CN106221278B - 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
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- CN106221278B CN106221278B CN201610595666.5A CN201610595666A CN106221278B CN 106221278 B CN106221278 B CN 106221278B CN 201610595666 A CN201610595666 A CN 201610595666A CN 106221278 B CN106221278 B CN 106221278B
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- vat yellow
- preparation
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- crude product
- rotating speed
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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 a kind of preparation method of reducing dye Vat Yellow 1, including grind, mediate, extraction step.Acted on by pre-grinding and nibbling shear, the Vat Yellow 1 of preparation has good vividness and tinting strength, tinting power, and the quality of product significantly improves, so as to enhance its use value.
Description
Technical field
The present invention relates to reducing dye technical field, and in particular to a kind of preparation method of reducing dye Vat Yellow 1.
Background technology
Reducing dye is the dyestuff that properties are all more excellent in dyestuff, and its is not soluble in water, 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, chromatogram is relatively complete, color and luster
It is bright-coloured, dyefastness is good, there is preferable fastness to washing and light fastness, it is fine that cotton, hair, silk, fiber crops, synthesis can be widely used in
Dimension and its blend fabric, the printing and dyeing of intertexture.Vat Yellow 1 is called reduction G, is a kind of orange or golden yellow powder, is dissolved in hot nitre
Base benzene, not soluble in water, acetone, ethanol, toluene or chloroform, there is high transparency and fast light, fastness to weathering, be mainly used in
Cotton, dimension and dimension/cotton, the dyeing of polyester cotton and its stamp, good level-dyeing property good to cotton fiber affinity；Also can be with aluminum metal pigment
Blending, for metal automobile coating (OEM), repair 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 not high, application performance is general so that its application by
To certain limitation.
The content of the invention
In view of the shortcomings of the prior art, the invention provides a kind of preparation side of the high reducing dye Vat Yellow 1 of tinctorial yield
Method.
To realize 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 added in mill, adds appropriate carboxymethyl chitosan thereto, is ground
It is 2-3 μm to granularity, obtains grinding material；
2) mediate：Grinding material is added in kneader, adds sodium chloride micro-powder thereto, is stirred, then to its
Middle addition hexamethyl phosphoramide, is stirred, and 0.5h is mediated under being 30rpm in 40 DEG C, rotating speed, with 2 DEG C/min heating rate
It is to mediate 1.5h under 35rpm to be warming up to 70 DEG C, adjust rotating speed, is warming up to 90 DEG C with 1 DEG C/min heating rate, maintains 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：Deionized water is added into kneaded mixture material, is filtered, 4-5 extremely salt-free, microwave drying of washing, powder
It is broken, sieving, produce.
Preferably, the addition of the carboxymethyl chitosan is the 0.3-0.5% of crude product Vat Yellow 1 quality.
Preferably, the sodium chloride micro-powder and the mass ratio of crude product Vat Yellow 1 are 3-4：1.
Preferably, the mass ratio of the hexamethyl phosphoramide and crude product Vat Yellow 1 is 9-11：10.
Preferably, 300 mesh sieves are crossed in the step 3).
Beneficial effect of the present invention：The present invention by crude product Vat Yellow 1 and carboxymethyl chitosan by carrying out pre-grinding, then and chlorine
Change sodium to be mediated in kneader, improve grinding efficiency, and segmentation is mediated under different temperatures and rotating speed so that material is not
Broken refinement is carried out with shearing force, the configuration of surface of particle is changed, energy-conservation, improves the purity of dyestuff, there is dyestuff bright-coloured
The tinting strength, tinting power become reconciled of color and luster, in addition, its transparency and dispersiveness are excellent, the quality of product is significantly improved, so as to enhance
Its use value.
Embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention 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 the premise of creative work, belongs to 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 added in mill, adds the carboxylic of crude product Vat Yellow 1 quality 0.4% thereto
Methyl chitosan, granularity is ground to as 2 μm, obtains grinding material；
2) mediate：Grinding material is added in kneader, adds the chlorination of 3.5 times of crude product Vat Yellow 1 quality thereto
Sodium micro mist, is stirred, then the hexamethyl phosphoramide of the quality such as addition and crude product Vat Yellow 1 thereto, is stirred, 40
DEG C, rotating speed be 30rpm under mediate 0.5h, using 2 DEG C/min heating rate be warming up to 70 DEG C, adjustment rotating speed as 35rpm under mediate
1.5h, it is warming up to 90 DEG C with 1 DEG C/min heating rate, maintains the constant kneading 1.5h of rotating speed, maintain temperature-resistant adjustment rotating speed
1h is mediated to 40rpm, obtains kneaded mixture material；
3) extract：Deionized water is added into kneaded mixture material, is filtered, 5 extremely salt-free, microwave drying of washing, is crushed,
300 sieves are crossed, are produced.
Embodiment 2：
The preparation method of reducing dye Vat Yellow 1, comprises the following steps：
1) grind：Crude product Vat Yellow 1 is added in mill, adds the carboxylic of crude product Vat Yellow 1 quality 0.3% thereto
Methyl chitosan, granularity is ground to as 2 μm, obtains grinding material；
2) mediate：Grinding material is added in kneader, adds the sodium chloride of 3 times of crude product Vat Yellow 1 quality thereto
Micro mist, be stirred, then thereto add 0.9 times of crude product Vat Yellow 1 quality hexamethyl phosphoramide, be stirred, 40 DEG C,
Rotating speed is to mediate 0.5h under 30rpm, is mediated under being warming up to 70 DEG C using 2 DEG C/min heating rate, adjusted rotating speed as 35rpm
1.5h, it is warming up to 90 DEG C with 1 DEG C/min heating rate, maintains the constant kneading 1.5h of rotating speed, maintain temperature-resistant adjustment rotating speed
1h is mediated to 40rpm, obtains kneaded mixture material；
3) extract：Deionized water is added into kneaded mixture material, is filtered, 4 extremely salt-free, microwave drying of washing, is crushed,
300 sieves are crossed, are produced.
