CN106147292A - A kind of high molecular reactive dye and preparation method thereof - Google Patents
A kind of high molecular reactive dye and preparation method thereof Download PDFInfo
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- CN106147292A CN106147292A CN201610507115.9A CN201610507115A CN106147292A CN 106147292 A CN106147292 A CN 106147292A CN 201610507115 A CN201610507115 A CN 201610507115A CN 106147292 A CN106147292 A CN 106147292A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B69/00—Dyes not provided for by a single group of this subclass
- C09B69/10—Polymeric dyes; Reaction products of dyes with monomers or with macromolecular compounds
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Abstract
The invention provides a kind of high molecular reactive dye and preparation method thereof.It is made up of following steps: (1) is by para-ester, lauroylamidopropyl betaine, sodium carbonate and deionized water mix and blend；(2) sodium nitrite and sodium alginate stirring are added；(3) put in ice-water bath, dropping hydrochloric acid and the mixture of deionized water, drip and complete follow-up continuous react to obtain mixture A；(4) by polyurethane, zinc ricinate and N, N dimethylformamide mix and blend；(5) it is placed in ice-water bath, dropping mixture A stirring；(6) 2,2 dihydromethyl propionic acids, sodium citrate, dehydroactic acid sodium and ascorbyl palmitate stirring are added；(7) it is placed in ice-water bath standing, adds sodium chloride stirring, filter to obtain precipitate；(8) it is drying to obtain.The high molecular reactive dye of the present invention, apparent shade depth value K/S is higher, and colour fixation is good, and dry friction and wet friction color fastness the highest grade, and washing simultaneously is basically unchanged color, not staining.
Description
Technical field
The present invention relates to textile material field, be specifically related to a kind of high molecular reactive dye and preparation method thereof.
Background technology
General dyestuff is to be fixed on by ionic bond, hydrogen bond or hydrophobic interaction etc. to be contaminated on material, but it combines
Power is strong, is placing, is washing and in dry cleaning processes, homogeneously dispersed state migrate to material surface, is constantly decolouring and variable color, very
Human body can penetrated into after human body Long contact time to some.Owing to many dyestuffs have potential carcinogenecity and at present
The canceration of most of organic dyestuff need to prove further, and therefore, people have to the novel dyestuff of research and development.
And high molecular reactive dye is to be combined with fiber by covalent bond, the wet colour fastness inherently solving coloured fibre is asked
Topic, but it can cause the loss of dyestuff due to the hydrolysis of active group during storing and using, and this is not only a kind of waste, and
And environment be also result in serious pollution.Therefore, exploitation color fastness is high, solid color is good, solvent resistant, heat-resisting and non-toxic and safe
High molecular reactive dye has important being worth and wide market.
Summary of the invention
Solve the technical problem that: it is an object of the invention to provide a kind of high molecular reactive dye, apparent shade depth value K/S is relatively
Height, colour fixation is good, and dry friction and wet friction color fastness the highest grade, washes simultaneously and is basically unchanged color, and not staining is water-fastness
Color fastness is high.
Technical scheme: a kind of high molecular reactive dye, is prepared from weight portion by following component: para-ester 30-50 part,
2,2-dihydromethyl propionic acid 5-10 part, zinc ricinate 0.5-1 part, polyurethane 10-30 part, lauroylamidopropyl betaine 1-2
Part, sodium carbonate 2-5 part, sodium nitrite 3-6 part, sodium chloride 2-5 part, sodium alginate 0.2-0.5 part, sodium citrate 0.1-0.3 part,
Dehydroactic acid sodium 0.1-0.2 part, ascorbyl palmitate 0.2-0.5 part, N,N-dimethylformamide 15-30 part, hydrochloric acid 5-
10 parts, deionized water 70-100 part.
