CN105951483A - color fixing agent for reactive dyeing and preparation method of color fixing agent - Google Patents
color fixing agent for reactive dyeing and preparation method of color fixing agent Download PDFInfo
- Publication number
- CN105951483A CN105951483A CN201610339306.9A CN201610339306A CN105951483A CN 105951483 A CN105951483 A CN 105951483A CN 201610339306 A CN201610339306 A CN 201610339306A CN 105951483 A CN105951483 A CN 105951483A
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- CN
- China
- Prior art keywords
- fixing agent
- color fixing
- villaumite
- allyl
- reactive dyeing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000004045 reactive dyeing Methods 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000010992 reflux Methods 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 20
- 239000003999 initiator Substances 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 238000009833 condensation Methods 0.000 claims abstract description 10
- 230000005494 condensation Effects 0.000 claims abstract description 10
- 238000007599 discharging Methods 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 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
- 239000000203 mixture Substances 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 11
- 239000002253 acid Substances 0.000 claims description 10
- -1 imidazoles chlorine Salt Chemical class 0.000 claims description 10
- 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
- 238000009413 insulation Methods 0.000 claims description 9
- 235000019394 potassium persulphate Nutrition 0.000 claims description 9
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 8
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 8
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 8
- 150000002460 imidazoles Chemical class 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
- 239000002994 raw material Substances 0.000 claims description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 abstract description 10
- 235000019270 ammonium chloride Nutrition 0.000 abstract description 7
- JDIIGWSSTNUWGK-UHFFFAOYSA-N 1h-imidazol-3-ium;chloride Chemical compound [Cl-].[NH2+]1C=CN=C1 JDIIGWSSTNUWGK-UHFFFAOYSA-N 0.000 abstract 1
- VBHXIMACZBQHPX-UHFFFAOYSA-N 2,2,2-trifluoroethyl prop-2-enoate Chemical compound FC(F)(F)COC(=O)C=C VBHXIMACZBQHPX-UHFFFAOYSA-N 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 15
- 239000000975 dye Substances 0.000 description 11
- 239000003643 water by type Substances 0.000 description 10
- 239000004744 fabric Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- 239000004753 textile Substances 0.000 description 6
- 150000004968 peroxymonosulfuric acids Chemical class 0.000 description 5
- 239000000985 reactive dye Substances 0.000 description 5
- 235000015165 citric acid Nutrition 0.000 description 4
- 238000004043 dyeing Methods 0.000 description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 150000003851 azoles Chemical class 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000013112 stability test Methods 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 235000011054 acetic acid Nutrition 0.000 description 2
- 150000003863 ammonium salts Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 230000001166 anti-perspirative effect Effects 0.000 description 1
- 239000003213 antiperspirant Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000013068 control sample Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000002242 deionisation method Methods 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
- 238000005516 engineering process Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine 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
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000011591 potassium Substances 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
- PYNUOAIJIQGACY-UHFFFAOYSA-N propylazanium;chloride Chemical compound Cl.CCCN PYNUOAIJIQGACY-UHFFFAOYSA-N 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 230000001681 protective effect Effects 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
- 238000005406 washing Methods 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 invention provides a color fixing agent for reactive dyeing and a preparation method of the color fixing agent. The preparation method includes the steps: (1) sequentially adding imidazolium chloride monomers, trifluoroethyl acrylate, dihydroxyethyldiallyl ammonium chloride, acidity regulator and deionized water into a reaction kettle equipped with a thermometer, a stirrer and a reflux condenser prior to starting reflux condensation, stirring and starting heating to increase temperature; (2) when the temperature rises to 85-100 DEG C, then dropwise adding initiator solution which is 1-10% in mass concentration and prepared with initiator and part of the deionized water, controlling the dropwise adding time between 0.5 hour and 3 hours, and controlling the temperature between 85 DEG C and 100 DEG C during dropwise adding; (3) after addition, performing thermal reaction for 1-5 hours, then adding the balance water, and discharging after stirring for 0.5 hour to obtain the color fixing agent.
