CN106317955A - Brown reduction dye and preparation method thereof - Google Patents
Brown reduction dye and preparation method thereof Download PDFInfo
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- CN106317955A CN106317955A CN201610595886.8A CN201610595886A CN106317955A CN 106317955 A CN106317955 A CN 106317955A CN 201610595886 A CN201610595886 A CN 201610595886A CN 106317955 A CN106317955 A CN 106317955A
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- raw material
- vat dye
- preparation
- copper powder
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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
- 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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Cosmetics (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a brown reduction dye and a preparation method thereof. The dye is prepared from 7-11 parts of 1,5-dichloroanthraquinone, 6-8 parts of 1-amination, 2-3 parts of copper powder, 6-9 parts of anhydrous calcium carbonate, 11-14 parts of urea, 7-12 parts of sodium fluoride, 5-9 parts of anhydrous sodium acetate and 3-7 parts of aluminum trichloride. In the method, condensation reaction is conducted first, then ring-closure reaction is conducted, utilization efficiency of raw materials is greatly improved during reaction, and raw material waste and pollution discharge are avoided. The technical processes are connected, the production period is effectively shortened, and the raw materials are mixed more evenly. The raw materials are easy to obtain, preparation cost is greatly reduced, and the method can be further applied and popularized in actual industrial production.
Description
Technical field
The present invention relates to reducing dye preparation field, be specifically related to a kind of brown vat dye and preparation method thereof.
Background technology
Along with the continuous lifting of present society's scientific and technological level, people for the quality of the life of self pursuit the most increasingly
Height, the development of reducing dye is that the natural reducing dye before used is bipseudoindoxyl dye structure away from you of existing more than 100 year of the present,
But on reality is applied, natural dyestuff amount to obtain is few, it is difficult to meet market and industrial requirement so that going back of synthesis
Former dyestuff is at home and abroad developed rapidly.Especially for the manufacturing enterprise of China, developing steps are later, and one is chosen especially
War.
But present reducing dye preparation technology is complex so that when carrying out actual production, easily produce serious
Raw material mixing uneven, and in process of production, the complex operation between individual technological process, the most easily cause the cycle produced
Extend.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of brown vat dye and preparation method thereof so that by former
Between material, each component mix homogeneously, shortens manufacturing cycle simultaneously.
For realizing object above, the present invention is achieved by the following technical programs:
A kind of brown vat dye, the component of raw material includes the following: 1,5-dichloroanthraquinone 7-11 part, 1-amino anthraquinones 6-8
Part, copper powder 2-3 part, Carbon Dioxide calcium 6-9 part, carbamide 11-14 part, sodium fluoride 7-12 part, anhydrous sodium acetate 5-9 part, tri-chlorination
Aluminum 3-7 part.
Preferably, the component of raw material includes the following: 1,5-dichloroanthraquinone 8-10 part, 1-amino anthraquinones 7-8 part, copper powder 2-3
Part, Carbon Dioxide calcium 6-8 part, carbamide 11-13 part, sodium fluoride 9-11 part, anhydrous sodium acetate 6-8 part, aluminum chloride 4-6 part.
Preferably, the component of raw material includes the following: 1,5-dichloroanthraquinone 9 parts, 1-amino anthraquinones 8 parts, copper powder 2 parts, anhydrous
Calcium carbonate 7 parts, 12 parts of carbamide, sodium fluoride 10 parts, anhydrous sodium acetate 7 parts, aluminum chloride 4 parts.
The preparation method of described brown vat dye, operating procedure is as follows:
1) by 1,5-dichloroanthraquinone, 1-amino anthraquinones, copper powder, Carbon Dioxide calcium mix by weight, at 90-98 DEG C
Carry out being dehydrated 20-30min, then carry out being incubated 1-2h, under conditions of carrying out intensification 230-250 DEG C subsequently, continue reaction 2-3h；
2) by step 1) product that generates after reaction proceeds to be incubated 5-7h, then lowers the temperature, pulverize after taking out product,
Standby；
3) under conditions of 30-40 DEG C, by step 2) process after product and carbamide, sodium fluoride, anhydrous sodium acetate, trichlorine
Change aluminum to mix by weight, and react 1-2h at temperature is warming up to 160-180 DEG C, be then incubated 20-40min, subsequently
Cooling, pulverizes, standby；
4) by step 3) process after raw material add sulphuric acid, and be warming up to 92-98 DEG C, be incubated 1h, be then diluted with water to
50-55 DEG C, filter, then be washed to neutrality, be dried.
