Embodiment one
A kind of color fixing agent for reactive dyeing of the present invention, the raw material components system matched by following portions by weight
Into：
Its preparation method, it is achieved by the steps of：
(1) equipped with thermometer, agitator, reflux condenser reactor in sequentially add 12 parts of 1- pi-allyl -3- first
Base imidazoles villaumite, 8 parts of acrylic acid trifluoro second fat, 10 parts of dihydroxy ethyl diallyl ammonium chlorides, 1 part of acetic acid, 10 parts of deionized waters
After open reflux condensation mode, stir, and begin to warm up heating；
(2) when temperature rises to 88 DEG C, then start that the ammonium persulfate solution that mass percent concentration is 2%, this mistake is added dropwise
Ammonium sulfate is formulated by 1 part of ammonium persulfate and 49 parts of deionized waters；Time for adding control temperature at 1 hour, dropwise addition
Control is at 90 DEG C；
(3) insulation reaction 3 hours again after adding, the water of surplus is subsequently added into, stirring discharges after 0.5 hour, produces described
Color fixing agent.
Embodiment two
A kind of color fixing agent for reactive dyeing of the present invention, the raw material components system matched by following portions by weight
Into：
Its preparation method, it is achieved by the steps of：
(1) equipped with thermometer, agitator, reflux condenser reactor in sequentially add 15 parts of 1- pi-allyl -3- second
Base imidazoles villaumite, 10 parts of acrylic acid trifluoro second fat, 12 parts of dihydroxy ethyl diallyl ammonium chlorides, 0.5 part of tartaric acid, 15 parts go from
Reflux condensation mode is opened after sub- water, is stirred, and begin to warm up heating；
(2) when temperature rises to 92 DEG C, then start that the sodium peroxydisulfate solution that mass percent concentration is 4%, this mistake is added dropwise
Metabisulfite solution is formulated by 0.5 part of sodium peroxydisulfate and 12 parts of deionized waters；Time for adding is controlled at 1.5 hours, dropwise addition
Temperature control is at 95 DEG C；
(3) insulation reaction 2.5 hours again after adding, the water of surplus is subsequently added into, stirring discharges after 0.5 hour, produces institute
State color fixing agent.
Embodiment three
A kind of color fixing agent for reactive dyeing of the present invention, the raw material components system matched by following portions by weight
Into：
Its preparation method, it is achieved by the steps of：
(1) equipped with thermometer, agitator, reflux condenser reactor in sequentially add 18 parts of 1- pi-allyls -3- oneself
Base imidazoles villaumite, 15 parts of acrylic acid trifluoro second fat, 15 parts of dihydroxy ethyl diallyl ammonium chlorides, 1 part of citric acid, 20 parts of deionizations
Reflux condensation mode is opened after water, is stirred, and begin to warm up heating；
(2) when temperature rises to 96 DEG C, then start that the potassium persulfate solution that mass percent concentration is 5%, this mistake is added dropwise
Potassium sulfate solution is formulated by 1 part of potassium peroxydisulfate and 19 parts of deionized waters；Time for adding control temperature at 1.5 hours, dropwise addition
Degree control is at 98 DEG C；
(3) insulation reaction 3.5 hours again after adding, the water of surplus is subsequently added into, stirring discharges after 0.5 hour, produces institute
State color fixing agent.
Example IV
A kind of color fixing agent for reactive dyeing of the present invention, the raw material components system matched by following portions by weight
Into：
Its preparation method, it is achieved by the steps of：
(1) equipped with thermometer, agitator, reflux condenser reactor in sequentially add 20 parts of 1- pi-allyls -3- pungent
Base imidazoles villaumite, 18 parts of acrylic acid trifluoro second fat, 20 parts of dihydroxy ethyl diallyl ammonium chlorides, 1 part of tartaric acid, 10 parts of deionizations
Reflux condensation mode is opened after water, is stirred, and begin to warm up heating；
(2) when temperature rises to 95 DEG C, then start that the ammonium persulfate solution that mass percent concentration is 5%, this mistake is added dropwise
Ammonium sulfate is formulated by 1 part of ammonium persulfate and 19 parts of part deionized water；Time for adding was controlled at 2.5 hours, was added dropwise
When temperature control at 98 DEG C；
(3) insulation reaction 3 hours again after adding, the water of surplus is subsequently added into, stirring discharges after 0.5 hour, produces described
Color fixing agent.