Description
Technical field
The invention belongs to field of fine chemical, particularly to a kind of color fixing agent for reactive dyeing
And preparation method thereof.
Background technology
Reactive dye are cheap, chromatograph is complete, bright in colour, be widely used in cotton fabric dyeing process.
Although the reactive group in reactive dyestuff molecule is easily combined with covalent bond with fiber, but color fastness is not
Preferable.It is in dyeing course, when particularly dye is dark, often occurs because dye strength is too high
Making to exist on dyed fabric the reactive dye of a large amount of non-set, the dyestuff of these non-sets is difficult to from dyeing
Eccysis on fabric, this some dyes will fade in washing process；Meanwhile, some active group is with fine
The chemical bond facile hydrolysis formed between dimension, causes wet colour fastness relatively low.And color fixing agent in early days is as solid
Toner Y is the product of the reactions such as formaldehyde, dicyandiamide and ammonium chloride, although can improve each of product dyed thereby
Fastness, but it is higher to there is content of formaldehyde, and the problem such as be detrimental to health, and has not met the world and has spun
Fabric requirement.Along with constantly expanding and living standards of the people, environmental consciousness of World Textile trade
Improve constantly, to textile comfortable, cleaning, safety etc. index propose higher requirement.
Since entering 21 century, World Textile Market fastness every to product dyed thereby proposes higher wanting
Ask, the product dyed thereby after color fixing agent processes, not only to have the soaping of certain grade, wash, rub resistance,
The fastness such as perspiration resistance, sun-resistant, chlorine-resistant drift, but also require without formaldehyde, nontoxic, do not affect and knit
Thing feel and complexion changed etc..Therefore, research meets ecological, environmental protective, formaldehydeless new reactive dyes with solid
Toner is a significant job.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that a kind of for reactive dyeing
Color fixing agent and preparation method thereof, this color fixing agent can more preferably improve fabric fastness to wet rubbing and washable color jail
Degree.
To achieve these goals, the present invention is by the following technical solutions:
A kind of color fixing agent for reactive dyeing, including the raw material components of following portions by weight proportioning:
Described imidazoles villaumite is 1-pi-allyl-3-Methylimidazole. villaumite, 1-pi-allyl-3-ethyl imidazol(e) chlorine
Any one in salt, 1-pi-allyl-3-hexyl imidazolium villaumite, 1-pi-allyl-3-octylimidazole villaumite
Or it is two or more with any mixture than mixing.
Described acid regulator be described acid regulator be any in citric acid, tartaric acid, acetic acid
One or more are with any mixture than mixing.
Described initiator be any one or two kinds in Ammonium persulfate., sodium peroxydisulfate and potassium peroxydisulfate with
On with any than mixing mixture.
The preparation method of a kind of color fixing agent for reactive dyeing and preparation method thereof, by as follows
Step realizes:
(1) equipped with thermometer, agitator, reflux condenser reactor in be sequentially added into described miaow
Azoles villaumite monomer, acrylic acid trifluoro second fat, dihydroxy ethyl diallyl ammonium chloride, acid regulator,
Open reflux condensation mode, stirring after deionized water, and begin to warm up intensification；
(2), when temperature rises to 85～100 DEG C, then starting to drip mass percent concentration is 1～10%
Initiator solution, this initiator solution is formulated by the described deionized water of described initiator and part；
Time for adding controls at 0.5～3 hour, and during dropping, temperature controls at 85～100 DEG C；
(3) insulation reaction 1～5 hours again after adding, be subsequently added into the water of surplus, and stirring 0.5 is little
Discharging time after, obtains described color fixing agent.
Compared with prior art, the present invention has a following remarkable result:
1, by introducing imidazole group, hydroxyl, aliphatic radical, halogen isoreactivity group so that preparation
Color fixing agent in use, color fixing agent molecule and dyestuff, fiber molecule active group (as hydroxyl,
Amino etc.) crosslink combination production color lake (fixation), reduce the dyestuff affinity to water,
Improve the effects such as wet colour fastness such as the soaping of dyed fabric, staining.Additionally, molecule has quaternary ammonium
Salt cation group, by the moon such as the sulfonic groups of cation base and reactive dye (including its hydrolised dye)
, there is Coulomb attraction effect in ion, neutralizes its electric charge, reduces the water solublity of dyestuff, and cloudy with dyestuff
Ions binding, increases the active force between dye molecule and fiber molecule, to improve wet fastness.
