CN109206941A - A kind of preparation method of Vickery blue finished product - Google Patents
A kind of preparation method of Vickery blue finished product Download PDFInfo
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- CN109206941A CN109206941A CN201811031078.4A CN201811031078A CN109206941A CN 109206941 A CN109206941 A CN 109206941A CN 201811031078 A CN201811031078 A CN 201811031078A CN 109206941 A CN109206941 A CN 109206941A
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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
- C09B67/0072—Preparations with anionic dyes or reactive dyes
- C09B67/0073—Preparations of acid or reactive dyes in liquid form
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- Organic Chemistry (AREA)
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Abstract
The present invention relates to acid dyes technical fields, more particularly to a kind of preparation method of Vickery blue finished product, the preparation method is that formula (II) compound, formula (III) compound are under the catalytic action of catalyst C-1, condensation reaction is made under alkaline condition, and the catalyst C-1 is Cu2O, the catalyst C-1 are to use copper sulphate, sucrose or glucose, sodium hydroxide hybrid reaction, are made through filtering.Preparation method of the invention can realize that higher conversion ratio, metal ion do not need to carry out refinement treatment less, disposing mother liquor is applied, and without dust pollution, clean and environmental protection are spray-dried under less catalyst amount.
Description
Technical field
The present invention relates to acid dyes technical field more particularly to a kind of preparation methods of Vickery blue finished product.
Background technique
It is well known that acid dyes have color is bright-coloured, dye-uptake and the good advantage of dyefastness, and the acidity of Anthraquinones
Dyestuff then more has excellent fastness to light.In the prior art, formula (I)Shown in acid
Property dyestuff production use following techniques: bromamine acid and 3-acetylaminoaniline in the presence of copper sulphate, Sold Stannous Chloride Catalyzes agent,
Be condensed under Fu's acid agent effect and generate target compound, then acid out, filtering, washing, filter cake mashing purification, again acid out filters pressing,
It standardizes and obtains after drying.The technique has the disadvantage in that
1, energy consumption is high, wastewater pressure is big, thus technique is cumbersome, process is complicated, acid out filtering is needed to re-refine washing ability
Qualified products are obtained, manpower and material resources investment is larger, generates a large amount of waste water；
2, since condensation reaction uses old-fashioned catalyst (copper sulphate, stannous chloride), the metal ions such as copper, tin are exceeded, go
Except the metal ion must refine, wash；
3, being standardized after drying will cause serious dyestuff dust pollution.
Therefore, it is necessary to a kind of environmental protection and energy saving, and catalyst amount is few, are not necessarily to refinement treatment, can reduce the clear of dust pollution
Clean technique.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of preparation method of Vickery blue finished product, the preparation method
It can realize that higher conversion ratio, metal ion do not need to carry out refinement treatment, disposing mother liquor less under less catalyst amount
It applies, is spray-dried without dust pollution, clean and environmental protection.
The present invention solves above-mentioned technical problem by following technological means:
The preparation method of the Vickery blue finished product of one kind such as formula (I),
The preparation method is that formula (II) compound, formula (III) compound be under the catalytic action of catalyst C-1, in alkalinity
Under the conditions of condensation reaction be made, (II) compound, the chemical structural formula of formula (III) compound are as follows:
The reaction equation being related to is as follows:
Further, the catalyst C-1 is Cu2O, the catalyst C-1 are with copper sulphate, sucrose or glucose, hydrogen-oxygen
Change sodium hybrid reaction, is made through filtering.The reaction equation being related to is as follows:
CuSO4+2NaOH→NaSO4+Cu(OH)2
2Cu(OH)2+CH2OH(CHOH)4CHO→Cu2O+2H2O+CH2OH(CHOH)4COOH
Cu2O catalyst is prepared with copper sulphate, glucose, sodium hydroxide, wherein play major catalytic is
Cu2Cu in O+Ion, and the Cu in the condensation reaction of formula (II) compound and formula (III) compound+Ion and Cu2+Ion exists
A kind of dynamic equilibrium can maintain always the activity of catalyst, Jin Erke in reaction under sucrose or glucose, Fu's acid agent effect
To reach comparatively ideal catalytic effect under the smaller dosage of catalyst.