Embodiment 3：
The preparation method of reducing dye Vat Yellow 1, comprises the following steps：
1) grind：Crude product Vat Yellow 1 is added in mill, adds the carboxylic of crude product Vat Yellow 1 quality 0.5% thereto
Methyl chitosan, granularity is ground to as 3 μm, obtains grinding material；
2) mediate：Grinding material is added in kneader, adds the sodium chloride of 4 times of crude product Vat Yellow 1 quality thereto
Micro mist, be stirred, then thereto add 1.1 times of crude product Vat Yellow 1 quality hexamethyl phosphoramide, be stirred, 40 DEG C,
Rotating speed is to mediate 0.5h under 30rpm, is mediated under being warming up to 70 DEG C using 2 DEG C/min heating rate, adjusted rotating speed as 35rpm
1.5h, it is warming up to 90 DEG C with 1 DEG C/min heating rate, maintains the constant kneading 1.5h of rotating speed, maintain temperature-resistant adjustment rotating speed
1h is mediated to 40rpm, obtains kneaded mixture material；
3) extract：Deionized water is added into kneaded mixture material, is filtered, 5 extremely salt-free, microwave drying of washing, is crushed,
300 sieves are crossed, are produced.
Embodiment 4：
The preparation method of reducing dye Vat Yellow 1, comprises the following steps：
1) grind：Crude product Vat Yellow 1 is added in mill, adds the carboxylic of crude product Vat Yellow 1 quality 0.5% thereto
Methyl chitosan, granularity is ground to as 2 μm, obtains grinding material；
2) mediate：Grinding material is added in kneader, adds the sodium chloride of 3 times of crude product Vat Yellow 1 quality thereto
Micro mist, be stirred, then thereto add 0.9 times of crude product Vat Yellow 1 quality hexamethyl phosphoramide, be stirred, 40 DEG C,
Rotating speed is to mediate 0.5h under 30rpm, is mediated under being warming up to 70 DEG C using 2 DEG C/min heating rate, adjusted rotating speed as 35rpm
1.5h, it is warming up to 90 DEG C with 1 DEG C/min heating rate, maintains the constant kneading 1.5h of rotating speed, maintain temperature-resistant adjustment rotating speed
1h is mediated to 40rpm, obtains kneaded mixture material；
3) extract：Deionized water is added into kneaded mixture material, is filtered, 5 extremely salt-free, microwave drying of washing, is crushed,
300 sieves are crossed, are produced.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments
The present invention is described in detail, it will be understood by those within the art that：It still can be to foregoing each implementation
Technical scheme described in example is modified, or carries out equivalent substitution to which part technical characteristic；And these modification or
Replace, the essence of appropriate technical solution is departed from the spirit and scope of various embodiments of the present invention technical scheme.
Claims (5)
1. a kind of preparation method of reducing dye Vat Yellow 1, it is characterised in that comprise the following steps：
1) grind：Crude product Vat Yellow 1 is added in mill, appropriate carboxymethyl chitosan is added thereto, is ground to grain
Spend for 2-3 μm, obtain grinding material；
2) mediate：Grinding material is added in kneader, adds sodium chloride micro-powder thereto, is stirred, then is added thereto
Enter hexamethyl phosphoramide, be stirred, mediate 0.5h under being 30rpm in 40 DEG C, rotating speed, heated up with 2 DEG C/min heating rate
It is to mediate 1.5h under 35rpm to 70 DEG C, adjustment rotating speed, is warming up to 90 DEG C with 1 DEG C/min heating rate, maintains that rotating speed is constant pinches
1.5h is closed, maintains temperature-resistant adjustment rotating speed to mediate 1h to 40rpm, obtains kneaded mixture material；
3) extract：Deionized water is added into kneaded mixture material, is filtered, 4-5 extremely salt-free, microwave drying of washing, is crushed, mistake
Sieve, is produced.
2. the preparation method of reducing dye Vat Yellow 1 as claimed in claim 1, it is characterised in that the carboxymethyl chitosan
Addition be crude product Vat Yellow 1 quality 0.3-0.5%.
3. the preparation method of reducing dye Vat Yellow 1 as claimed in claim 1, it is characterised in that the 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 the hexamethyl phosphoramide
Mass ratio with crude product Vat Yellow 1 is 9-11：10.
5. the preparation method of reducing dye Vat Yellow 1 as claimed in claim 1, it is characterised in that 300 are crossed in the step 3)
Mesh sieve.
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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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| 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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| Publication Number | Publication Date |
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| CN106221278A CN106221278A (en) | 2016-12-14 |
| CN106221278B true CN106221278B (en) | 2017-11-10 |
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| 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 |
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 |
|---|
| 还原黄G的颜料化工艺进展;张天永等;《染料与染色》;20021230;第39卷(第06期);7-10 * |
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| CN106221278A (en) | 2016-12-14 |
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| GR01 | Patent grant | ||
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| 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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| 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 | ||
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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 |