CN212864625U - Pigment yellow 13 synthesis equipment - Google Patents

Pigment yellow 13 synthesis equipment Download PDF

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CN212864625U
CN212864625U CN202021091137.XU CN202021091137U CN212864625U CN 212864625 U CN212864625 U CN 212864625U CN 202021091137 U CN202021091137 U CN 202021091137U CN 212864625 U CN212864625 U CN 212864625U
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kettle
centrifugal pump
metering tank
diazo
pigment yellow
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陈建新
倪越彪
章立新
方标
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Shaoxing Shangyu Daxin Color Chemical Co ltd
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Shaoxing Shangyu Daxin Color Chemical Co ltd
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Abstract

The utility model discloses a pigment yellow 13 synthesis device, which comprises a sodium nitrite dissolution kettle, a hydrochloric acid metering tank, a sodium nitrite solution metering tank, a diazo kettle, a first centrifugal pump, a tubular filter, a particle dry ice manufacturing machine, an acetoacetanilide pulping kettle, an emulsifying pump, a coupling kettle, a liquid alkali metering tank, a magnetic filter barrel, a second centrifugal pump and a dark flow membrane filter press; the sodium nitrite dissolving kettle is communicated with the inner cavity of the diazo kettle through a first centrifugal pump and a sodium nitrite solution metering tank in sequence; the hydrochloric acid metering tank is communicated with the inner cavity of the diazo kettle; the diazo kettle is communicated with the inner cavity of the coupling kettle sequentially through the first centrifugal pump and the tubular filter. The utility model discloses can solve the technical problem who how to optimize pigment yellow 13's synthesizer, make its easy operation, it is of high quality, the waste water volume is few.

