CN106566275A - Production process of vat olive R - Google Patents
Production process of vat olive R Download PDFInfo
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- CN106566275A CN106566275A CN201611031540.1A CN201611031540A CN106566275A CN 106566275 A CN106566275 A CN 106566275A CN 201611031540 A CN201611031540 A CN 201611031540A CN 106566275 A CN106566275 A CN 106566275A
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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
- C09B5/24—Dyes with an anthracene nucleus condensed with one or more heterocyclic rings with or without carbocyclic rings the heterocyclic rings being only condensed with an anthraquinone nucleus in 1-2 or 2-3 position
- C09B5/26—Carbazoles of the anthracene series
- C09B5/28—Anthrimide carbazoles
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D209/00—Heterocyclic compounds containing five-membered rings, condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D209/56—Ring systems containing three or more rings
- C07D209/80—[b, c]- or [b, d]-condensed
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
- Cosmetics (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention discloses a production process of vat olive R. The production process of the vat olive R is characterized by comprising the following specific steps: S1, dehydrogenation condensation; S, acylation loop closing; S3, oxidization and filtering; and S4, grinding, spraying drying, sample making, mixing, quality inspection, preparation of a finished product and warehouse entry. According to the production process, sodium chlorate replaces manganese dioxide to carry out production, so that the production process is greatly simplified; therefore, the production process is more simplified and more convenient to operate; and the production process of the vat olive R is higher in practicability.
Description
Technical field
The present invention relates to Vat Olive R technical field, specially a kind of Vat Olive R production technology.
Background technology
Nineteen ninety builds up 50 tons of Vat Olive Rs of annual output（Vat Olive R is " Vat Black 27 100 "）Workshop, then formally
Go into operation, waken up with 1- amino anthracenes by the production technology of FIATBB and 1-chloroanthraquinone is contracted as primary raw material in nitro benzene solvent
Close, then Jing is nitrified, reduced, o-dichlorohenzene makees the Benzenecarbonyl chloride. acylation of solvent and closed loop is aoxidized, in order to get rid of poisonous Nitrobenzol
Solvent replaced liquid phase condensations in 1993 using solid phase condensation, but the shortcoming of this process route is that operation is long, is related to primary product
Plant many.
After 1997, it is referred from written by Japanese thin Tian Feng《Dyestuff chemistry manufacture is theoretical》Data, with Isosorbide-5-Nitrae diaminoanthraquinone-
Wake up and 1- amino anthraquinones are primary raw material, and with manganese dioxide make oxidant respectively, sodium hydrosulfite is compiled for the glue oxygen of reducing agent and closes work
Skill, and make enemy's agent for Benzenecarbonyl chloride. with benzoic acid in oleum medium with reference to United States Patent (USP), thus make enemyization and close
Ring is incorporated in one procedure and carries out.
After 2009, through technological innovation, and manganese dioxide and sodium hydrosulfite is replaced to define current existing using sodium chlorate
The easy production process route of comparison employed in production.
The content of the invention
It is an object of the invention to provide a kind of Vat Olive R production technology, the Vat Olive R production technology concrete steps
It is as follows：
S1：Dehydrogenative condensation, pot press-in sodium chlorate measuring tank is standby by preparing for the sodium chlorate solution for preparing, and the sulphuric acid that tank car comes is put into
Sulphuric acid geosyncline, sample analysis are qualified（>98%）, squeeze into sulphuric acid storage tank with submerged pump, then to squeeze into sulfuric acid gauge tank with submerged pump standby
With by sulfuric acid gauge tank by 98% sulphuric acid（370L) slowly it is put into condensation pot and put into 1- amino anthracenes in order with 1 hour in the case where companion is stirred
Quinone and Isosorbide-5-Nitrae-diamino-anthraquinone, maintain at room temperature 2.5 hours, then by water measuring tank lentamente Deca water in 2-3 hours
（480L), water finishes sample analysis condensation acidity, and temperature is less than 62 DEG C, uniform Deca sodium chlorate solution again after maintaining 1 hour
（330L), at 58-62 DEG C, after maintaining 2 hours, it is in blackish green or bluish violet to sample and material is observed on sheet glass to temperature control
For terminal, in case dilution, add water 3000L in dilution pot, and above-mentioned reaction mass is slowly put under stirring, half an hour is stirred, with pressure
Diluted material is pressed into pressure filter by contracting air, presses complete centrifugal pump that hot water in hot water storgae is pumped into into pressure filter washing material, is washed till