Embodiment five
A kind of color fixing agent for reactive dyeing of the present invention, the raw material components system matched by following portions by weight
Into：
Wherein：Imidazoles villaumite monomer uses 1- pi-allyl -3- methylimidazole villaumites and 1- pi-allyl -3- ethyl imidazol(e) villaumites
Mixture, and the amount ratio of 1- pi-allyl -3- methylimidazole villaumites and 1- pi-allyl -3- ethyl imidazol(e) villaumites be 1:1, i.e.
1- pi-allyl -3- methylimidazole villaumites and the dosage of 1- pi-allyl -3- ethyl imidazol(e) villaumites are 11 parts.
Its preparation method, it is achieved by the steps of：
(1) equipped with thermometer, agitator, reflux condenser reactor in sequentially add 11 parts of 1- pi-allyl -3- first
Base imidazoles villaumite, 11 parts of 1- pi-allyl -3- ethyl imidazol(e)s villaumites, 12 parts of acrylic acid trifluoro second fat, 25 parts of allyls of dihydroxy ethyl two
Reflux condensation mode is opened after ammonium chloride, 1.5 parts of citric acids, 10 parts of deionized waters, is stirred, and begin to warm up heating；
(2) when temperature rises to 90 DEG C, then start that the sodium peroxydisulfate solution that mass percent concentration is 5%, this mistake is added dropwise
Metabisulfite solution is formulated by 1 part of sodium peroxydisulfate and 19 parts of deionized waters；Time for adding control temperature at 2.5 hours, dropwise addition
Degree control is at 96 DEG C；
(3) insulation reaction 4 hours again after adding, the water of surplus is subsequently added into, stirring discharges after 0.5 hour, produces described
Color fixing agent.
Embodiment six
A kind of color fixing agent for reactive dyeing of the present invention, the raw material components system matched by following portions by weight
Into：
Wherein：
Imidazoles villaumite monomer is using the mixed of 1- pi-allyl -3- methylimidazole villaumites and 1- pi-allyl -3- ethyl imidazol(e) villaumites
Compound, and the amount ratio of 1- pi-allyl -3- methylimidazole villaumites and 1- pi-allyl -3- ethyl imidazol(e) villaumites is 1:2, i.e. 1- alkene
Propyl group -3- methylimidazole villaumites and the dosage of 1- pi-allyl -3- ethyl imidazol(e) villaumites are respectively 8 parts and 16 parts.
Initiator is using sodium peroxydisulfate and the mixture of potassium peroxydisulfate, and the amount ratio of sodium peroxydisulfate and potassium peroxydisulfate is 1:
2, i.e. the dosage of sodium peroxydisulfate and potassium peroxydisulfate is respectively 0.75 part.
Its preparation method, it is achieved by the steps of：
(1) equipped with thermometer, agitator, reflux condenser reactor in sequentially add 8 parts of 1- pi-allyl -3- methyl
Imidazoles villaumite and 16 parts of 1- pi-allyl -3- ethyl imidazol(e)s villaumites, 6 parts of acrylic acid trifluoro second fat, 10 parts of dihydroxy ethyl diallyls
Reflux condensation mode is opened after ammonium chloride, 0.5 part of acetic acid, 8 parts of deionized waters, is stirred, and begin to warm up heating；
(2) when temperature rises to 92 DEG C, then start that the initiator solution that mass percent concentration is 3% is added dropwise, this initiation
Agent solution is formulated by 0.75 part of sodium peroxydisulfate, 0.75 part of potassium peroxydisulfate and 48.5 parts of deionized waters；Time for adding is controlled 2
Hour, temperature control is at 97 DEG C during dropwise addition；
(3) insulation reaction 4.5 hours again after adding, the water of surplus is subsequently added into, stirring discharges after 0.5 hour, produces institute
State color fixing agent.
