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Production system and process method for continuously synthesizing bisazo pigment

A production system, bisazo technology, applied in chemical instruments and methods, azo dyes, organic dyes, etc., can solve problems such as unsuitable azo pigments, no process parameters, and no structural parameters of microchannel reactors

Active Publication Date: 2020-07-07
SHENYANG RES INST OF CHEM IND +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to the sensitivity of the coupling reaction to pH changes, if the pH change is not well controlled during the two-step coupling reaction, side reactions are prone to occur, such as the self-coupling reaction of diazonium salts to generate monocouples. Precipitation and coating of nitrogen compounds, etc., these situations will have a great impact on the quality of pigments
[0004] The traditional batch method for synthesizing disazo pigments, due to factors such as uneven heat and mass transfer in the batch reactor, will lead to the decomposition of diazonium salts and self-coupling reactions, which will cause the particle size of the pigment particles to increase. Wider particle size distribution, lower pigment yield and quality, will also lead to large differences in shade and intensity between batches of pigments produced
And according to the batch synthesis method of azo pigment yellow 14 disclosed by Chinese patent (CN106752254A), it can be seen that the reaction time used by the method of batch synthesis needs at least 2 hours, and the change of the pH of the coupling reaction system needs to be monitored at any time. Greatly reduced production efficiency
Regarding the continuous synthesis of azo pigments, related reports include: (1) Yang Lintao, Shenyang Chemical Industry Research Institute, etc., used binary mixing microchannel and ternary mixing microchannel reactors to carry out continuous synthesis of azo pigments (dyeing and Dyeing, Vol. 54 No. 2, April 2017) However, the process given in the report is the process of feeding two reaction liquids, and there are no specific process parameters, nor does it involve specific microchannel reactors Structural parameters
(2) Chinese invention patent (CN104479394A) discloses a method for the continuous synthesis of azo pigments in a branched spiral tube, utilizing the efficient mixing effect of the secondary flow of the spiral tube to strengthen the coupling reaction, but there is no The synthesis process of disazo pigments is specifically mentioned, and the branched helical tube reactor still cannot solve the problem of difficult pH control in the production process of disazo pigments, so this reactor is not suitable for disazo pigments with high requirements for color light continuous synthesis of
(3) Chinese invention patent (CN102618063B) discloses a reactor with a scaling helical structure for the continuous synthesis of azo dyes, but this structure is not suitable for the synthesis of azo pigments because the pigments will deposit in the scaling structure, clogged pipe
The above structure is more suitable for the synthesis process of products with low viscosity, such as the preparation of inorganic nanoparticles, but it is not suitable for the synthesis process of pigments, because the existence of structures such as collection chambers will lead to the deposition of reactants and pigments, and block the pipeline
And if the reactor is used in the synthesis process of disazo pigments, the problem of pH regulation in the reaction process cannot be solved, and it will still lead to poor shade, transparency and strength of disazo pigment products.
[0006] Based on the above research progress, it can be seen that there is still no specific microreactor device and process route for the continuous synthesis of disazo pigments in microreactors to achieve continuous synthesis of high transparency and high strength disazo pigments.

Method used

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  • Production system and process method for continuously synthesizing bisazo pigment
  • Production system and process method for continuously synthesizing bisazo pigment
  • Production system and process method for continuously synthesizing bisazo pigment

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Embodiment 1

[0049] Such as Figure 1-8 Shown, the present invention includes continuous diazotization device and continuous coupling reaction device, wherein such as figure 1 As shown, the continuous diazotization device includes a sodium nitrite solution storage tank 1, a water storage tank 2, a slurry storage tank 3, a high-pressure tank 7, a membrane dispersion microreactor 8, a first delay tube 9 and a diazonium salt solution Storage tank 10, wherein film dispersion microreactor 8 is provided with dispersed phase fluid inlet pipe 81, continuous phase fluid inlet pipe 82 and mixed solution outlet pipe 83, sodium nitrite solution storage tank 1 passes through the first nitriding pipeline 11 and The dispersed phase fluid inlet pipe 81 is connected, and the first nitriding pipeline 11 is provided with the first nitriding input pump 4, and the high pressure tank 7 is provided with an elastic sealing sheet 701, and the water storage tank 2 The second nitriding pipeline 12 is connected to t...