Neutrality, then material is dried up with compressed air, the laggard rake type dryer of discharging is dried, and is dried to moisture content and is less than 1%, and blowing barrelling is pressed
Filter filter, washing liquid enter condensation sedimentation tank, and supernatant overflows into acidproof sewer and processed to three wastes workshop；
S2：Acylated closed loop, oleum is put into oleum storage tank, oleum is squeezed into into oleum with submerged pump by tank car
Measuring tank, sample analysis（Sulfur trioxide content 17-22%）It is standby, 20% oleum 280L is slowly put into into acylation by measuring tank
In closed loop pot, point 4-5 time plus condensation substance and benzoic mixture in 2 hours（Stirring should be stopped during charging, temperature is less than 55
℃）, in 55-62 DEG C, stirring is maintained 3 hours, is then cooled to 30 DEG C, and by water juice measuring tank Deca water, temperature control is 32 ± 2
DEG C, addition hydroquinone is finished, and maintained at this temperature, until temperature rises to peak, sample on sheet glass
Observation material is reaction end in brownish red, is stirred half an hour in cooling, standby；
S3：Oxidation and filtration, add water 200L in oxidation pot, opens stirring and adds 20 kilograms of sodium chlorate, after 15 minutes, receives acylation
Closed loop pot material, temperature is less than 55 DEG C, by complete sample analysis acidity, is warming up to 80 DEG C, maintains 2 hours, takes every 15 minutes
Sample checks that oxidant whether there is, and such as oxidant is not enough, should every time add 2 kilograms of sodium chlorates, until meeting the requirements, maintains knot
Beam, by material mortejus is put into, and with compressed air pressure filter is pressed into, and reusable heat water washing is to neutrality, then dries up discharging barrelling, claims
Post processing, sample analysis coloured light, intensity, moisture content etc. are sent into after weight, diafiltration liquid enters acidproof pond, under supernatants after precipitation overflow is entered
Water channel, is processed to three wastes workshop；
S4：Sand milling, be spray-dried, draw a design, blending, quality inspection, finished product and warehouse entry, start sanding-pan stirring, add former dyestuff and three
The diffusant of/mono- amount of calculation, adds water in right amount, carries out sand milling, and the diffusant of its surplus is added after 20 hours, continues sand milling
Sand milling slurry diffusion and pH value is surveyed in 1-2 hours, sampling, it is qualified after use vacuum suction material feeding pot, then with compressed air by sand
Defibrination is depressed into grinding machine groove, and material flows into underground groove Jing after sand mill sand milling, material Jing after grinding machine grinds three times to spray drying groove,
It is to be spray dried, spray drying tower is preheated, when column bottom temperature rises to 100-110 DEG C, open reciprocating diaphragm pump and related system
Pipe valve, by material be delivered to tower top spray gun atomization, during material spray control 85-95 DEG C of column bottom temperature, hot-air from spray tower tower
Jacking enter it is parallel with the dyestuff sand milling slurry of atomization in tower and under, into microballon shape dry powder, most of dry powder is from tower for material wink-dry
Bottom outlet loads in charging basket, and a small amount of fine powder is fitted in charging basket Jing after cyclone separator, has sprayed from bottom of towe, cyclone separator per criticizing
Sampling in charging basket send analysis room to survey moisture content（≤5%）, and quality supervision section analysis coloured light, intensity are sent in sampling.With quality supervision section data during blending
It is that foundation is allocated, is mixed in blender after crushed, analyzes qualified rear packaging and be commercial dye, after finished product
Warehouse entry is preserved.
Preferably, the sodium chlorate solution Wei 30g/L in step S1.
Preferably, the hydroquinone purity in step S2 is that, more than or equal to 99%, addition is 0.8 kilogram, condensation
Thing consumption is 80 kilograms, and benzoic acid consumption is 60 kilograms.
Preferably, the sand milling slurry diffusion in step S4 is 5 grades, pH value 7-8.
Compared with prior art, the invention has the beneficial effects as follows：The present invention replaces manganese dioxide to be given birth to using sodium chlorate
Produce, greatly simplified production technology so that production technology more simplifies, it is more convenient to operate so that Vat Olive R
Production technology has more practicality.
Description of the drawings
Fig. 1 is production technological process of the present invention.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, below in conjunction with specific embodiment, to this
Invention is further elaborated.It should be appreciated that specific embodiment described herein is only to explain the present invention, not
For limiting the present invention.
