CN106221278A - A kind of preparation method of reducing dye Vat Yellow 1 - Google Patents
A kind of preparation method of reducing dye Vat Yellow 1 Download PDFInfo
- Publication number
- CN106221278A CN106221278A CN201610595666.5A CN201610595666A CN106221278A CN 106221278 A CN106221278 A CN 106221278A CN 201610595666 A CN201610595666 A CN 201610595666A CN 106221278 A CN106221278 A CN 106221278A
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- CN
- China
- Prior art keywords
- vat yellow
- preparation
- rotating speed
- crude product
- reducing dye
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Classifications
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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
- C09B5/00—Dyes with an anthracene nucleus condensed with one or more heterocyclic rings with or without carbocyclic rings
- C09B5/02—Dyes with an anthracene nucleus condensed with one or more heterocyclic rings with or without carbocyclic rings the heterocyclic ring being only condensed in peri position
- C09B5/20—Flavanthrones
- C09B5/22—Preparation from starting materials already containing the flavanthrone nucleus
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0071—Process features in the making of dyestuff preparations; Dehydrating agents; Dispersing agents; Dustfree compositions
- C09B67/0077—Preparations with possibly reduced vat, sulfur or indigo dyes
Abstract
The invention discloses the preparation method of a kind of reducing dye Vat Yellow 1, including grinding, kneading, extraction step.By pre-grinding and nibbling shear effect, the Vat Yellow 1 of preparation has good vividness and tinting strength, tinting power, and the quality of product significantly improves, thus enhances its use value.
Description
Technical field
The present invention relates to reducing dye technical field, be specifically related to the preparation method of a kind of reducing dye Vat Yellow 1.
Background technology
Reducing dye is that in dyestuff, properties all compares excellent dyestuff, and it is water insoluble, the company of borrowing in alkaline solution
Sodium sulfite (sodium hydrosulfite) carries out reduction treatment, and makes stock-dye.The kind of reducing dye is numerous, chromatograph is relatively complete, color and luster
Bright-coloured, dyefastness good, has preferable fastness to washing and light fastness, it is possible to be widely used in cotton, hair, silk, fiber crops, synthesis fine
Dimension and blend fabric, the printing and dyeing of intertexture.Vat Yellow 1 is again reduction G, is a kind of orange or golden yellow powder, is dissolved in hot nitre
Base benzene, water insoluble, acetone, ethanol, toluene or chloroform, there is high transparency and fast light, fastness to weathering, be mainly used in
Cotton, tie up and tie up/cotton, the dyeing of polyester cotton and stamp thereof, good to cotton fiber affinity, good level-dyeing property；Also can be with aluminum metal pigment
Blending, for metal automobile coating (OEM), repairs paint and coloring plastic；It is also applied for polyacrylonitrile fibre dope dyeing, timber
And artistic coating coloring.But, the tinctorial yield of presently commercially available Vat Yellow 1 is the highest, and application performance is general, so that its application is subject to
To certain restriction.
Summary of the invention
For the deficiencies in the prior art, the invention provides the preparation side of the high reducing dye Vat Yellow 1 of a kind of tinctorial yield
Method.
For realizing object above, the present invention is achieved by the following technical programs:
The preparation method of reducing dye Vat Yellow 1, comprises the following steps:
1) grind: crude product Vat Yellow 1 is joined in dismembyator, is added thereto to appropriate carboxymethyl chitosan, grind
It is 2-3 μm to granularity, obtains grinding material；
2) mediating: joined by grinding material in kneader, be added thereto to sodium chloride micro-powder, stirring mixes, then to it
Middle addition hexamethyl phosphoramide, stirring mixing, 40 DEG C, rotating speed be under 30rpm kneading 0.5h, with the heating rate of 2 DEG C/min
Be warming up to 70 DEG C, adjust rotating speed be under 35rpm kneading 1.5h, with the heating rate of 1 DEG C/min be warming up to 90 DEG C, maintain rotating speed not
Become and mediate 1.5h, maintain temperature-resistant adjustment rotating speed to mediate 1h to 40rpm, obtain kneaded mixture material；
3) extract: in kneaded mixture material, add deionized water, sucking filtration, wash 4-5 time extremely the most salt-free, microwave drying, powder
Broken, sieve, to obtain final product.
Preferably, the addition of described carboxymethyl chitosan is the 0.3-0.5% of crude product Vat Yellow 1 quality.