Embodiment 2

[0059] When the above system is working, the liquid in the slurry storage tank 3 is preferentially flowed into the lower part of the high-pressure tank 7 by using the third nitriding input pump 6, and the input is stopped after the high-pressure tank 7 is filled, and the solution in the sodium nitrite solution storage tank 1 passes through the first The nitriding pipeline 11 flows into the dispersed phase fluid inlet pipe 81, and flows into the diazotization microchannel 851 of the continuous diazotization device after passing through the porous dispersion membrane 84, and the water in the water storage tank 2 passes through the second nitriding input pump 5 enters the upper part of the high-pressure tank 7, and the slurry is pressed into the membrane dispersion microreactor 8 through the sealing sheet 701 in the high-pressure tank 7, and then flows into the diazotization microchannel 851 through the continuous phase fluid inlet pipe 82, the After the reaction of the solution i...

Embodiment 3

[0068] (1) At room temperature (25°C), take 17.25g of 3,3'-dichlorobenzidine hydrochloride (DCB hydrochloride) in a 500mL beaker, add 17.75g of concentrated hydrochloric acid (37%), and 250mL of deionized water, stirring to obtain a uniform DCB hydrochloride slurry; take 7.11g of sodium nitrite solid in a 500mL beaker, add 250mL of deionized water, and stir until the sodium nitrite solid is completely dissolved to obtain a sodium nitrite solution;

[0069] (2) Under the ice water bath of 0-4 ℃, adopt the 3rd nitriding input pump 6 (peristaltic pump) to squeeze all DCB hydrochloride slurry into the high-pressure tank 7, then use the 2nd nitriding input pump 5 (advection pump) ) and high-pressure tank 7 to control the flow of DCB hydrochloride slurry to be 30ml / min, and to control the flow of sodium nitrite solution with the first nitriding input pump 4 (advection pump) to be 30ml / min, and the two solutions are micro-reacted in the membrane dispersion The mixing reaction was car...

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Abstract

The invention belongs to the field of pigment synthesis, and particularly relates to a production system and a process method for continuously synthesizing a bisazo pigment. The method comprises the following steps: carrying out diazotization reaction on a hydrochloric acid solution of a diazo component and a sodium nitrite solution in a membrane dispersion microreactor to prepare a diazonium saltsolution A; preparing a coupling component solution B from a coupling component and sodium hydroxide; preparing acetic acid and sodium acetate into a buffer solution C with the pH value of 4.3; and simultaneously introducing the solution A, the solution B and the solution C into a double-sided microporous dispersion microreactor according to a certain flow ratio, carrying out a coupling reactionto generate a bisazo pigment crude product, and further treating the crude product to obtain the azo pigment product. The continuous diazotization reaction is realized by adopting the membrane dispersion microreactor, the continuous coupling reaction is realized by adopting the double-sided microporous dispersion reactor, and the continuous synthesis of the bisazo pigment is realized through the two reactions. The invention has the advantages of simple process, short reaction period, easiness in temperature control and easiness in pH adjustment.

Description

technical field [0001] The invention belongs to the field of pigment synthesis, and in particular relates to a production system and a process method for continuously synthesizing disazo pigments. Background technique [0002] Azo pigments refer to a class of synthetic pigments containing azo groups in their molecules. They are the main category of organic pigments, accounting for about 40% of the total organic pigments. According to the number of azo groups contained in the pigment molecules, it can be divided into monoazo pigments and disazo pigments. Among them, disazo pigments are widely used in the fields of ink industry, high-grade automobile topcoat, advanced engineering plastics, resins and fiber products. It is a disazo pigment with great market influence and strong technical representativeness. Its continuous production technology It can be popularized and applied to the production of other disazo pigments. [0003] The production process of azo pigments mainly i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B33/153
CPCC09B33/153
Inventor 鄢冬茂徐建鸿刘东王法军周川黄晋培杨林涛胥维昌龚党生张学龙闫士杰刘冰
Owner SHENYANG RES INST OF CHEM IND
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