By above-described embodiment one to the six directions into color fixing agent handle the bafta after the dyeing of 3 grams of reactive scarlet respectively, use
The solid technique of leaching, color fixing agent dosage are 2% (o.w.f), and pH is 6~7, and temperature is 60 DEG C, time 30min, bath raio 1:12.Cotton is knitted
Main performance index after thing fixation is as shown in table 1.
Main performance index of the bafta of table 1 after the fixation treatment of above-described embodiment one to six
Remarks：
1. crock fastness method of testing presses GB/T3920-2008《Textile color stability tests colour fastness to rubbing》Method is surveyed
It is fixed；
2. soaping fastness method of testing presses GB/T3921-2008《Textile color stability tests color fastness to washing》Method is surveyed
It is fixed；
3. sweat leaching fastness method of testing presses GB/T5713-2013《Textile color stability tests color fastness to water》Method is surveyed
It is fixed.
4. control sample is the aldehyde-free colour stabilizer of Guangzhou Zhuan Jie Chemical Co., Ltd.s production, concentration 30%.
Described in above, only this wound is used using the embodiment of this origination techniques content, any those skilled in the art
Make done modifications and changes, all belong to the scope of the claims of this creation opinion, and be not limited to those disclosed embodiments.
Claims (8)
- A kind of 1. color fixing agent for reactive dyeing, it is characterised in that：Include the raw material components of following portions by weight proportioning：
- A kind of 2. color fixing agent for reactive dyeing according to claim 1, it is characterised in that：The imidazoles villaumite Monomer is 1- pi-allyl -3- methylimidazole villaumites, 1- pi-allyl -3- ethyl imidazol(e)s villaumite, 1- pi-allyl -3- hexyl imidazolium chlorine Any one in salt, 1- pi-allyl -3- octylimidazole villaumites or the two or more mixtures with any ratio mixing.
- A kind of 3. color fixing agent for reactive dyeing according to claim 1, it is characterised in that：The acid regulation Agent is any one or the two or more mixtures with any ratio mixing in citric acid, tartaric acid, acetic acid.
- A kind of 4. color fixing agent for reactive dyeing according to claim 1, it is characterised in that：The initiator is Any one in ammonium persulfate, sodium peroxydisulfate or potassium peroxydisulfate or the two or more mixtures with any ratio mixing.
- A kind of 5. preparation side of color fixing agent for reactive dyeing according to Claims 1-4 any claim Method, it is characterised in that be achieved by the steps of：(1) equipped with thermometer, agitator, reflux condenser reactor in sequentially add the imidazoles villaumite monomer, propylene Reflux condensation mode is opened after sour trifluoro ethyl ester, dihydroxy ethyl diallyl ammonium chloride, acid regulator, deionized water, is stirred, and open Beginning heat temperature raising；(2) when temperature rises to 85~100 DEG C, then start that the initiator solution that mass percent concentration is 1~10% is added dropwise, this Initiator solution is formulated by the initiator and the part deionized water；Time for adding was controlled at 0.5~3 hour, drop Added-time temperature control is at 85~100 DEG C；(3) insulation reaction 1~5 hour again after adding, is subsequently added into the water of surplus, and stirring discharges after 0.5 hour, produced described solid Toner.
- A kind of 6. preparation method of color fixing agent for reactive dyeing according to claim 5, it is characterised in that：Institute Imidazoles villaumite is stated as 1- pi-allyl -3- methylimidazole villaumites, 1- pi-allyl -3- ethyl imidazol(e)s villaumite, 1- pi-allyl -3- hexyl miaows Any one in azoles villaumite, 1- pi-allyl -3- octylimidazole villaumites or the two or more mixtures with any ratio mixing.
- A kind of 7. preparation method of color fixing agent for reactive dyeing according to claim 5, it is characterised in that：Institute Acid regulator is stated as any one in citric acid, tartaric acid, acetic acid or two or more with any mixture than mixing.
- A kind of 8. preparation method of color fixing agent for reactive dyeing according to claim 5, it is characterised in that：Institute Initiator is stated as any one in ammonium persulfate, sodium peroxydisulfate or potassium peroxydisulfate or two or more with any mixing than mixing Thing.