2, the formaldehydeless pollution of prepared color fixing agent, effectively reduces fabric formaldehyde content, promotes fabric
Quality, meet the health demand of environmental requirement and the people, there is wide market prospect.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further elaborated on.
A kind of color fixing agent for reactive dyeing of the present invention, including following portions by weight proportioning
Raw material components:
Described imidazoles villaumite is 1-pi-allyl-3-Methylimidazole. villaumite, 1-pi-allyl-3-ethyl imidazol(e) chlorine
Any one in salt, 1-pi-allyl-3-hexyl imidazolium villaumite, 1-pi-allyl-3-octylimidazole villaumite
Or it is two or more with any mixture than mixing.
Described acid regulator be described acid regulator be any in citric acid, tartaric acid, acetic acid
One or more are with any mixture than mixing.
Described initiator be any one or two kinds in Ammonium persulfate., sodium peroxydisulfate or potassium peroxydisulfate with
On with any than mixing mixture.
The preparation method of a kind 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 be sequentially added into described miaow
Azoles villaumite monomer, acrylic acid trifluoro second fat, dihydroxy ethyl diallyl ammonium chloride, acid regulator,
Open reflux condensation mode, stirring after deionized water, and begin to warm up intensification；
(2), when temperature rises to 85～100 DEG C, then starting to drip mass percent concentration is 1～10%
Initiator solution, this initiator solution is formulated by the described deionized water of described initiator and part；
Time for adding controls at 0.5～3 hour, and during dropping, temperature controls at 85～100 DEG C；
(3) insulation reaction 1～5 hours again after adding, be subsequently added into the water of surplus, and stirring 0.5 is little
Discharging time after, obtains described 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, former by following portions by weight proportioning
Material component is made:
Its preparation method, is achieved by the steps of:
(1) equipped with thermometer, agitator, reflux condenser reactor in be sequentially added into 12 parts
1-pi-allyl-3-Methylimidazole. villaumite, 8 parts of acrylic acid trifluoro second fat, 10 parts of dihydroxy ethyl diallyls
Open reflux condensation mode, stirring after ammonium chloride, 1 part of acetic acid, 10 parts of deionized waters, and begin to warm up liter
Temperature；
(2), when temperature rises to 88 DEG C, then start to drip the persulfuric acid that mass percent concentration is 2%
Ammonium salt solution, this ammonium persulfate solution is formulated by 1 part of Ammonium persulfate. and 49 parts of deionized waters；Dropping
Time controls at 1 hour, and during dropping, temperature controls at 90 DEG C；
(3) insulation reaction 3 hours again after adding, are subsequently added into the water of surplus, after stirring 0.5 hour
Discharging, obtains described color fixing agent.
Embodiment two
A kind of color fixing agent for reactive dyeing of the present invention, former by following portions by weight proportioning
Material component is made:
Its preparation method, is achieved by the steps of:
(1) equipped with thermometer, agitator, reflux condenser reactor in be sequentially added into 15 parts
1-pi-allyl-3-ethyl imidazol(e) villaumite, 10 parts of acrylic acid trifluoro second fat, 12 parts of dihydroxy ethyl two allyls
Open reflux condensation mode, stirring after ammonium chloride, 0.5 part of tartaric acid, 15 parts of deionized waters, and start
Heat temperature raising；
(2), when temperature rises to 92 DEG C, then start to drip the persulfuric acid that mass percent concentration is 4%
Sodium solution, this sodium peroxydisulfate solution is formulated by 0.5 part of sodium peroxydisulfate and 12 parts of deionized waters；Drip
Adding the time controls at 1.5 hours, and during dropping, temperature controls at 95 DEG C；
(3) insulation reaction 2.5 hours again after adding, are subsequently added into the water of surplus, stir 0.5 hour
Rear discharging, obtains described color fixing agent.