It is further preferred that described a kind of high molecular reactive dye, following component it is prepared from weight portion: para-position
Ester 35-45 part, 2,2-dihydromethyl propionic acid 6-9 part, zinc ricinate 0.6-0.9 part, polyurethane 15-25 part, lauramide third
Base glycine betaine 1.2-1.8 part, sodium carbonate 3-4 part, sodium nitrite 4-5 part, sodium chloride 3-4 part, sodium alginate 0.3-0.4 part, lemon
Lemon acid sodium 0.15-0.25 part, dehydroactic acid sodium 0.11-0.16 part, ascorbyl palmitate 0.3-0.4 part, N, N-dimethyl
Methanamide 20-25 part, hydrochloric acid 6-9 part, deionized water 80-90 part.
The preparation method of above-mentioned high molecular reactive dye comprises the following steps:
(1) by para-ester, lauroylamidopropyl betaine, sodium carbonate and 50-70 part deionized water mix and blend 20-40 minute；
(2) add sodium nitrite and sodium alginate, stir 10-30 minute under rotating speed 300-500r/min；
(3) put in ice-water bath, be slowly added into hydrochloric acid and the mixture of residue deionized water, after dropping, continue insulation anti-
Answer 30-40 minute to obtain mixture A；
(4) by polyurethane, zinc ricinate and N,N-dimethylformamide mix and blend 10-20 minute；
(5) it is placed in ice-water bath, is slowly added dropwise mixture A, stir 30-50 minute；
(6) addition 2,2-dihydromethyl propionic acid, sodium citrate, dehydroactic acid sodium and ascorbyl palmitate, stir 20-40
Minute；
(7) it is placed in ice-water bath standing 12-14 hour, adds sodium chloride and stir 30-50 minute, filter to obtain precipitate；
(8) put into and vacuum drying oven is dried 24-26 hour at temperature 70-80 DEG C and get final product.
It is further preferred that step (2) medium speed is 350-450r/min, mixing time is 15-25 minute.
It is further preferred that mixing time is 35-45 minute in step (5).
It is further preferred that time of repose is 12.5-13.5 hour in step (7).
It is further preferred that temperature is 75 DEG C in step (8), drying time is 25 hours.
Beneficial effect: apparent shade depth value K/S of the high molecular reactive dye of the present invention is higher, and colour fixation is good, does simultaneously
Friction and wet friction color fastness the highest grade, the highest is all up 5 grades, it addition, washing is basically unchanged color, and not staining, water-fast
Wash color fastness and be also all up 5 grades.
Detailed description of the invention
Embodiment 1
A kind of high molecular reactive dye, is prepared from weight portion by following component: para-ester 30 parts, 2,2-dihydromethyl propionic acid
5 parts, zinc ricinate 0.5 part, polyurethane 10 parts, lauroylamidopropyl betaine 1 part, sodium carbonate 2 parts, sodium nitrite 3 parts, chlorine
Change 2 parts of sodium, sodium alginate 0.2 part, sodium citrate 0.1 part, 0.1 part of dehydroactic acid sodium, ascorbyl palmitate 0.2 part, N,
Dinethylformamide 15 parts, hydrochloric acid 5 parts, deionized water 70 parts.
The preparation method of above-mentioned high molecular reactive dye is:
(1) by para-ester, lauroylamidopropyl betaine, sodium carbonate and 50 parts of deionized water mix and blends 20 minutes；
(2) add sodium nitrite and sodium alginate, stir 10 minutes under rotating speed 300r/min；
(3) put in ice-water bath, be slowly added into hydrochloric acid and the mixture of residue deionized water, after dropping, continue insulation anti-
Answer 30 minutes to obtain mixture A；
(4) by polyurethane, zinc ricinate and N,N-dimethylformamide mix and blend 10 minutes；
(5) it is placed in ice-water bath, is slowly added dropwise mixture A, stir 30 minutes；
(6) addition 2,2-dihydromethyl propionic acid, sodium citrate, dehydroactic acid sodium and ascorbyl palmitate, stir 20 points
Clock；
(7) it is placed in ice-water bath standing 12 hours, adds sodium chloride and stir 30 minutes, filter to obtain precipitate；
(8) put into and vacuum drying oven is dried 24 hours under temperature 70 C and get final product.
