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A kind of black pigment and its preparation method and application

A technology of black pigments and pigments, applied in the field of black pigments and their preparation, can solve the problems of easy detachment, small space structure, and failure to meet the requirements of use

Active Publication Date: 2020-09-08
湖州市聚立新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Nigrosine No. 1 has effects that other black pigments such as carbon black cannot achieve in many applications. However, dichromate is usually used as an initiator in the synthesis process, and a large amount of chromium-containing wastewater is difficult to dispose of during the production process. Water and soil are seriously polluted, and the product structure also contains a large amount of chromium (hexavalent chromium). The mass percentage of chromium is more than 20%, which brings great health risks to the human body, so it is restricted in many occasions.
[0005] In the current method of preparing nigrosine without dichromate, persulfate, chlorate, hydrogen peroxide or other oxidizing agents will be used. During the polymerization process, chloride ions are paired on the molecular chain in the form of counter anions (with amino and imino effect), due to the small spatial structure of chloride ions, the hydrogen bond between molecules is strengthened, the molecular chain becomes stiff, and the particles are easy to reunite. In addition, chlorine is also structurally unstable and easy to come out
If the chloride ions are not removed, only a dark green product is obtained, which is agglomerated in large quantities and cannot be dispersed, and cannot be used as a pigment; after the chloride ions are removed, the intermolecular hydrogen bonding weakens and becomes easy to disperse. However, due to the loss of protons on the nitrogen atom, the conjugation effect of the entire molecular chain is weakened, and the absorption capacity of visible light is reduced. The blackness value of the obtained product is not high, and the hue is brown. Requirements

Method used

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  • A kind of black pigment and its preparation method and application
  • A kind of black pigment and its preparation method and application
  • A kind of black pigment and its preparation method and application

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preparation example Construction

[0033] The preparation method of organic black pigment provided by the present invention includes the steps:

[0034] The first step is to mix the acid-containing aqueous solution, aniline, catalyst and aluminum salt to obtain solution 1;

[0035] In the second step, the solution 1 is mixed with an aqueous solution containing an oxidant, and the organic black pigment provided by the invention is obtained by oxidative polymerization.

[0036] In one embodiment of the present invention, the above-mentioned first step is to add aniline to the acid-containing aqueous solution to obtain an aniline salt mixture and then mix with the catalyst and the aluminum salt.

[0037] In one embodiment of the present invention, the above-mentioned first step is to add aniline to the acid-containing aqueous solution to obtain an aniline salt mixture, then add the catalyst, and then add the aluminum salt, and mix until all is dissolved.

[0038] In the above first step, the acid can be an inorganic acid or...

Embodiment 1

[0056] Preparation of organic black pigment 1

[0057] Add 15g (0.15mol) of 36% hydrochloric acid and 3g (0.03mol) of 98% sulfuric acid to 150ml of aqueous solution, then add 14g (0.15mol) of aniline, stir at room temperature for 20 minutes, and then add 1g of ferrous chloride ( 0.005mol), 4g (0.017mol) of aluminum chloride, after all dissolved, at 30°C, add 80g (0.3mol) of 40% sodium chlorate aqueous solution at a time, stir and react at 70°C for 3 hours, and the reaction is complete. After the reaction, the reaction solution was filtered and washed with water. The resulting filter cake was dispersed with 300 ml of water, neutralized to pH 7.5 with ammonia, and then filtered and washed with water. The filter cake was dried at 120°C and pulverized to obtain the organic Black pigment 1.

[0058] The obtained organic black pigment 1 was subjected to elemental analysis and infrared analysis to confirm the change in the aluminum content and characteristic peaks. See the result figure...

Embodiment 2

[0060] Preparation of organic black pigment 2

[0061] Add 15g (0.15mol) of 36% hydrochloric acid and 3g (0.03mol) of 98% sulfuric acid to 150ml of aqueous solution, then add 14g (0.15mol) of aniline, stir at room temperature for 20 minutes, and then add 1g of ferrous chloride ( 0.005mol), 8g (0.033mol) of aluminum chloride, after all is dissolved, at 30°C, add 80g (0.3mol) of 40% sodium chlorate aqueous solution at a time, stir and react at 70°C for 3 hours, and the reaction is complete. After the reaction, the reaction solution was filtered and washed with water. The resulting filter cake was dispersed with 300 ml of water, neutralized to pH 7.5 with ammonia, and then filtered and washed with water. The filter cake was dried at 120°C and pulverized to obtain the organic Black pigment 2.

[0062] The obtained organic black pigment 2 was subjected to elemental analysis and infrared analysis to confirm changes in the aluminum content and characteristic peaks. See the result figur...

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Abstract

The invention discloses a black pigment as well as a preparation method and application thereof. The pigment contains no heavy metal element chromium and contains aluminum, wherein the content of thealuminum element is 0.5-20 wt% in terms of the total weight of the pigment.

Description

Technical field [0001] The invention relates to organic pigments, in particular to a black pigment using aniline as a raw material and a preparation method and application thereof. Background technique [0002] Pigments or dyes synthesized with aniline as the main raw material are usually called aniline black (ANILINE BLACK). The aniline black involved in the present invention is an aniline polymer and belongs to organic pigments. One of them is usually called "aniline black No. 1" "(Chinese name: cl pigment black 1, English name: ANILINE BLACK, cas accession number: 13007-86-8, molecular formula is C 66 H 51 N 11 Cr 3 O 12 The structural formula is shown in the following formula II), which is a pigment containing hexavalent chromium, which can also be called "chromium-containing aniline black", which has a very high blackness and a very blue hue. [0003] [0004] Nigrosine No. 1 has effects that carbon black and other black pigments cannot achieve in many applications. However, d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09B17/02C09B67/20
CPCC09B17/02C09B67/0065
Inventor 史利斌
Owner 湖州市聚立新材料科技有限公司