Embodiment three
A kind of color fixing agent for reactive dyeing of the present invention, former by following portions by weight proportioning
Material component is made:
Its preparation method, is achieved by the steps of:
(1) equipped with thermometer, agitator, reflux condenser reactor in be sequentially added into 18 parts
1-pi-allyl-3-hexyl imidazolium villaumite, 15 parts of acrylic acid trifluoro second fat, 15 parts of dihydroxy ethyl diene
Open reflux condensation mode, stirring after propyl ammonium chloride, 1 part of citric acid, 20 parts of deionized waters, and start
Heat temperature raising；
(2), when temperature rises to 96 DEG C, then start to drip the persulfuric acid that mass percent concentration is 5%
Potassium solution, this potassium persulfate solution is formulated by 1 part of potassium peroxydisulfate and 19 parts of deionized waters；Dropping
Time controls at 1.5 hours, and during dropping, temperature controls at 98 DEG C；
(3) insulation reaction 3.5 hours again after adding, are subsequently added into the water of surplus, stir 0.5 hour
Rear discharging, obtains described color fixing agent.
Embodiment four
A kind of color fixing agent for reactive dyeing of the present invention, former by following portions by weight proportioning
Material component is made:
Its preparation method, is achieved by the steps of:
(1) equipped with thermometer, agitator, reflux condenser reactor in be sequentially added into 20 parts
1-pi-allyl-3-octylimidazole villaumite, 18 parts of acrylic acid trifluoro second fat, 20 parts of dihydroxy ethyl two allyls
Open reflux condensation mode, stirring after ammonium chloride, 1 part of tartaric acid, 10 parts of deionized waters, and start to add
Heat heats up；
(2), when temperature rises to 95 DEG C, then start to drip the persulfuric acid that mass percent concentration is 5%
Ammonium salt solution, this ammonium persulfate solution is formulated by 1 part of Ammonium persulfate. and 19 parts of deionized waters of part；
Time for adding controls at 2.5 hours, and during dropping, temperature controls at 98 DEG C；
(3) insulation reaction 3 hours again after adding, are subsequently added into the water of surplus, after stirring 0.5 hour
Discharging, obtains described color fixing agent.
Embodiment five
A kind of color fixing agent for reactive dyeing of the present invention, former by following portions by weight proportioning
Material component is made:
Wherein: imidazoles villaumite monomer uses 1-pi-allyl-3-Methylimidazole. villaumite and 1-pi-allyl-3-second
The mixture of base imidazoles villaumite, and 1-pi-allyl-3-Methylimidazole. villaumite and 1-pi-allyl-3-ethyl miaow
The amount ratio of azoles villaumite is 1:1, i.e. 1-pi-allyl-3-Methylimidazole. villaumite and 1-pi-allyl-3-second
The consumption of base imidazoles villaumite is 11 parts.
Its preparation method, is achieved by the steps of:
(1) equipped with thermometer, agitator, reflux condenser reactor in be sequentially added into 11 parts
1-pi-allyl-3-Methylimidazole. villaumite, 11 parts of 1-pi-allyl-3-ethyl imidazol(e) villaumites, 12 parts of propylene
Acid trifluoro second fat, 25 parts of dihydroxy ethyl diallyl ammonium chlorides, 1.5 parts of citric acids, 10 parts of deionizations
Open reflux condensation mode, stirring after water, and begin to warm up intensification；
(2), when temperature rises to 90 DEG C, then start to drip the persulfuric acid that mass percent concentration is 5%
Sodium solution, this sodium peroxydisulfate solution is formulated by 1 part of sodium peroxydisulfate and 19 parts of deionized waters；Dropping
Time controls at 2.5 hours, and during dropping, temperature controls at 96 DEG C；
(3) insulation reaction 4 hours again after adding, are subsequently added into the water of surplus, after stirring 0.5 hour
Discharging, obtains described color fixing agent.