Preferably, described sodium chloride micro-powder is 3-4:1 with the mass ratio of crude product Vat Yellow 1.
Preferably, described hexamethyl phosphoramide is 9-11:10 with the mass ratio of crude product Vat Yellow 1.
Preferably, described step 3) middle 300 mesh sieves excessively.
The method have the benefit that the present invention is by carrying out pre-grinding, then and chlorine by crude product Vat Yellow 1 and carboxymethyl chitosan
Change sodium to mediate in kneader, improve grinding efficiency, and segmentation is mediated under different temperatures and rotating speed so that material is not
Carry out broken refinement with shearing force, change the configuration of surface of particle, energy-conservation, improve the purity of dyestuff, make dyestuff have bright-coloured
The tinting strength, tinting power become reconciled of color and luster, additionally, its transparency and excellent dispersion, significantly improve the quality of product, thus enhance
Its use value.
Detailed description of the invention
For making the purpose of the embodiment of the present invention, technical scheme and advantage clearer, below in conjunction with the embodiment of the present invention,
Technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is the present invention one
Divide embodiment rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not making
The every other embodiment obtained under creative work premise, broadly falls into the scope of protection of the invention.
Embodiment 1:
The preparation method of reducing dye Vat Yellow 1, comprises the following steps:
1) grind: crude product Vat Yellow 1 is joined in dismembyator, is added thereto to the carboxylic of crude product Vat Yellow 1 quality 0.4%
Methyl chitosan, being ground to granularity is 2 μm, obtains grinding material；
2) mediate: grinding material is joined in kneader, be added thereto to the chlorination of 3.5 times of crude product Vat Yellow 1 quality
Sodium micropowder, stirring mixing, then be added thereto to and the hexamethyl phosphoramide of the quality such as crude product Vat Yellow 1, stirring mixing, 40
DEG C, rotating speed be under 30rpm kneading 0.5h, with the heating rate of 2 DEG C/min be warming up to 70 DEG C, adjust rotating speed as 35rpm under mediate
1.5h, is warming up to 90 DEG C with the heating rate of 1 DEG C/min, maintains rotating speed constant kneading 1.5h, maintain temperature-resistant adjustment rotating speed
Mediate 1h to 40rpm, obtain kneaded mixture material；
3) extract: in kneaded mixture material, add deionized water, sucking filtration, wash 5 times to the most salt-free, microwave drying, pulverizing,
Cross 300 sieves, to obtain final product.
Embodiment 2:
The preparation method of reducing dye Vat Yellow 1, comprises the following steps:
1) grind: crude product Vat Yellow 1 is joined in dismembyator, is added thereto to the carboxylic of crude product Vat Yellow 1 quality 0.3%
Methyl chitosan, being ground to granularity is 2 μm, obtains grinding material；
2) mediate: grinding material is joined in kneader, be added thereto to the sodium chloride of 3 times of crude product Vat Yellow 1 quality
Micropowder, stirring mixing, then be added thereto to the hexamethyl phosphoramide of 0.9 times of crude product Vat Yellow 1 quality, stirring mixing, 40 DEG C,
Rotating speed be under 30rpm kneading 0.5h, with the heating rate of 2 DEG C/min be warming up to 70 DEG C, adjust rotating speed as 35rpm under mediate
1.5h, is warming up to 90 DEG C with the heating rate of 1 DEG C/min, maintains rotating speed constant kneading 1.5h, maintain temperature-resistant adjustment rotating speed
Mediate 1h to 40rpm, obtain kneaded mixture material；
3) extract: in kneaded mixture material, add deionized water, sucking filtration, wash 4 times to the most salt-free, microwave drying, pulverizing,
Cross 300 sieves, to obtain final product.