Description

Pigment yellow 13 synthesis equipment
Technical Field
The utility model relates to a synthetic equipment of pigment yellow 13.
Background
The pigment yellow has various types, mainly comprises isoindolinone pigments, benzimidazolone pigments, benzidine yellow pigments, azo acid yellow pigments, polyvinyl ketone azo pigments and the like, and is widely applied to the industries of coatings, plastics, textiles, printing ink and the like. By changing the molecular structure inside the organic pigment yellow, high-grade organic pigment with bright color, excellent heat resistance, weather fastness and solvent resistance can be prepared, and the organic pigment can be widely applied to the fields of high-grade automobile finish, high-grade engineering plastics, resin, fiber products and the like. While pigment yellow 12, pigment yellow 13, pigment yellow 83 in the benzidine yellow pigments are the three pigments most commonly used in the organic pigment yellow series.
The molecular structural formula of pigment yellow 13 is as follows:
Figure BDA0002538536270000011
the dosage forms of the variety have 135 brands. Compared with pigment yellow 12, the modified pigment yellow has better solvent resistance and crystallization resistance and excellent migration resistance, accords with the color tone of printing ink, and is more adopted in Europe, such as pigment yellow 127 and pigment yellow 176. The strength is 25% higher under the same specific surface area and particle size; recrystallization is not easy to occur in ball milling, and the light fastness of the same depth is 1-2 grade higher than that of pigment yellow 12; the dosage form has high transparency, translucency and high nontransparent type, such as I rga l ite yellow BKW with the specific surface area of 10m 2/g. A large amount of the product is used for packaging printing ink, glazing resistant paint and sterilization treatment; the dye is used for coloring plastics, the migration resistance is good in soft PVC, the light fastness is grade 6-7, and the dye is limited to be used below 200 ℃ in HDPE due to the thermal cracking effect of the dye, and is only 0.12%.
The prior literature reports methods for synthesizing pigment yellow 13: adding 30% hydrochloric acid into a diazo kettle, adding dichlorobenzidine, pulping and dissolving, adding water for dilution, adding ice for cooling, adding sodium nitrite for diazotization, adding diatomite or active carbon for decoloration after diazotization is finished, and filtering to obtain diazo liquid containing diazonium salt. Adding water, liquid alkali and 2, 4-dimethyl-N-acetoacetanilide into a coupling kettle, stirring for dissolving, then adding hydrochloric acid or acetic acid, carrying out acid precipitation, adding sodium acetate, then cooling, adding diazo liquid, after coupling is finished, adding liquid alkali for adjusting the pH value, then heating, adding rosin and calcium chloride, and after reaction is finished, filtering and washing to obtain pigment yellow 13. The pigment yellow 13 obtained by the method has the advantages of good product quality, high cost, large dissolved and separated wastewater amount and high wastewater COD.
SUMMERY OF THE UTILITY MODEL
The utility model provides a yellow 13's of pigment synthesizer solves the technical problem who how to optimize yellow 13's of pigment synthesizer, makes its easy operation, and is of high quality, and the waste water volume is few.
The pigment yellow 13 synthesis equipment comprises a sodium nitrite dissolution kettle, a hydrochloric acid metering tank, a sodium nitrite solution metering tank, a diazo kettle, a first centrifugal pump, a tubular filter, a particle dry ice manufacturing machine, an acetoacetanilide pulping kettle, an emulsion pump, a coupling kettle, a liquid alkali metering tank, a magnetic filter barrel, a second centrifugal pump and a dark flow diaphragm filter press; the sodium nitrite dissolving kettle is communicated with the inner cavity of the diazo kettle through a first centrifugal pump and a sodium nitrite solution metering tank in sequence; the hydrochloric acid metering tank is communicated with the inner cavity of the diazo kettle; the diazo kettle is communicated with the inner cavity of the coupling kettle through a first centrifugal pump and a tubular filter in sequence; the particle dry ice manufacturing machine is provided with two branch channels, wherein one branch channel is communicated with the inner cavity of the diazo kettle, and the other branch channel is communicated with the inner cavity of the coupling kettle; the liquid caustic soda metering tank and the acetacetanilide pulping kettle are respectively communicated with the inner cavity of the coupling kettle; and a liquid outlet of the coupling kettle is communicated with the magnetic filter barrel, the second centrifugal pump and the undercurrent diaphragm filter press in sequence.
The tubular filter is filled with diatomite or active carbon.
The dark current diaphragm filter press is a dark current plate and frame filter press.
The first centrifugal pump and the second centrifugal pump are both fluoroplastic centrifugal pumps.
And the sodium nitrite dissolving kettle, the diazo kettle, the acetanilide pulping kettle and the coupling kettle are all provided with feed ports.
The branch channel is open.
The utility model has the advantages that:
1. the dry ice is used for refrigeration, so that the cost is low, the refrigeration effect is good, and the waste water is less.
2. And the tubular filter is adopted, so that the equipment investment is reduced, and the operation flow is reduced.
3. The acetoacetanilide is pulped and emulsified, so that the investment of other raw materials is reduced, and the cost is reduced.
4. The magnetic filter is adopted to remove iron, the operation is convenient, and the product quality is improved.
In conclusion, the process flow and the equipment are simple to operate, the product quality is good, the cost is low, and the quantity of three wastes is small.
Drawings
Fig. 1 is a schematic structural diagram of the present invention;
in the figure, 1, a diazo kettle, 2, a hydrochloric acid metering tank, 3, a sodium nitrite solution metering tank, 4, a sodium nitrite dissolving kettle, 5, a first centrifugal pump, 6, a tubular filter, 7, a particle dry ice manufacturing machine, 8, a blind flow membrane filter press, 9, an acetoacetanilide pulping kettle, 10, an emulsifying pump, 11, a coupling kettle, 12, a liquid alkali metering tank, 13, a magnetic filter barrel and 14, a second centrifugal pump are arranged.
Detailed Description
Referring to fig. 1, the pigment yellow 13 synthesis equipment in the figure comprises a diazo kettle 1, a hydrochloric acid metering tank 2, a sodium nitrite solution metering tank 3, a sodium nitrite dissolving kettle 4, a first centrifugal pump 5, a tubular filter 6, a particle dry ice manufacturing machine 7, an acetoacetanilide pulping kettle 9, an emulsification pump 10, a coupling kettle 11, a liquid caustic soda metering tank 12, a magnetic filter barrel 13, a second centrifugal pump 14 and a dark flow membrane filter press 8. The components are all existing components, the innovation point of the scheme is that the design of product production is completed by the connection relation of the components, corresponding valves are designed among the components, and the existing conventional components such as a material conveying pump are added according to needs.