Embodiment six
A kind of color fixing agent for reactive dyeing of the present invention, former by following portions by weight proportioning
Material component is made:
Wherein:
Imidazoles villaumite monomer uses 1-pi-allyl-3-Methylimidazole. villaumite and 1-pi-allyl-3-ethyl imidazol(e)
The mixture of villaumite, and 1-pi-allyl-3-Methylimidazole. villaumite and 1-pi-allyl-3-ethyl imidazol(e) villaumite
Amount ratio be 1:2, i.e. 1-pi-allyl-3-Methylimidazole. villaumite and 1-pi-allyl-3-ethyl imidazol(e)
The consumption of villaumite is respectively 8 parts and 16 parts.
Initiator uses sodium peroxydisulfate and the mixture of potassium peroxydisulfate, and sodium peroxydisulfate and potassium peroxydisulfate
Amount ratio is 1:2, i.e. the consumption of sodium peroxydisulfate and potassium peroxydisulfate is respectively 0.75 part.
Its preparation method, is achieved by the steps of:
(1) equipped with thermometer, agitator, reflux condenser reactor in be sequentially added into 8 parts of 1-
Pi-allyl-3-Methylimidazole. villaumite and 16 parts of 1-pi-allyl-3-ethyl imidazol(e) villaumites, 6 parts of acrylic acid three
Open after fluorine second fat, 10 parts of dihydroxy ethyl diallyl ammonium chlorides, 0.5 part of acetic acid, 8 parts of deionized waters
Reflux condensation mode, stirring, and begin to warm up intensification；
(2), when temperature rises to 92 DEG C, then start to drip the initiator that mass percent concentration is 3%
Solution, this initiator solution by 0.75 part of sodium peroxydisulfate, 0.75 part of potassium peroxydisulfate and 48.5 parts go from
Sub-water is formulated；Time for adding controls at 2 hours, and during dropping, temperature controls at 97 DEG C；
(3) insulation reaction 4.5 hours again after adding, are subsequently added into the water of surplus, stir 0.5 hour
Rear discharging, obtains described color fixing agent.
The color fixing agent that above-described embodiment one to six directions becomes processes cotton after reactive scarlet 3 grams dyeing respectively knit
Thing, uses the solid technique of leaching, and color fixing agent consumption is 2% (o.w.f), and pH is 6～7, and temperature is 60 DEG C,
Time is 30min, bath raio 1:12.Main performance index after bafta fixation is as shown in table 1.
Table 1 bafta main performance index after above-described embodiment one to six fixation treatment
Remarks:
1. crock fastness method of testing presses GB/T3920-2008 " textile color stability test rub resistance color jail
Degree " method mensuration；
2. soaping fastness method of testing presses GB/T3921-2008 " textile color stability test washable color jail
Degree " method mensuration；
3. antiperspirant leaching fastness method of testing presses GB/T5713-2013 " textile color stability test resistance to water colour jail
Degree " method mensuration.
4. control sample is the aldehyde-free colour stabilizer that Guangzhou Zhuan Jie Chemical Co., Ltd. produces, and concentration is 30%.
Described above, only utilize the embodiment of this origination techniques content, any be familiar with art
Person uses modification, the change that this creation done, and all belongs to the scope of the claims that this creation is advocated, and is not limited to
Those disclosed embodiments.
Claims (8)
1. the color fixing agent for reactive dyeing, it is characterised in that: include following portions by weight proportioning
Raw material components:
A kind of color fixing agent for reactive dyeing the most according to claim 1, it is characterised in that:
Described imidazoles villaumite monomer be 1-pi-allyl-3-Methylimidazole. villaumite, 1-pi-allyl-3-ethyl imidazol(e) villaumite,
Any one or two kinds in 1-pi-allyl-3-hexyl imidazolium villaumite, 1-pi-allyl-3-octylimidazole villaumite with
On with any than mixing mixture.
A kind of color fixing agent for reactive dyeing the most according to claim 1, it is characterised in that:
Described acid regulator be in citric acid, tartaric acid, acetic acid any one or two or more with any than mixed
The mixture closed.