Embodiment 2
A kind of high molecular reactive dye, is prepared from weight portion by following component: para-ester 40 parts, 2,2-dihydromethyl propionic acid
7.5 parts, zinc ricinate 0.75 part, polyurethane 20 parts, lauroylamidopropyl betaine 1.5 parts, sodium carbonate 3.5 parts, nitrous acid
4.5 parts of sodium, 3.5 parts of sodium chloride, sodium alginate 0.35 part, sodium citrate 0.2 part, 0.15 part of dehydroactic acid sodium, ascorbic acid palm fibre
Palmitic acid acid esters 0.35 part, N,N-dimethylformamide 22.5 parts, hydrochloric acid 7. part 5, deionized water 85 parts.
The preparation method of above-mentioned high molecular reactive dye is:
(1) by para-ester, lauroylamidopropyl betaine, sodium carbonate and 60 parts of deionized water mix and blends 30 minutes；
(2) add sodium nitrite and sodium alginate, stir 20 minutes under rotating speed 350r/min；
(3) put in ice-water bath, be slowly added into hydrochloric acid and the mixture of residue deionized water, after dropping, continue insulation anti-
Answer 35 minutes to obtain mixture A；
(4) by polyurethane, zinc ricinate and N,N-dimethylformamide mix and blend 15 minutes；
(5) it is placed in ice-water bath, is slowly added dropwise mixture A, stir 40 minutes；
(6) addition 2,2-dihydromethyl propionic acid, sodium citrate, dehydroactic acid sodium and ascorbyl palmitate, stir 30 points
Clock；
(7) it is placed in ice-water bath standing 13 hours, adds sodium chloride and stir 40 minutes, filter to obtain precipitate；
(8) put into and vacuum drying oven is dried 25 hours at temperature 75 DEG C and get final product.
Embodiment 3
A kind of high molecular reactive dye, is prepared from weight portion by following component: para-ester 50 parts, 2,2-dihydromethyl propionic acid
10 parts, zinc ricinate 1 part, polyurethane 30 parts, lauroylamidopropyl betaine 2 parts, sodium carbonate 5 parts, sodium nitrite 6 parts, chlorine
Change 5 parts of sodium, sodium alginate 0.5 part, sodium citrate 0.3 part, 0.2 part of dehydroactic acid sodium, ascorbyl palmitate 0.5 part, N,
Dinethylformamide 30 parts, hydrochloric acid 10 parts, deionized water 100 parts.
The preparation method of above-mentioned high molecular reactive dye is:
(1) by para-ester, lauroylamidopropyl betaine, sodium carbonate and 70 parts of deionized water mix and blends 40 minutes；
(2) add sodium nitrite and sodium alginate, stir 30 minutes under rotating speed 400r/min；
(3) put in ice-water bath, be slowly added into hydrochloric acid and the mixture of residue deionized water, after dropping, continue insulation anti-
Answer 40 minutes to obtain mixture A；
(4) by polyurethane, zinc ricinate and N,N-dimethylformamide mix and blend 20 minutes；
(5) it is placed in ice-water bath, is slowly added dropwise mixture A, stir 50 minutes；
(6) addition 2,2-dihydromethyl propionic acid, sodium citrate, dehydroactic acid sodium and ascorbyl palmitate, stir 40 points
Clock；
(7) it is placed in ice-water bath standing 14 hours, adds sodium chloride and stir 50 minutes, filter to obtain precipitate；
(8) put into and vacuum drying oven is dried 26 hours at temperature 80 DEG C and get final product.