Embodiment 1
A kind of Vat Olive R production technology, the Vat Olive R production technology is comprised the following steps that：
S1：Dehydrogenative condensation, pot press-in sodium chlorate measuring tank is standby by preparing for the sodium chlorate solution for preparing, and the sulphuric acid that tank car comes is put into
Sulphuric acid geosyncline, sample analysis are qualified（>98%）, squeeze into sulphuric acid storage tank with submerged pump, then to squeeze into sulfuric acid gauge tank with submerged pump standby
With by sulfuric acid gauge tank by 98% sulphuric acid（370L) slowly it is put into condensation pot and put into 1- amino anthracenes in order with 1 hour in the case where companion is stirred
Quinone and Isosorbide-5-Nitrae-diamino-anthraquinone, maintain at room temperature 2.5 hours, then by water measuring tank lentamente Deca water in 2-3 hours
（480L), water finishes sample analysis condensation acidity, and temperature is less than 62 DEG C, uniform Deca sodium chlorate solution again after maintaining 1 hour
（330L), at 58-62 DEG C, after maintaining 2 hours, it is in blackish green or bluish violet to sample and material is observed on sheet glass to temperature control
For terminal, in case dilution, add water 3000L in dilution pot, and above-mentioned reaction mass is slowly put under stirring, half an hour is stirred, with pressure
Diluted material is pressed into pressure filter by contracting air, presses complete centrifugal pump that hot water in hot water storgae is pumped into into pressure filter washing material, is washed till
Neutrality, then material is dried up with compressed air, the laggard rake type dryer of discharging is dried, and is dried to moisture content and is less than 1%, and blowing barrelling is pressed
Filter filter, washing liquid enter condensation sedimentation tank, and supernatant overflows into acidproof sewer and processed to three wastes workshop；
S2：Acylated closed loop, oleum is put into oleum storage tank, oleum is squeezed into into oleum with submerged pump by tank car
Measuring tank, sample analysis（Sulfur trioxide content 17-22%）It is standby, 20% oleum 280L is slowly put into into acylation by measuring tank
In closed loop pot, point 4-5 time plus condensation substance and benzoic mixture in 2 hours（Stirring should be stopped during charging, temperature is less than 55
℃）, in 55-62 DEG C, stirring is maintained 3 hours, is then cooled to 30 DEG C, and by water juice measuring tank Deca water, temperature control is 32 ± 2
DEG C, addition hydroquinone is finished, and maintained at this temperature, until temperature rises to peak, sample on sheet glass
Observation material is reaction end in brownish red, is stirred half an hour in cooling, standby；
S3：Oxidation and filtration, add water 200L in oxidation pot, opens stirring and adds 20 kilograms of sodium chlorate, after 15 minutes, receives acylation
Closed loop pot material, temperature is less than 55 DEG C, by complete sample analysis acidity, is warming up to 80 DEG C, maintains 2 hours, takes every 15 minutes
Sample checks that oxidant whether there is, and such as oxidant is not enough, should every time add 2 kilograms of sodium chlorates, until meeting the requirements, maintains knot
Beam, by material mortejus is put into, and with compressed air pressure filter is pressed into, and reusable heat water washing is to neutrality, then dries up discharging barrelling, claims
Post processing, sample analysis coloured light, intensity, moisture content etc. are sent into after weight, diafiltration liquid enters acidproof pond, under supernatants after precipitation overflow is entered
Water channel, is processed to three wastes workshop；
S4：Sand milling, be spray-dried, draw a design, blending, quality inspection, finished product and warehouse entry, start sanding-pan stirring, add former dyestuff and three
The diffusant of/mono- amount of calculation, adds water in right amount, carries out sand milling, and the diffusant of its surplus is added after 20 hours, continues sand milling
Sand milling slurry diffusion and pH value is surveyed in 1-2 hours, sampling, it is qualified after use vacuum suction material feeding pot, then with compressed air by sand
Defibrination is depressed into grinding machine groove, and material flows into underground groove Jing after sand mill sand milling, material Jing after grinding machine grinds three times to spray drying groove,
It is to be spray dried, spray drying tower is preheated, when column bottom temperature rises to 100-110 DEG C, open reciprocating diaphragm pump and related system
Pipe valve, by material be delivered to tower top spray gun atomization, during material spray control 85-95 DEG C of column bottom temperature, hot-air from spray tower tower
Jacking enter it is parallel with the dyestuff sand milling slurry of atomization in tower and under, into microballon shape dry powder, most of dry powder is from tower for material wink-dry
Bottom outlet loads in charging basket, and a small amount of fine powder is fitted in charging basket Jing after cyclone separator, has sprayed from bottom of towe, cyclone separator per criticizing
Sampling in charging basket send analysis room to survey moisture content（≤5%）, and quality supervision section analysis coloured light, intensity are sent in sampling.With quality supervision section data during blending
It is that foundation is allocated, is mixed in blender after crushed, analyzes qualified rear packaging and be commercial dye, after finished product
Warehouse entry is preserved.