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| CN201711480067.XA CN108049223B (en) | 2016-05-20 | 2016-05-20 | Color fixing agent for reactive dye dyeing and preparation method thereof |
| CN201810000214.7A CN108179642B (en) | 2016-05-20 | 2016-05-20 | Preparation method of color fixing agent for reactive dye dyeing |
| CN201610339306.9A CN105951483B (en) | 2016-05-20 | 2016-05-20 | A kind of color fixing agent for reactive dyeing and preparation method thereof |
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| CN201810000214.7A Division CN108179642B (en) | 2016-05-20 | 2016-05-20 | Preparation method of color fixing agent for reactive dye dyeing |
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| CN105951483B (en) * | 2016-05-20 | 2018-01-12 | 刘剑锋 | A kind of color fixing agent for reactive dyeing and preparation method thereof |
| CN106758411A (en) * | 2016-12-07 | 2017-05-31 | 郑州源冉生物技术有限公司 | A kind of alkaline-resisting environmentally friendly color fixing agent of activity and preparation method thereof |
| CN108660811A (en) * | 2018-07-06 | 2018-10-16 | 李美琴 | A kind of quaternary ammonium salt cationic color fixing agent and preparation method thereof |
| CN111287002B (en) * | 2020-03-26 | 2021-07-13 | 广州三骏佳纺织合成材料厂有限公司 | Formaldehyde-free chlorine-resistant color fixing agent and preparation method thereof |
| CN112574355B (en) * | 2020-11-16 | 2022-03-18 | 临清三和纺织集团有限公司 | Active dye acid-proof agent and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS57154480A (en) * | 1981-03-12 | 1982-09-24 | Sanyo Chemical Ind Ltd | Wet fastness increasing agent and method |
| DE3703293A1 (en) * | 1987-02-04 | 1988-08-18 | Cassella Ag | WET FASTNESS IMPROVEMENT OF SULFUR DYE COLORS |
| JPH06108382A (en) * | 1992-09-25 | 1994-04-19 | Senka Kk | Improvement of wet color fastness |
| CN101608407B (en) * | 2009-07-04 | 2011-01-26 | 金根苗 | Production process for improving wet rubbing fastness of reactive dye |
| CN101768883B (en) * | 2009-12-25 | 2011-06-29 | 青岛大学 | Preparation method of formaldehyde-free active dye fixing agent |
| CN102493222B (en) * | 2011-11-08 | 2014-01-01 | 青岛大学 | Dyeing method of reactive dye containing ionic liquid |
| CN102797170B (en) * | 2012-09-06 | 2014-08-13 | 苏州联胜化学有限公司 | Formaldehyde-free fixing agent and preparation method thereof |
| CN103397539B (en) * | 2013-07-10 | 2015-08-26 | 宁波市江北东丽化工助剂有限公司 | A kind of REACTIVE DYES promoter and preparation method thereof |
| CN103696296B (en) * | 2013-12-27 | 2015-12-30 | 石狮市清源精细化工有限公司 | A kind of REACTIVE DYES cationic formaldehyde-free fixing agent and preparation method thereof |
| CN104452368B (en) * | 2014-12-30 | 2016-08-17 | 福建清源科技有限公司 | A kind of formaldehyde-free color fixing agent for reactive dyes and preparation method thereof |
| CN105332298A (en) * | 2015-12-10 | 2016-02-17 | 陈逸君 | Color fixing agent for dyeing of reactive dyes |
| CN105951483B (en) * | 2016-05-20 | 2018-01-12 | 刘剑锋 | A kind of color fixing agent for reactive dyeing and preparation method thereof |
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| CN105951483A (en) | 2016-09-21 |
| CN108049223B (en) | 2020-01-10 |
| CN108179642B (en) | 2020-11-13 |
| CN108049223A (en) | 2018-05-18 |
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Denomination of invention: A fixing agent for reactive dye dyeing and its preparation method Effective date of registration: 20231017 Granted publication date: 20180112 Pledgee: Jiangxi Hukou rural commercial bank Limited by Share Ltd. Pledgor: Jiujiang Zhongjia Industrial Co.,Ltd. Registration number: Y2023980061576 |
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