Further, in the condensation reaction, the dosage of catalyst C-1 presses the molar ratio 1 of copper ion and formula (II) compound:
28~35 add.
Further, the preparation method of above-mentioned Vickery blue finished product is specific as follows:
Water is added in a kettle, stirs addition formula (II) compound, stirring adds formula (III) compound, stirring heating
To 58~82 DEG C, catalyst C-1 is added, acid binding agent is added and adjusts pH=7.5~9.0, adjusts pH and adds sucrose or Portugal in the process
Grape sugar, is then stirred to react 2~3h in 65~85 DEG C, obtains reaction solution；
Liquid alkaline is added into reaction solution, and is warming up to 90 DEG C of heat preservation 30min, water supplement, then plus pearlite filtering aid, mistake
Filter obtains reaction filtrate；
Reaction filtrate is cooled to 40~55 DEG C, adjusts pH=7~9 with hydrochloric acid, stirring cooling precipitates, and filters pressing obtains
Disposing mother liquor is applied, and filter cake is stand-by；
Water and filter cake are added in a kettle, mashing is warming up to 80 DEG C, after addition dispersing agent and filler are standardized,
Slurry is obtained, control slurry concentration is spray-dried for 20~30%, obtains Vickery blue finished product.
Catalyst C-1 and sucrose or glucose, which are used in mixed way, can extend catalyst C-1 service life, make catalyst amount
It is double-diminished, and metal ion is few, the reaction later period makes copper ion form Kocide SD precipitating through processing, filters off through past insoluble matter
It removes, so that metal ion in target product is reached standard requirements, target product filter cake, filtrate is obtained by filtration through being precipitated again in reaction filtrate
Recovery reduces waste water and generates.Using spray drying, dust pollution is avoided.
Further, the acid binding agent is the mixing of one or both of soda ash, sodium bicarbonate, ammonium bicarbonate, potassium carbonate.
Further, the concentration of the slurry is controlled 20%.
Further, specific step is as follows for the preparation method of Vickery blue finished product:
2800kg water is added in a kettle, 382kg formula (II) compound is added in stirring, stirs 10min, adds 185kg
Formula (III) compound, stirring are warming up to 58~82 DEG C, and catalyst C-1 is added, and soda ash is added and adjusts pH=7.5~9.0, adjusts pH
6kg glucose is added in the process, is then stirred to react 2~3h in 65~85 DEG C, is obtained reaction solution；
5kg liquid alkaline is added into reaction solution, and is warming up to 90 DEG C of heat preservations 30min, water supplement 1000kg, then plus perlite
Filter aid, filtering obtain reaction filtrate；
Reaction filtrate is cooled to 40~55 DEG C, adjusts pH=7~9 with hydrochloric acid, stirring cooling precipitates, and filters pressing obtains
Disposing mother liquor is applied, and filter cake is stand-by；
1200kg water and filter cake are added in a kettle, mashing is warming up to 80 DEG C, and dispersing agent is added and filler is marked
After standardization, slurry is obtained, control slurry concentration is spray-dried for 20~30%, obtains Vickery blue finished product.
Preparation method of the invention is applied using disposing mother liquor, reduces the discharge of waste water to a certain extent；Condensation is anti-
The a small amount of catalyst C-1 of middle use and sucrose or glucose are answered, that is, can reach 93~95% conversion ratio, and containing few in reaction solution
The copper ion of amount, can not be washed with water, refine, that is, can reach the quality requirements of required product, really realize and produce without waste water metaplasia,
Environmental friendly cleaning.
Disposing mother liquor of the invention waits applying, and simplifies the process flows such as acid out, purification, washing, and dispersion is added in filter cake mashing
Agent and filler are standardized, and direct-injection spray drying reduces production waste water, are reduced dust pollution, are reduced energy consumption and be produced into
This.