Embodiment 3:
The preparation method of reducing dye Vat Yellow 1, comprises the following steps:
1) grind: crude product Vat Yellow 1 is joined in dismembyator, is added thereto to the carboxylic of crude product Vat Yellow 1 quality 0.5%
Methyl chitosan, being ground to granularity is 3 μm, obtains grinding material；
2) mediate: grinding material is joined in kneader, be added thereto to the sodium chloride of 4 times of crude product Vat Yellow 1 quality
Micropowder, stirring mixing, then be added thereto to the hexamethyl phosphoramide of 1.1 times of crude product Vat Yellow 1 quality, stirring mixing, 40 DEG C,
Rotating speed be under 30rpm kneading 0.5h, with the heating rate of 2 DEG C/min be warming up to 70 DEG C, adjust rotating speed as 35rpm under mediate
1.5h, is warming up to 90 DEG C with the heating rate of 1 DEG C/min, maintains rotating speed constant kneading 1.5h, maintain temperature-resistant adjustment rotating speed
Mediate 1h to 40rpm, obtain kneaded mixture material；
3) extract: in kneaded mixture material, add deionized water, sucking filtration, wash 5 times to the most salt-free, microwave drying, pulverizing,
Cross 300 sieves, to obtain final product.
Embodiment 4:
The preparation method of reducing dye Vat Yellow 1, comprises the following steps:
1) grind: crude product Vat Yellow 1 is joined in dismembyator, is added thereto to the carboxylic of crude product Vat Yellow 1 quality 0.5%
Methyl chitosan, being ground to granularity is 2 μm, obtains grinding material；
2) mediate: grinding material is joined in kneader, be added thereto to the sodium chloride of 3 times of crude product Vat Yellow 1 quality
Micropowder, stirring mixing, then be added thereto to the hexamethyl phosphoramide of 0.9 times of crude product Vat Yellow 1 quality, stirring mixing, 40 DEG C,
Rotating speed be under 30rpm kneading 0.5h, with the heating rate of 2 DEG C/min be warming up to 70 DEG C, adjust rotating speed as 35rpm under mediate
1.5h, it is warming up to 90 DEG C with the heating rate of 1 DEG C/min, maintains rotating speed constant kneading 1.5h, maintain temperature-resistant adjustment rotating speed
Mediate 1h to 40rpm, obtain kneaded mixture material；
3) extract: in kneaded mixture material, add deionized water, sucking filtration, wash 5 times to the most salt-free, microwave drying, pulverizing,
Cross 300 sieves, to obtain final product.
Above example only in order to technical scheme to be described, is not intended to limit；Although with reference to previous embodiment
The present invention is described in detail, it will be understood by those within the art that: it still can be to aforementioned each enforcement
Technical scheme described in example is modified, or wherein portion of techniques feature is carried out equivalent；And these amendment or
Replace, do not make the essence of appropriate technical solution depart from the spirit and scope of various embodiments of the present invention technical scheme.
Claims (5)
1. the preparation method of a reducing dye Vat Yellow 1, it is characterised in that comprise the following steps:
1) grind: crude product Vat Yellow 1 is joined in dismembyator, is added thereto to appropriate carboxymethyl chitosan, is ground to grain
Degree is 2-3 μm, obtains grinding material；
2) mediate: grinding material is joined in kneader, be added thereto to sodium chloride micro-powder, stirring mixing, then add wherein
Enter hexamethyl phosphoramide, stirring mixing, 40 DEG C, rotating speed be kneading 0.5h under 30rpm, heat up with the heating rate of 2 DEG C/min
To 70 DEG C, to adjust rotating speed be kneading 1.5h under 35rpm, be warming up to 90 DEG C with the heating rate of 1 DEG C/min, maintain that rotating speed is constant pinches
Close 1.5h, maintain temperature-resistant adjustment rotating speed to mediate 1h to 40rpm, obtain kneaded mixture material；
3) extract: in kneaded mixture material, add deionized water, sucking filtration, wash 4-5 time extremely the most salt-free, microwave drying, pulverizing, mistake
Sieve, to obtain final product.
2. the preparation method of reducing dye Vat Yellow 1 as claimed in claim 1, it is characterised in that described carboxymethyl chitosan
The 0.3-0.5% that addition is crude product Vat Yellow 1 quality.
3. the preparation method of reducing dye Vat Yellow 1 as claimed in claim 1, it is characterised in that described sodium chloride micro-powder with
The mass ratio of crude product Vat Yellow 1 is 3-4:1.
4. the preparation method of reducing dye Vat Yellow 1 as claimed in claim 1, it is characterised in that described hexamethyl phosphoramide
It is 9-11:10 with the mass ratio of crude product Vat Yellow 1.