Sodium chlorate solution Wei 30g/L in step S1.
Hydroquinone purity in step S2 is that, more than or equal to 99%, addition is 0.8 kilogram, and condensation substance consumption is
80 kilograms, benzoic acid consumption is 60 kilograms.
Sand milling slurry diffusion in step S4 is 5 grades, pH value 7-8.
The present invention replaces manganese dioxide to be produced using sodium chlorate, greatly simplified production technology so that production work
Skill more simplifies, and it is more convenient to operate so that the production technology of Vat Olive R has more practicality.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any those familiar with the art the invention discloses technical scope in, technology according to the present invention scheme and its
Inventive concept equivalent or change in addition, all should be included within the scope of the present invention.
Claims (4)
1. a kind of Vat Olive R production technology, it is characterised in that：The Vat Olive R production technology is comprised the following steps that：
S1：Dehydrogenative condensation, pot press-in sodium chlorate measuring tank is standby by preparing for the sodium chlorate solution for preparing, and the sulphuric acid that tank car comes is put into
Sulphuric acid geosyncline, sample analysis are qualified（>98%）, squeeze into sulphuric acid storage tank with submerged pump, then to squeeze into sulfuric acid gauge tank with submerged pump standby
With by sulfuric acid gauge tank by 98% sulphuric acid（370L) slowly it is put into condensation pot and put into 1- amino anthracenes in order with 1 hour in the case where companion is stirred
Quinone and Isosorbide-5-Nitrae-diamino-anthraquinone, maintain at room temperature 2.5 hours, then by water measuring tank lentamente Deca water in 2-3 hours
（480L), water finishes sample analysis condensation acidity, and temperature is less than 62 DEG C, uniform Deca sodium chlorate solution again after maintaining 1 hour
（330L), at 58-62 DEG C, after maintaining 2 hours, it is in blackish green or bluish violet to sample and material is observed on sheet glass to temperature control
For terminal, in case dilution, add water 3000L in dilution pot, and above-mentioned reaction mass is slowly put under stirring, half an hour is stirred, with pressure
Diluted material is pressed into pressure filter by contracting air, presses complete centrifugal pump that hot water in hot water storgae is pumped into into pressure filter washing material, is washed till
Neutrality, then material is dried up with compressed air, the laggard rake type dryer of discharging is dried, and is dried to moisture content and is less than 1%, and blowing barrelling is pressed
Filter filter, washing liquid enter condensation sedimentation tank, and supernatant overflows into acidproof sewer and processed to three wastes workshop；
S2：Acylated closed loop, oleum is put into oleum storage tank, oleum is squeezed into into oleum with submerged pump by tank car
Measuring tank, sample analysis（Sulfur trioxide content 17-22%）It is standby, 20% oleum 280L is slowly put into into acylation by measuring tank
In closed loop pot, point 4-5 time plus condensation substance and benzoic mixture in 2 hours（Stirring should be stopped during charging, temperature is less than 55
℃）, in 55-62 DEG C, stirring is maintained 3 hours, is then cooled to 30 DEG C, and by water juice measuring tank Deca water, temperature control is 32 ± 2
DEG C, addition hydroquinone is finished, and maintained at this temperature, until temperature rises to peak, sample on sheet glass
Observation material is reaction end in brownish red, is stirred half an hour in cooling, standby；
S3：Oxidation and filtration, add water 200L in oxidation pot, opens stirring and adds 20 kilograms of sodium chlorate, after 15 minutes, receives acylation
Closed loop pot material, temperature is less than 55 DEG C, by complete sample analysis acidity, is warming up to 80 DEG C, maintains 2 hours, takes every 15 minutes
Sample checks that oxidant whether there is, and such as oxidant is not enough, should every time add 2 kilograms of sodium chlorates, until meeting the requirements, maintains knot
Beam, by material mortejus is put into, and with compressed air pressure filter is pressed into, and reusable heat water washing is to neutrality, then dries up discharging barrelling, claims
Post processing, sample analysis coloured light, intensity, moisture content etc. are sent into after weight, diafiltration liquid enters acidproof pond, under supernatants after precipitation overflow is entered
Water channel, is processed to three wastes workshop；