The connection relation of the components is as follows: the sodium nitrite dissolving kettle 4 forms a material circulation relationship with the inner cavity of the diazo kettle 1 through a first centrifugal pump 5, a sodium nitrite solution metering tank 3 and a pipeline in sequence, so that the sodium sulfite solution is led into the diazo kettle 1 according to a specific amount; the hydrochloric acid metering tank 2 and the inner cavity of the diazo kettle 1 form a material circulation relationship by using a pipeline, so that the hydrochloric acid solution is introduced into the diazo kettle 1 according to a specific amount; the diazotization reaction of the sodium nitrite solution and the hydrochloric acid solution is carried out in a diazotization kettle 1 to form the 3,3' -dichlorobenzidine solution.
The bottom of the diazotization kettle 1 forms a material flow relationship with the inner cavity of the coupling kettle 11 through a first centrifugal pump 5, a tubular filter 6 and a pipeline in sequence, so that a diazonium salt solution formed by diazotization in the diazotization kettle 1, namely a 3,3' -dichlorobenzidine solution, is introduced into the coupling kettle 11 to wait for the coupling reaction with the 2, 4-dimethyl-N-acetoacetanilide to form pigment yellow 13.
The dry ice outlet of the granular dry ice making machine 7 is provided with two branch channels, wherein one branch channel is communicated with the inner cavity of the diazo kettle 1, and the other branch channel is communicated with the inner cavity of the coupling kettle 11; the branch channel adopts a non-closed structure with an opening, such as a groove-shaped structure, so that the danger caused by the expansion of the gasified volume of the dry ice is avoided or the pipe diameter of the branch channel is designed to be a safe size. The liquid caustic soda metering tank 12, the acetacetanilide pulping kettle 9 and the inner cavity of the coupling kettle 22 form a material circulation relationship by using pipelines respectively; the liquid outlet of the coupling kettle 22 sequentially passes through the magnetic filter barrel 13, the second centrifugal pump 14 and the undercurrent membrane filter press 8 to form a material circulation relationship by using pipelines, so that the filter press for the pigment yellow 13 is formed.
In practical application, the tubular filter 6 is filled with diatomite or activated carbon, the blind flow diaphragm filter press 8 is a blind flow plate-and-frame filter press, the first centrifugal pump 5 and the second centrifugal pump 14 are both fluoroplastic centrifugal pumps, and the sodium nitrite dissolution kettle 4, the diazo kettle 1, the acetoacetanilide pulping kettle 9 and the coupling kettle 11 are respectively provided with corresponding material feeding ports.
Understanding the above connection relationships, such as communication or connection, will be understood by those skilled in the art from the description of the embodiment and the representation in fig. 1, and the embodiment expressed by the present idea will be clearly understood by those skilled in the art from the description of the embodiment and the representation in fig. 1.
The reaction equation of the scheme is as follows:
1. diazotization:
Figure BDA0002538536270000051
wherein,
Figure BDA0002538536270000052
is the bis-chloro-benzidine, and the compound is the bis-chloro-benzidine,
Figure BDA0002538536270000053
is 3,3' -dichlorobenzidine.
2. Coupling:
Figure BDA0002538536270000054
wherein,
Figure BDA0002538536270000055
is 2, 4-dimethyl-N-acetoacetanilide,
Figure BDA0002538536270000056
pigment yellow 13.
The operation process and principle of the scheme are as follows:
300kg of water and 150.5kg of sodium nitrite are added to a sodium nitrite dissolution kettle 4, stirred to be fully dissolved, and pumped to a sodium nitrite solution metering tank 3 by a pump for standby. The granulated dry ice maker 7 prepares dry ice for use. Adding 3000kg of water into a diazo kettle 1, adding 600kg of hydrochloric acid from a hydrochloric acid metering tank 2, starting stirring, adding 275kg of dichlorobenzidine, beating and stirring, dissolving, then adding dry ice into a granular dry ice manufacturing machine 7, cooling to-5-0 ℃, quickly adding a sodium nitrite solution into a sodium nitrite solution metering tank 3 for diazotization, controlling the reaction temperature to be below 3 ℃ by adding dry ice in the granular dry ice manufacturing machine 7 during the reaction, and reacting for 0.75-1.5h until potassium iodide starch test paper is bluish.
4000kg of water and 2kg of EDTA (ethylene diamine tetraacetic acid) are added into an acetoacetanilide pulping kettle 9, stirring is started, 434kg of 2, 4-dimethyl-N-acetoacetanilide is added, the mixture is pulped for 2 hours, then a coupled liquid emulsion pump is added into a coupling kettle through an emulsion pump 10, stirring is started, the volume is adjusted to 8000L, dry ice is added into the tank 8, the temperature is reduced to 8-10 ℃, a pigment yellow 13 is obtained by coupling the diazo pump into the coupling kettle 11 through a first centrifugal pump-5 and a tubular filter 6, 30kg of 30% liquid caustic soda is dropped into a liquid caustic soda metering tank 12 after the diazo liquid is added, the pH value of the solution is adjusted to 3.5-4, stirring is carried out for 0.5-1 hour, 60kg of rosin and 30kg of anhydrous calcium chloride are added after the temperature is increased to 50 ℃, the temperature is increased to 55-60 ℃ after the diazo liquid is added, the reaction is finished at the temperature for 1.5-2.5 hours, the reaction was complete. And then iron is removed through a magnetic filter barrel 13, and then the mixture is pressed to a dark current membrane filter press 15 through a second centrifugal pump 14, pressed to be dry and washed to be neutral, so that the modified pigment yellow 13 is obtained.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the above description, in combination with the drawings in the embodiments of the present invention, clearly and completely describes the technical solutions in the embodiments of the present invention, and obviously, the described embodiments are some embodiments of the present invention, not all embodiments. The components of embodiments of the present invention, as generally described and illustrated in the figures herein, may be arranged and designed in a wide variety of different configurations.
Thus, the above detailed description of the embodiments of the invention provided in the accompanying drawings is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative efforts belong to the protection scope of the present invention.