5. the preparation method of reducing dye Vat Yellow 1 as claimed in claim 1, it is characterised in that described step 3) middle excessively 300
Mesh sieve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610595666.5A CN106221278B (en) | 2016-07-26 | 2016-07-26 | A kind of preparation method of reducing dye Vat Yellow 1 |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610595666.5A CN106221278B (en) | 2016-07-26 | 2016-07-26 | A kind of preparation method of reducing dye Vat Yellow 1 |
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| CN106221278A true CN106221278A (en) | 2016-12-14 |
| CN106221278B CN106221278B (en) | 2017-11-10 |
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| CN201610595666.5A Active CN106221278B (en) | 2016-07-26 | 2016-07-26 | A kind of preparation method of reducing dye Vat Yellow 1 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111704808A (en) * | 2020-07-24 | 2020-09-25 | 蓬莱新光颜料化工有限公司 | A pigment Red 57:1 preparation method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1463141A (en) * | 1974-09-26 | 1977-02-02 | Ici Ltd | Process for converting colouring matters to pigmentary form |
| US4298526A (en) * | 1978-11-30 | 1981-11-03 | Basf Aktiengesellschaft | Preparation of easily dispersible and deeply colored pigmentary forms |
| CN1918244A (en) * | 2003-12-31 | 2007-02-21 | 太阳化学公司 | Preparation of yellow pigment |
| CN101457027A (en) * | 2007-12-14 | 2009-06-17 | 上海捷虹颜料化工集团股份有限公司 | High-grade glow blue pigment and preparation method thereof |
| CN103483865A (en) * | 2013-09-11 | 2014-01-01 | 吴江市冰心文教用品有限公司 | Preparation method of yellow-green pigment for plastic |
-
2016
- 2016-07-26 CN CN201610595666.5A patent/CN106221278B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1463141A (en) * | 1974-09-26 | 1977-02-02 | Ici Ltd | Process for converting colouring matters to pigmentary form |
| US4298526A (en) * | 1978-11-30 | 1981-11-03 | Basf Aktiengesellschaft | Preparation of easily dispersible and deeply colored pigmentary forms |
| CN1918244A (en) * | 2003-12-31 | 2007-02-21 | 太阳化学公司 | Preparation of yellow pigment |
| CN101457027A (en) * | 2007-12-14 | 2009-06-17 | 上海捷虹颜料化工集团股份有限公司 | High-grade glow blue pigment and preparation method thereof |
| CN103483865A (en) * | 2013-09-11 | 2014-01-01 | 吴江市冰心文教用品有限公司 | Preparation method of yellow-green pigment for plastic |
Non-Patent Citations (1)
| Title |
|---|
| 张天永等: "还原黄G的颜料化工艺进展", 《染料与染色》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111704808A (en) * | 2020-07-24 | 2020-09-25 | 蓬莱新光颜料化工有限公司 | A pigment Red 57:1 preparation method |
| CN111704808B (en) * | 2020-07-24 | 2022-06-17 | 蓬莱新光颜料化工有限公司 | A pigment Red 57:1 preparation method |
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| Publication number | Publication date |
|---|---|
| CN106221278B (en) | 2017-11-10 |
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| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CB03 | Change of inventor or designer information |
Inventor after: Wang Hongwei Inventor after: Gao Hongyu Inventor after: Xu Huixiang Inventor after: Sun Maoyi Inventor after: Guo Yuan Inventor after: Jiang Dawei Inventor after: Xu Lanxiang Inventor before: Wang Hongwei Inventor before: Xu Huixiang Inventor before: Li Zhen Inventor before: Jiang Dawei Inventor before: Gao Hongyu Inventor before: Guo Yuan |
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| CB03 | Change of inventor or designer information | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20171030 Address after: 235200 Anhui province Xiaoxian YONGGU Light Industrial Park Patentee after: Anhui Cage chemical Polytron Technologies Inc Address before: 235200 Anhui city of Suzhou province Xiaoxian YONGGU Light Industrial Park Patentee before: Xiao County Kaiqi Chemical Technology Co., Ltd. |
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| TR01 | Transfer of patent right | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 235200 Xiaoxian Yong Gu Light Chemical Industrial Park, Anhui Patentee after: Anhui rongchuang Chemical Technology Co.,Ltd. Address before: 235200 Xiaoxian Yong Gu Light Chemical Industrial Park, Anhui Patentee before: ANHUI KAIQI CHEMICAL TECHNOLOGY Co.,Ltd. |
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| CP01 | Change in the name or title of a patent holder |