Embodiment 4
A kind of high molecular reactive dye, is prepared from weight portion by following component: para-ester 35 parts, 2,2-dihydromethyl propionic acid
6 parts, zinc ricinate 0.6 part, polyurethane 15 parts, lauroylamidopropyl betaine 1.2 parts, sodium carbonate 3 parts, sodium nitrite 4 parts,
3 parts of sodium chloride, sodium alginate 0.3 part, sodium citrate 0.15 part, 0.11 part of dehydroactic acid sodium, ascorbyl palmitate 0.3
Part, N,N-dimethylformamide 20 parts, hydrochloric acid 6 parts, deionized water 80 parts.
The preparation method of above-mentioned high molecular reactive dye is:
(1) by para-ester, lauroylamidopropyl betaine, sodium carbonate and 55 parts of deionized water mix and blends 25 minutes；
(2) add sodium nitrite and sodium alginate, stir 15 minutes under rotating speed 450r/min；
(3) put in ice-water bath, be slowly added into hydrochloric acid and the mixture of residue deionized water, after dropping, continue insulation anti-
Answer 35 minutes to obtain mixture A；
(4) by polyurethane, zinc ricinate and N,N-dimethylformamide mix and blend 15 minutes；
(5) it is placed in ice-water bath, is slowly added dropwise mixture A, stir 35 minutes；
(6) addition 2,2-dihydromethyl propionic acid, sodium citrate, dehydroactic acid sodium and ascorbyl palmitate, stir 25 points
Clock；
(7) it is placed in ice-water bath standing 12.5 hours, adds sodium chloride and stir 35 minutes, filter to obtain precipitate；
(8) put into and vacuum drying oven is dried 25 hours at temperature 75 DEG C and get final product.
Embodiment 5
A kind of high molecular reactive dye, is prepared from weight portion by following component: para-ester 45 parts, 2,2-dihydromethyl propionic acid
9 parts, zinc ricinate 0.9 part, polyurethane 25 parts, lauroylamidopropyl betaine 1.8 parts, sodium carbonate 4 parts, sodium nitrite 5 parts,
4 parts of sodium chloride, sodium alginate 0.4 part, sodium citrate 0.25 part, 0.16 part of dehydroactic acid sodium, ascorbyl palmitate 0.4
Part, N,N-dimethylformamide 25 parts, hydrochloric acid 9 parts, deionized water 90 parts.
The preparation method of above-mentioned high molecular reactive dye is:
(1) by para-ester, lauroylamidopropyl betaine, sodium carbonate and 65 parts of deionized water mix and blends 35 minutes；
(2) add sodium nitrite and sodium alginate, stir 25 minutes under rotating speed 500r/min；
(3) put in ice-water bath, be slowly added into hydrochloric acid and the mixture of residue deionized water, after dropping, continue insulation anti-
Answer 35 minutes to obtain mixture A；
(4) by polyurethane, zinc ricinate and N,N-dimethylformamide mix and blend 15 minutes；
(5) it is placed in ice-water bath, is slowly added dropwise mixture A, stir 45 minutes；
(6) addition 2,2-dihydromethyl propionic acid, sodium citrate, dehydroactic acid sodium and ascorbyl palmitate, stir 35 points
Clock；
(7) it is placed in ice-water bath standing 13.5 hours, adds sodium chloride and stir 45 minutes, filter to obtain precipitate；
(8) put into and vacuum drying oven is dried 25 hours at temperature 75 DEG C and get final product.
Comparative example 1
The present embodiment is not contain zinc ricinate with the difference of embodiment 5.Specifically:
A kind of high molecular reactive dye, is prepared from weight portion by following component: para-ester 45 parts, 2,2-dihydromethyl propionic acid
9 parts, polyurethane 25 parts, lauroylamidopropyl betaine 1.8 parts, sodium carbonate 4 parts, sodium nitrite 5 parts, 4 parts of sodium chloride, alginic acid
0.4 part of sodium, sodium citrate 0.25 part, 0.16 part of dehydroactic acid sodium, ascorbyl palmitate 0.4 part, N, N-dimethyl formyl
Amine 25 parts, hydrochloric acid 9 parts, deionized water 90 parts.