Specific embodiment
Below with reference to specific embodiment, the present invention is described in detail:
A kind of preparation method of Vickery blue finished product of the invention, the chemical structural formula of Vickery blue are as follows:
The preparation method of the Vickery blue finished product is shown in following embodiment:
Embodiment one
It takes 0.8kg copper sulphate to be added in 10kg water to stir to being completely dissolved, 10kg liquid alkaline and 0.4kg glucose is then added
Reaction filters, is dried to obtain catalyst C-1.
2800kg water is added in a kettle, 382kg formula (II) (100%) compound is added in stirring, stirs 10min, throws
Add 185kg formula (III) (100%) compound, stirring is warming up to 58~82 DEG C, and catalyst C-1 is added, and the dosage of catalyst C-1 is pressed
The ratio of the molar ratio 1:0.075 of illuminated (II) compound and copper ion is added, and soda ash is added and adjusts pH=7.5~9.0,
It adjusts pH and adds 6kg sucrose in the process, be then stirred to react 2~3h in 65~85 DEG C, obtain reaction solution；
5kg liquid alkaline is added into reaction solution, and is warming up to 90 DEG C of heat preservations 30min, water supplement 1000kg, then plus perlite
Filter aid, filtering obtain reaction filtrate；
Reaction filtrate is cooled to 40~55 DEG C, adjusts pH=7~9 with hydrochloric acid, stirring cooling precipitates, and filters pressing obtains
Disposing mother liquor is applied, and filter cake is stand-by；
1200kg water and filter cake are added in a kettle, mashing is warming up to 80 DEG C, and dispersing agent is added and filler is marked
After standardization, slurry is obtained, control slurry concentration is spray-dried for 20%, obtains Vickery blue finished product.
Embodiment two
The dosage of the present embodiment catalyst C-1 according to formula (II) compound and the molar ratio 1:0.051 of copper ion ratio
It is added, other processing steps and condition are the same as example 1.
Embodiment three
The dosage of the present embodiment catalyst C-1 according to formula (II) compound and the molar ratio 1:0.034 of copper ion ratio
It is added, other processing steps and condition are the same as example 1.
Example IV
It takes 0.8kg copper sulphate to be added in 10kg water to stir to being completely dissolved, 10kg liquid alkaline then is added and 0.4kg sucrose is anti-
It answers, filters, be dried to obtain catalyst C-1.
2800kg water is added in a kettle, 382kg formula (II) compound is added in stirring, stirs 10min, adds 185kg
Formula (III) compound, stirring are warming up to 58~82 DEG C, catalyst C-1 are added, the dosage of catalyst C-1 is according to formula (II) compound
It is added with the ratio of the molar ratio 28:1 of copper ion, sodium bicarbonate is added and adjusts pH=7.5~9.0, adjust benefit during pH
Add 8kg glucose, is then stirred to react 2~3h in 65~85 DEG C, obtains reaction solution；
5kg liquid alkaline is added into reaction solution, and is warming up to 90 DEG C of heat preservations 30min, water supplement 1000kg, then plus perlite
Filter aid, filtering obtain reaction filtrate；
Reaction filtrate is cooled to 40~55 DEG C, adjusts pH=7~9 with hydrochloric acid, stirring cooling precipitates, and filters pressing obtains
Disposing mother liquor is applied, and filter cake is stand-by；
1200kg water and filter cake are added in a kettle, mashing is warming up to 80 DEG C, and dispersing agent is added and filler is marked
After standardization, slurry is obtained, control slurry concentration is spray-dried for 20%, obtains Vickery blue finished product.