A kind of color fixing agent for reactive dyeing the most according to claim 1, it is characterised in that:
Described initiator be in Ammonium persulfate., sodium peroxydisulfate or potassium peroxydisulfate any one or two or more with arbitrarily
Mixture than mixing.
5. according to a kind of fixation for reactive dyeing described in Claims 1-4 any claim
The preparation method of agent, it is characterised in that be achieved by the steps of:
(1) equipped with thermometer, agitator, reflux condenser reactor in be sequentially added into described imidazoles chlorine
Salt monomer, acrylic acid trifluoro second fat, dihydroxy ethyl diallyl ammonium chloride, acid regulator, deionized water
Rear unlatching reflux condensation mode, stirring, and begin to warm up intensification；
(2), when temperature rises to 85～100 DEG C, then starting to drip mass percent concentration is 1～10% draw
Sending out agent solution, this initiator solution is formulated by the described deionized water of described initiator and part；During dropping
Between control at 0.5～3 hour, during dropping, temperature controls at 85～100 DEG C；
(3) insulation reaction 1～5 hours again after adding, be subsequently added into the water of surplus, after stirring 0.5 hour
Discharging, obtains described color fixing agent.
The preparation method of a kind of color fixing agent for reactive dyeing the most according to claim 5, its
It is characterised by: described imidazoles villaumite is 1-pi-allyl-3-Methylimidazole. villaumite, 1-pi-allyl-3-ethyl imidazol(e)
In villaumite, 1-pi-allyl-3-hexyl imidazolium villaumite, 1-pi-allyl-3-octylimidazole villaumite any one or
Two or more with any mixture than mixing.
The preparation method of a kind of color fixing agent for reactive dyeing the most according to claim 5, its
Be characterised by: described acid regulator be in citric acid, tartaric acid, acetic acid any one or two or more
With any mixture than mixing.
The preparation method of a kind of color fixing agent for reactive dyeing the most according to claim 5, its
It is characterised by: described initiator is any one or two kinds in Ammonium persulfate., sodium peroxydisulfate or potassium peroxydisulfate
Above with any mixture than mixing.
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| 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 |
| CN201711480067.XA CN108049223B (en) | 2016-05-20 | 2016-05-20 | Color fixing agent for reactive dye dyeing and preparation method thereof |
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| CN201711480067.XA Division CN108049223B (en) | 2016-05-20 | 2016-05-20 | Color fixing agent for reactive dye dyeing and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN111287002A (en) * | 2020-03-26 | 2020-06-16 | 刘俊文 | Formaldehyde-free chlorine-resistant color fixing agent and preparation method thereof |
| CN112574355A (en) * | 2020-11-16 | 2021-03-30 | 临清三和纺织集团有限公司 | Active dye acid-proof agent and preparation method thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108179642B (en) * | 2016-05-20 | 2020-11-13 | 南通市武鑫化工有限公司 | Preparation method of color fixing agent for reactive dye dyeing |
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| CN111287002A (en) * | 2020-03-26 | 2020-06-16 | 刘俊文 | Formaldehyde-free chlorine-resistant color fixing agent and preparation method thereof |
| CN112574355A (en) * | 2020-11-16 | 2021-03-30 | 临清三和纺织集团有限公司 | Active dye acid-proof agent and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108049223A (en) | 2018-05-18 |
| CN105951483B (en) | 2018-01-12 |
| CN108049223B (en) | 2020-01-10 |
| CN108179642B (en) | 2020-11-13 |
| CN108179642A (en) | 2018-06-19 |
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Effective date of registration: 20190731 Address after: 332000 No. 33 Zheji Road, Jinshawan Industrial Park, Hukou County, Jiujiang City, Jiangxi Province Patentee after: Jiujiang Zhongjia Industrial Co.,Ltd. Address before: 362700 Baochang Garden No. 6 905, No. 229 Huixing Road, Shishi City, Quanzhou City, Fujian Province Patentee before: Liu Jianfeng |
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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 |