Preferably, described step 2) in, the product after pulverizing is put in water and is stirred, and heats up, insulation, then lowers the temperature
Process, and carry out filtration drying, pulverizing.
Preferably, described step 3) when lowering the temperature, when being cooled to 50-60 DEG C, pulverize while hot.
The invention provides a kind of brown vat dye and preparation method thereof, use in method first carries out shrink instead
Should, carrying out ring-closure reaction, in reaction, be greatly improved the utilization ratio of raw material, it is to avoid the waste of raw material and exhaust emission,
And be mutually linked between each technological process, it is effectively shortened the production cycle so that mix more uniform between raw material.Each component
Raw material easily obtains, and greatly reduces prepared composition, can be further generalized application in industry actual production.
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 enforcement of the present invention
Example, is clearly and completely described the technical scheme in the embodiment of the present invention, it is clear that described embodiment is the present invention
A part of embodiment rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not having
Have and make the every other embodiment obtained under creative work premise, broadly fall into the scope of protection of the invention.
Embodiment 1:
The present embodiment provides a kind of brown vat dye, and the component of raw material includes the following: 1,5-dichloroanthraquinone 9 parts, 1-ammonia
Base anthraquinone 8 parts, copper powder 2 parts, Carbon Dioxide calcium 7 parts, 12 parts of carbamide, sodium fluoride 10 parts, anhydrous sodium acetate 7 parts, aluminum chloride 4
Part.
Embodiment 2:
The present embodiment provides a kind of brown vat dye, and the component of raw material includes the following: 1,5-dichloroanthraquinone 7 parts, 1-ammonia
Base anthraquinone 6 parts, copper powder 3 parts, Carbon Dioxide calcium 6 parts, 12 parts of carbamide, sodium fluoride 9 parts, anhydrous sodium acetate 5 parts, aluminum chloride 6 parts.
Embodiment 3:
The present embodiment provides a kind of brown vat dye, and the component of raw material includes the following: 1,5-dichloroanthraquinone 11 parts, 1-ammonia
Base anthraquinone 6 parts, copper powder 2 parts, Carbon Dioxide calcium 9 parts, 14 parts of carbamide, sodium fluoride 11 parts, anhydrous sodium acetate 6 parts, aluminum chloride 5
Part.
Embodiment 4:
The present embodiment provides a kind of brown vat dye, and the component of raw material includes the following: 1,5-dichloroanthraquinone 10 parts, 1-ammonia
Base anthraquinone 7 parts, copper powder 3 parts, Carbon Dioxide calcium 8 parts, 12 parts of carbamide, sodium fluoride 12 parts, anhydrous sodium acetate 6 parts, aluminum chloride 6
Part.
Embodiment 5:
The present embodiment provides a kind of brown vat dye, and the component of raw material includes the following: 1,5-dichloroanthraquinone 8 parts, 1-ammonia
Base anthraquinone 8 parts, copper powder 2 parts, Carbon Dioxide calcium 7 parts, 11 parts of carbamide, sodium fluoride 7 parts, anhydrous sodium acetate 9 parts, aluminum chloride 4 parts.
The preparation method of brown vat dye, operating procedure is as follows:
1) by 1,5-dichloroanthraquinone, 1-amino anthraquinones, copper powder, Carbon Dioxide calcium mix by weight, at 90-98 DEG C
Carry out being dehydrated 20-30min, then carry out being incubated 1-2h, under conditions of carrying out intensification 230-250 DEG C subsequently, continue reaction 2-3h；
2) by step 1) product that generates after reaction proceeds to be incubated 5-7h, then lowers the temperature, take out powder after product
Broken, standby；
3) under conditions of 30-40 DEG C, by step 2) process after product and carbamide, sodium fluoride, anhydrous sodium acetate, trichlorine
Change aluminum to mix by weight, and react 1-2h at temperature is warming up to 160-180 DEG C, be then incubated 20-40min, subsequently
Cooling, pulverizes, standby；
4) by step 3) process after raw material add sulphuric acid, and be warming up to 92-98 DEG C, be incubated 1h, be then diluted with water to
50-55 DEG C, filter, then be washed to neutrality, be dried.
Step 2) in, the product after pulverizing is put in water and is stirred, and heats up, insulation, then carries out cooling process, and carries out
It is filtered dry dry, pulverizing.
Step 3) when lowering the temperature, when being cooled to 50-60 DEG C, pulverize while hot.