The preparation method of above-mentioned high molecular reactive dye is:
(1) by para-ester, lauroylamidopropyl betaine, sodium carbonate and 65 parts of deionized water mix and blends 35 minutes；
(2) add sodium nitrite and sodium alginate, stir 25 minutes under rotating speed 500r/min；
(3) put in ice-water bath, be slowly added into hydrochloric acid and the mixture of residue deionized water, after dropping, continue insulation anti-
Answer 35 minutes to obtain mixture A；
(4) by polyurethane and N,N-dimethylformamide mix and blend 15 minutes；
(5) it is placed in ice-water bath, is slowly added dropwise mixture A, stir 45 minutes；
(6) addition 2,2-dihydromethyl propionic acid, sodium citrate, dehydroactic acid sodium and ascorbyl palmitate, stir 35 points
Clock；
(7) it is placed in ice-water bath standing 13.5 hours, adds sodium chloride and stir 45 minutes, filter to obtain precipitate；
(8) put into and vacuum drying oven is dried 25 hours at temperature 75 DEG C and get final product.
Comparative example 2
The present embodiment is not contain sodium alginate and sodium citrate with the difference of embodiment 5.Specifically:
A kind of high molecular reactive dye, is prepared from weight portion by following component: para-ester 45 parts, 2,2-dihydromethyl propionic acid
9 parts, zinc ricinate 0.9 part, polyurethane 25 parts, lauroylamidopropyl betaine 1.8 parts, sodium carbonate 4 parts, sodium nitrite 5 parts,
4 parts of sodium chloride, 0.16 part of dehydroactic acid sodium, ascorbyl palmitate 0.4 part, N,N-dimethylformamide 25 parts, hydrochloric acid 9
Part, deionized water 90 parts.
The preparation method of above-mentioned high molecular reactive dye is:
(1) by para-ester, lauroylamidopropyl betaine, sodium carbonate and 65 parts of deionized water mix and blends 35 minutes；
(2) add sodium nitrite, stir 25 minutes under rotating speed 500r/min；
(3) put in ice-water bath, be slowly added into hydrochloric acid and the mixture of residue deionized water, after dropping, continue insulation anti-
Answer 35 minutes to obtain mixture A；
(4) by polyurethane, zinc ricinate and N,N-dimethylformamide mix and blend 15 minutes；
(5) it is placed in ice-water bath, is slowly added dropwise mixture A, stir 45 minutes；
(6) addition 2,2-dihydromethyl propionic acid, dehydroactic acid sodium and ascorbyl palmitate, stir 35 minutes；
(7) it is placed in ice-water bath standing 13.5 hours, adds sodium chloride and stir 45 minutes, filter to obtain precipitate；
(8) put into and vacuum drying oven is dried 25 hours at temperature 75 DEG C and get final product.
The embodiment of material of the present invention and the partial properties index of comparative example see table, it will be seen that material of the present invention
Apparent shade depth value K/S of material is higher, and colour fixation is good, and dry friction simultaneously and wet friction color fastness the highest grade, Gao Douke
Reaching 5 grades, it addition, washing is basically unchanged color, not staining, water-fastness color fastness is also all up 5 grades.
The partial properties index of table 1 high molecular reactive dye
Claims (7)
1. a high molecular reactive dye, it is characterised in that: it is prepared from weight portion by following component: para-ester 30-50 part,
2,2-dihydromethyl propionic acid 5-10 part, zinc ricinate 0.5-1 part, polyurethane 10-30 part, lauroylamidopropyl betaine 1-2
Part, sodium carbonate 2-5 part, sodium nitrite 3-6 part, sodium chloride 2-5 part, sodium alginate 0.2-0.5 part, sodium citrate 0.1-0.3 part,
Dehydroactic acid sodium 0.1-0.2 part, ascorbyl palmitate 0.2-0.5 part, N,N-dimethylformamide 15-30 part, hydrochloric acid 5-
10 parts, deionized water 70-100 part.