Embodiment five
2800kg water is added in a kettle, 382kg formula (II) compound is added in stirring, stirs 10min, adds 185kg
Formula (III) compound, stirring are warming up to 58~82 DEG C, catalyst C-1 are added, the dosage of catalyst C-1 is according to formula (II) compound
It is added with the ratio of the molar ratio 35:1 of copper ion, ammonium bicarbonate, the potassium carbonate mixtures that mass ratio is 1:1 is added, adjust pH
=7.5~9.0, it adjusts pH and adds 7kg sucrose in the process, be then stirred to react 2~3h in 65~85 DEG C, obtain reaction solution；
5kg liquid alkaline is added into reaction solution, and is warming up to 90 DEG C of heat preservations 30min, water supplement 1000kg, then plus perlite
Filter aid, filtering obtain reaction filtrate；
Reaction filtrate is cooled to 40~55 DEG C, adjusts pH=7~9 with hydrochloric acid, stirring cooling precipitates, and filters pressing obtains
Disposing mother liquor is applied, and filter cake is stand-by；
1200kg water and filter cake are added in a kettle, mashing is warming up to 80 DEG C, and dispersing agent is added and filler is marked
After standardization, slurry is obtained, control slurry concentration is spray-dried for 20%, obtains Vickery blue finished product.
Comparative example
Water 3200kg is added using old technique as comparative example in the present invention in a kettle, stir lower throw-in type (II)
(100%) 382kg is stirred 10 minutes, adds (III) compound (100%) 180kg, and stirring is warming up to 60~75 DEG C, in three times
Copper sulphate, stannous chloride mixed catalyst is added, controls pH=7.5~9.0 with 423kg soda ash or sodium bicarbonate, controls temperature 68
Under the conditions of~85 DEG C, it is stirred to react 3~5 hours to terminal, obtains reaction solution；
Reaction solution is cooled to 40~45 DEG C or so, analysis is clear, seeps and encloses using light gray without blue as terminal, and filtering obtains
Filtrate recovery is reacted, filter cake is stand-by；
It takes 35 kilogram of 98% sulfuric acid to be added in 5 tons of water, 50 kilograms of refined salt is added, preparation obtains acid washing water, washed with pickling
Filter cake is washed to wash water in lilac red, obtains wet product；
It takes 10 tons of water to be warming up to 70~71 DEG C, is added with stirring 1 batch of wet product, (be diluted to 5- with 50kg30% liquid alkaline
10%) pH=10~10.2, are adjusted, about must be 30~45 minutes, 14 tons are obtained, immediately acid out, 260kg30% hydrochloric acid is added to adjust PH=
1.5~2, point seeps circle, and outer ring is micro- purple, and inner lane is that micro- blue or grey blue is that terminal is precipitated to obtain in 68~70 DEG C of filters pressings of temperature
To 730kg wet product, signature 533.8kg, yield 1.397, statistics produces mark product per ton and about generates 35 tons of waste water or so, by wet product
It crushes, appropriate amount of addition agent is added, filler is standardized finished product.
The preparation method of embodiment one, two, three and comparative example is compared, data as shown in Table 1 are obtained:
Table 1
Table 1 statistics indicate that: old technology catalyst amount is more, is otherwise unable to reach terminal, and metal ion needs to refine more
Processing, can generate a large amount of waste water, not environmentally；New process catalyst amount is few, high conversion rate, and metal ion can not refine place less
Reason, is produced using no waste water, is clean and environmental protection technique.
The above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although referring to preferred embodiment to this hair
It is bright to be described in detail, those skilled in the art should understand that, it can modify to technical solution of the present invention
Or equivalent replacement should all cover without departing from the objective and range of technical solution of the present invention in claim of the invention
In range.Technology not described in detail in the present invention, shape, construction portion are well-known technique.
Claims (7)
1. the preparation method of one kind such as Vickery blue finished product of formula (I),
It is characterized in that, the preparation method is that formula (II) compound, formula (III) compound catalyst C-1 catalytic action
Under, condensation reaction is made under alkaline condition, and (II) compound, the chemical structural formula of formula (III) compound are as follows:
2. a kind of preparation method of Vickery blue finished product according to claim 1, which is characterized in that the catalyst
C-1 is Cu2O, the catalyst C-1 are to use copper sulphate, sucrose or glucose, sodium hydroxide hybrid reaction, are made through filtering.
3. a kind of preparation method of Vickery blue finished product according to claim 2, which is characterized in that the condensation is anti-
The dosage of Ying Zhong, catalyst C-1 are added by molar ratio 1:28~35 of copper ion and formula (II) compound.