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 (6)
1. a brown vat dye, it is characterised in that the component of raw material includes the following: 1,5-dichloroanthraquinone 7-11 part, 1-ammonia
Base anthraquinone 6-8 part, copper powder 2-3 part, Carbon Dioxide calcium 6-9 part, carbamide 11-14 part, sodium fluoride 7-12 part, anhydrous sodium acetate 5-9
Part, aluminum chloride 3-7 part.
2. brown vat dye as claimed in claim 1, it is characterised in that the component of raw material includes the following: 1,5-bis-chrloroanthracene
Quinone 8-10 part, 1-amino anthraquinones 7-8 part, copper powder 2-3 part, Carbon Dioxide calcium 6-8 part, carbamide 11-13 part, sodium fluoride 9-11 part,
Anhydrous sodium acetate 6-8 part, aluminum chloride 4-6 part.
3. brown vat dye as claimed in claim 1, it is characterised in that the component of raw material includes the following: 1,5-bis-chrloroanthracene
Quinone 9 parts, 1-amino anthraquinones 8 parts, copper powder 2 parts, Carbon Dioxide calcium 7 parts, 12 parts of carbamide, sodium fluoride 10 parts, anhydrous sodium acetate 7 parts,
Aluminum chloride 4 parts.
4. the preparation method of the brown vat dye as described in claim 1-3 any of which item, it is characterised in that operating procedure
As follows:
1) by 1,5-dichloroanthraquinone, 1-amino anthraquinones, copper powder, Carbon Dioxide calcium mix by weight, carry out at 90-98 DEG C
Dehydration 20-30min, then carry out being incubated 1-2h, continue reaction 2-3h under conditions of carrying out intensification 230-250 DEG C subsequently；
2) by step 1) product that generates after reaction proceeds to be incubated 5-7h, then lowers the temperature, pulverize after taking out product, standby
With；
3) under conditions of 30-40 DEG C, by step 2) process after product and carbamide, sodium fluoride, anhydrous sodium acetate, aluminum chloride
Mix by weight, and react 1-2h at temperature is warming up to 160-180 DEG C, be then incubated 20-40min, lower the temperature subsequently,
Pulverize, standby；
4) by step 3) process after raw material add sulphuric acid, and be warming up to 92-98 DEG C, be incubated 1h, be then diluted with water to 50-55
DEG C, filter, then be washed to neutrality, be dried.
5. the preparation method of brown vat dye as claimed in claim 4, it is characterised in that described step 2) in, by powder
Product after broken is put in water and is stirred, and heats up, insulation, then carries out cooling process, and carries out filtration drying, pulverizing.
6. the preparation method of brown vat dye as claimed in claim 5, it is characterised in that described step 3) lower the temperature
Time, when being cooled to 50-60 DEG C, pulverize while hot.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610595886.8A CN106317955A (en) | 2016-07-26 | 2016-07-26 | Brown reduction dye and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610595886.8A CN106317955A (en) | 2016-07-26 | 2016-07-26 | Brown reduction dye and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN106317955A true CN106317955A (en) | 2017-01-11 |
Family
ID=57739285
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610595886.8A Pending CN106317955A (en) | 2016-07-26 | 2016-07-26 | Brown reduction dye and preparation method thereof |
Country Status (1)
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102660131A (en) * | 2012-04-19 | 2012-09-12 | 徐州开达精细化工有限公司 | Method for producing vat yellow 3RT |
| CN104277486A (en) * | 2014-09-15 | 2015-01-14 | 萧县凯奇化工科技有限公司 | Synthesis method of vat yellow 3RR |
| CN104497617A (en) * | 2014-11-29 | 2015-04-08 | 萧县凯奇化工科技有限公司 | Vat dye brown GG and preparation method thereof |
-
2016
- 2016-07-26 CN CN201610595886.8A patent/CN106317955A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102660131A (en) * | 2012-04-19 | 2012-09-12 | 徐州开达精细化工有限公司 | Method for producing vat yellow 3RT |
| CN104277486A (en) * | 2014-09-15 | 2015-01-14 | 萧县凯奇化工科技有限公司 | Synthesis method of vat yellow 3RR |
| CN104497617A (en) * | 2014-11-29 | 2015-04-08 | 萧县凯奇化工科技有限公司 | Vat dye brown GG and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| WILLIAMB RADLEY，P.N.PANDIT: "《The Cyclisation of 1:4- and 1:5-Di-(α-anthracquinylamino)-anthraquinones to Derivatives of Carbazole》", 《JOURNAL OF THE CHEMICAL SOCIETY》 * |
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Application publication date: 20170111 |
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