Claims (6)

1. Pigment yellow 13's synthesis equipment, its characterized in that: the device comprises a sodium nitrite dissolving kettle, a hydrochloric acid metering tank, a sodium nitrite solution metering tank, a diazo kettle, a first centrifugal pump, a tubular filter, a particle dry ice manufacturing machine, an acetoacetanilide pulping kettle, an emulsifying pump, a coupling kettle, a liquid alkali metering tank, a magnetic filter barrel, a second centrifugal pump and a undercurrent diaphragm filter press; the sodium nitrite dissolving kettle is communicated with the inner cavity of the diazo kettle through a first centrifugal pump and a sodium nitrite solution metering tank in sequence; the hydrochloric acid metering tank is communicated with the inner cavity of the diazo kettle; the diazo kettle is communicated with the inner cavity of the coupling kettle through a first centrifugal pump and a tubular filter in sequence; the particle dry ice manufacturing machine is provided with two branch channels, wherein one branch channel is communicated with the inner cavity of the diazo kettle, and the other branch channel is communicated with the inner cavity of the coupling kettle; the liquid caustic soda metering tank and the acetacetanilide pulping kettle are respectively communicated with the inner cavity of the coupling kettle; and a liquid outlet of the coupling kettle is communicated with the magnetic filter barrel, the second centrifugal pump and the undercurrent diaphragm filter press in sequence.
2. A pigment yellow 13 synthesis plant according to claim 1, characterized in that: the tubular filter is filled with diatomite or active carbon.
3. A pigment yellow 13 synthesis plant according to claim 1, characterized in that: the dark current diaphragm filter press is a dark current plate and frame filter press.
4. A pigment yellow 13 synthesis plant according to claim 1, characterized in that: the first centrifugal pump and the second centrifugal pump are both fluoroplastic centrifugal pumps.
5. A pigment yellow 13 synthesis plant according to claim 1, characterized in that: and the sodium nitrite dissolving kettle, the diazo kettle, the acetanilide pulping kettle and the coupling kettle are all provided with feed ports.
6. A pigment yellow 13 synthesis plant according to claim 1, characterized in that: the branch channel is open.
CN202021091137.XU 2020-06-15 2020-06-15 Pigment yellow 13 synthesis equipment Active CN212864625U (en)

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Application Number Priority Date Filing Date Title
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