A kind of high molecular reactive dye the most according to claim 1, it is characterised in that: prepared with weight portion by following component
Form: para-ester 35-45 part, 2,2-dihydromethyl propionic acid 6-9 part, zinc ricinate 0.6-0.9 part, polyurethane 15-25 part, the moon
Osmanthus amido propyl betaine 1.2-1.8 part, sodium carbonate 3-4 part, sodium nitrite 4-5 part, sodium chloride 3-4 part, sodium alginate 0.3-
0.4 part, sodium citrate 0.15-0.25 part, dehydroactic acid sodium 0.11-0.16 part, ascorbyl palmitate 0.3-0.4 part, N,
Dinethylformamide 20-25 part, hydrochloric acid 6-9 part, deionized water 80-90 part.
3. the preparation method of a kind of high molecular reactive dye described in any one of claim 1 to 2, it is characterised in that: include with
Lower step:
(1) by para-ester, lauroylamidopropyl betaine, sodium carbonate and 50-70 part deionized water mix and blend 20-40 minute；
(2) add sodium nitrite and sodium alginate, stir 10-30 minute under rotating speed 300-500r/min；
(3) put in ice-water bath, be slowly added into hydrochloric acid and the mixture of residue deionized water, after dropping, continue insulation anti-
Answer 30-40 minute to obtain mixture A；
(4) by polyurethane, zinc ricinate and N,N-dimethylformamide mix and blend 10-20 minute；
(5) it is placed in ice-water bath, is slowly added dropwise mixture A, stir 30-50 minute；
(6) addition 2,2-dihydromethyl propionic acid, sodium citrate, dehydroactic acid sodium and ascorbyl palmitate, stir 20-40
Minute；
(7) it is placed in ice-water bath standing 12-14 hour, adds sodium chloride and stir 30-50 minute, filter to obtain precipitate；
(8) put into and vacuum drying oven is dried 24-26 hour at temperature 70-80 DEG C and get final product.
The preparation method of a kind of high molecular reactive dye the most according to claim 3, it is characterised in that: described step (2)
Medium speed is 350-450r/min, and mixing time is 15-25 minute.
The preparation method of a kind of high molecular reactive dye the most according to claim 3, it is characterised in that: described step (5)
Middle mixing time is 35-45 minute.
The preparation method of a kind of high molecular reactive dye the most according to claim 3, it is characterised in that: described step (7)
Middle time of repose is 12.5-13.5 hour.
The preparation method of a kind of high molecular reactive dye the most according to claim 3, it is characterised in that: described step (8)
Middle temperature is 75 DEG C, and drying time is 25 hours.
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| CN201610507115.9A CN106147292A (en) | 2016-07-01 | 2016-07-01 | A kind of high molecular reactive dye and preparation method thereof |
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| CN201610507115.9A CN106147292A (en) | 2016-07-01 | 2016-07-01 | A kind of high molecular reactive dye and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
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| CN106147292A true CN106147292A (en) | 2016-11-23 |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101768373A (en) * | 2010-01-08 | 2010-07-07 | 武汉科技学院 | Method for preparing water soluble vinyl-sulfone polyurethane class high molecular reactive dye with diazo coupling method |
-
2016
- 2016-07-01 CN CN201610507115.9A patent/CN106147292A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101768373A (en) * | 2010-01-08 | 2010-07-07 | 武汉科技学院 | Method for preparing water soluble vinyl-sulfone polyurethane class high molecular reactive dye with diazo coupling method |
Non-Patent Citations (3)
| Title |
|---|
| 无: "（二）高分子材料的防老化", 《老化通讯》 * |
| 赵小平 等: "2,2-二羟甲基丙酸(DMPA)性能、用途及合成工艺", 《精细与专用化学品》 * |
| 金雪: "水溶性聚氨酯基高分子染料制备及其对纤维素染色探讨", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
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Application publication date: 20161123 |