4. a kind of preparation method of Vickery blue finished product according to claim 3, which is characterized in that the preparation side
Method is specific as follows:
Water is added in a kettle, stirs addition formula (II) compound, stirring adds formula (III) compound, and stirring is warming up to 58
~82 DEG C, catalyst C-1 is added, acid binding agent is added and adjusts pH=7.5~9.0, adjusts pH and adds sucrose or glucose in the process,
It then is stirred to react 2~3h in 65~85 DEG C, obtains reaction solution；
Liquid alkaline is added into reaction solution, and is warming up to 90 DEG C of heat preservation 30min, water supplement, then plus pearlite filtering aid, filtering,
Obtain reaction filtrate；
Reaction filtrate is cooled to 40~55 DEG C, adjusts pH=7~9, stirring cooling, precipitating, filters pressing, obtained mother liquor with hydrochloric acid
Recovery, filter cake are stand-by；
Water and filter cake are added in a kettle, mashing is warming up to 80 DEG C, after addition dispersing agent and filler are standardized, obtains
Slurry, control slurry concentration are spray-dried for 20~30%, obtain Vickery blue finished product.
5. a kind of preparation method of Vickery blue finished product according to claim 4, which is characterized in that the acid binding agent
For the mixing of one or both of soda ash, sodium bicarbonate, ammonium bicarbonate, potassium carbonate.
6. a kind of preparation method of Vickery blue finished product according to claim 5, which is characterized in that the slurry
Concentration is controlled 20%.
7. a kind of preparation method of Vickery blue finished product according to claim 6, which is characterized in that specific steps are such as
Under:
2800kg water is added in a kettle, 382kg formula (II) compound is added in stirring, stirs 10min, adds 185kg formula
(III) compound, stirring are warming up to 58~82 DEG C, and catalyst C-1 is added, and soda ash is added and adjusts pH=7.5~9.0, adjusts pH mistake
6kg glucose is added in journey, is then stirred to react 2~3h in 65~85 DEG C, is obtained reaction solution；
5kg liquid alkaline is added into reaction solution, and is warming up to 90 DEG C of heat preservations 30min, water supplement 1000kg, then adds perlite drainage
Agent, filtering obtain reaction filtrate；
Reaction filtrate is cooled to 40~55 DEG C, adjusts pH=7~9, stirring cooling, precipitating, filters pressing, obtained mother liquor with hydrochloric acid
Recovery, filter cake are stand-by；
1200kg water and filter cake are added in a kettle, mashing is warming up to 80 DEG C, and dispersing agent is added and filler is standardized
Afterwards, slurry is obtained, control slurry concentration is spray-dried for 20%, obtains Vickery blue finished product.
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| CN201811031078.4A CN109206941A (en) | 2018-09-05 | 2018-09-05 | A kind of preparation method of Vickery blue finished product |
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| CN201811031078.4A CN109206941A (en) | 2018-09-05 | 2018-09-05 | A kind of preparation method of Vickery blue finished product |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002012786A (en) * | 2000-06-27 | 2002-01-15 | Sumitomo Chem Co Ltd | Process for preparing anthraquinone reactive dye |
| CN101585974A (en) * | 2008-12-12 | 2009-11-25 | 天津市德凯化工有限公司 | Method for preparing wool reactive-dye brilliant blue |
| CN102863815A (en) * | 2012-08-06 | 2013-01-09 | 湖北华丽染料工业有限公司 | Method for preparing active dye for blue wool |
-
2018
- 2018-09-05 CN CN201811031078.4A patent/CN109206941A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002012786A (en) * | 2000-06-27 | 2002-01-15 | Sumitomo Chem Co Ltd | Process for preparing anthraquinone reactive dye |
| CN101585974A (en) * | 2008-12-12 | 2009-11-25 | 天津市德凯化工有限公司 | Method for preparing wool reactive-dye brilliant blue |
| CN102863815A (en) * | 2012-08-06 | 2013-01-09 | 湖北华丽染料工业有限公司 | Method for preparing active dye for blue wool |
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