S4：Sand milling, be spray-dried, draw a design, blending, quality inspection, finished product and warehouse entry, start sanding-pan stirring, add former dyestuff and three
The diffusant of/mono- amount of calculation, adds water in right amount, carries out sand milling, and the diffusant of its surplus is added after 20 hours, continues sand milling
Sand milling slurry diffusion and pH value is surveyed in 1-2 hours, sampling, it is qualified after use vacuum suction material feeding pot, then with compressed air by sand
Defibrination is depressed into grinding machine groove, and material flows into underground groove Jing after sand mill sand milling, material Jing after grinding machine grinds three times to spray drying groove,
It is to be spray dried, spray drying tower is preheated, when column bottom temperature rises to 100-110 DEG C, open reciprocating diaphragm pump and related system
Pipe valve, by material be delivered to tower top spray gun atomization, during material spray control 85-95 DEG C of column bottom temperature, hot-air from spray tower tower
Jacking enter it is parallel with the dyestuff sand milling slurry of atomization in tower and under, into microballon shape dry powder, most of dry powder is from tower for material wink-dry
Bottom outlet loads in charging basket, and a small amount of fine powder is fitted in charging basket Jing after cyclone separator, has sprayed from bottom of towe, cyclone separator per criticizing
Sampling in charging basket send analysis room to survey moisture content（≤5%）, and quality supervision section analysis coloured light, intensity are sent in sampling, with quality supervision section data during blending
It is that foundation is allocated, is mixed in blender after crushed, analyzes qualified rear packaging and be commercial dye, after finished product
Warehouse entry is preserved.
2. a kind of Vat Olive R production technology according to claim 1, it is characterised in that：Chloric acid in step S1
Sodium solution Wei 30g/L.
3. a kind of Vat Olive R production technology according to claim 1, it is characterised in that：In step S2 to benzene
Diphenol purity is that, more than or equal to 99%, addition is 0.8 kilogram, and condensation substance consumption is 80 kilograms, and benzoic acid consumption is 60 kilograms.
4. a kind of Vat Olive R production technology according to claim 1, it is characterised in that：Sand milling in step S4
Slurry diffusion is 5 grades, pH value 7-8.
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| CN201611031540.1A CN106566275B (en) | 2016-11-22 | 2016-11-22 | A kind of Vat Olive R production technology |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611031540.1A CN106566275B (en) | 2016-11-22 | 2016-11-22 | A kind of Vat Olive R production technology |
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| CN106566275B CN106566275B (en) | 2019-10-11 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3023220A (en) * | 1959-10-22 | 1962-02-27 | Gen Aniline & Film Corp | Process of preparing anthramid vat dyestuff |
| US3079398A (en) * | 1959-08-08 | 1963-02-26 | Hoechst Ag | Process for preparing leuco sulfuric acid esters of vat dyestuffs |
| GB981041A (en) * | 1960-10-28 | 1965-01-20 | Ciba Ltd | New anthraquinone dyestuffs and process for their manufacture and use |
| US3230232A (en) * | 1959-12-17 | 1966-01-18 | I C I Organics Inc | Process for the preparation of certain anthraquinone-carbazole dyestuffs |
| US4520202A (en) * | 1981-12-09 | 1985-05-28 | Bayer Aktiengesellschaft | Process for preparing 4,4'-dibenzoylaminodianthrimidecarbazole |
-
2016
- 2016-11-22 CN CN201611031540.1A patent/CN106566275B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3079398A (en) * | 1959-08-08 | 1963-02-26 | Hoechst Ag | Process for preparing leuco sulfuric acid esters of vat dyestuffs |
| US3023220A (en) * | 1959-10-22 | 1962-02-27 | Gen Aniline & Film Corp | Process of preparing anthramid vat dyestuff |
| US3230232A (en) * | 1959-12-17 | 1966-01-18 | I C I Organics Inc | Process for the preparation of certain anthraquinone-carbazole dyestuffs |
| GB981041A (en) * | 1960-10-28 | 1965-01-20 | Ciba Ltd | New anthraquinone dyestuffs and process for their manufacture and use |
| US3338904A (en) * | 1960-10-28 | 1967-08-29 | Ciba Ltd | Anthraquinone dyestuffs |
| US4520202A (en) * | 1981-12-09 | 1985-05-28 | Bayer Aktiengesellschaft | Process for preparing 4,4'-dibenzoylaminodianthrimidecarbazole |
Non-Patent Citations (2)
| Title |
|---|
| 上海市染化十一厂: ""还原橄榄R新工艺试验成功"", 《染料与染色》 * |
| 刘云 主编: "《日用化学品原材料技术手册》", 31 October 2003, 化学工业出版社 * |
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