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Aniline black and resin composition, aqueous dispersion, and solvent dispersion using said aniline black

A nigrosine and dispersion technology, applied in the field of nigrosine, can solve the problems of low volume impedance value, reduced charge retention ability, and high volume impedance value, and achieve the effects of excellent dispersibility, high impedance value and excellent blackness.

Active Publication Date: 2013-09-11
TODA IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the dispersion of carbon black in the binder resin is difficult, and the volume resistance value is also low. Therefore, in the case of the former, there is a problem that the charging performance of the developer is hindered (the charging retention ability is reduced).
In the latter case, it is difficult to provide dispersion stability of carbon black in the dispersion liquid, so the fluidity is poor, and there is a problem that the volume resistance value of the resist film is low
[0009] In general, it is known that aniline black has a higher volume resistivity value than inorganic black pigments such as carbon black, and studies on the application of aniline black have been conducted in order to overcome the above-mentioned problems.

Method used

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  • Aniline black and resin composition, aqueous dispersion, and solvent dispersion using said aniline black
  • Aniline black and resin composition, aqueous dispersion, and solvent dispersion using said aniline black
  • Aniline black and resin composition, aqueous dispersion, and solvent dispersion using said aniline black

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0139] Add 30g (0.32mol) of aniline to 33.8g (0.33mol) of 35% hydrochloric acid and 1250ml of water, stir and mix at a liquid temperature of 60°C, and add 15.0g (0.086mol) of 4-hydroxybenzenesulfonic acid to dissolve it uniformly , add dropwise a solution of 4.6g (0.0363mol) of ferrous chloride dissolved in 70ml of water and 78.0g (0.69mol) of 30% hydrogen peroxide over 2 hours, then stir and mix at a liquid temperature of 60°C for 1 hour, and the reaction is completed . After the reaction, the reaction solution was filtered and washed with water, and the obtained filter cake was dispersed again with 1000 ml of water, neutralized to pH6.5 with 10% sodium hydroxide, and after the pH was stable, filtered and washed with water, the paste Drying at 60° C. yielded nigrosine (black pigment-1).

[0140] For the obtained nigrosine, carry out FT-IR measurement by KBr tablet method, at 1070~1030cm -1 There was a peak nearby, and the presence of a sulfo group was confirmed.

Embodiment 2～4

[0142] In addition to various changes to the amount of water, the type and amount of acid to be added, the type and amount of catalyst to be added, and the method of addition, the type and amount of oxidant to be added, and the method of addition, reaction temperature and aging time, and neutralization pH, the same as the above implementation Example 1 was operated in the same manner to obtain nigrosine.

[0143] The production conditions at this time are shown in Table 1, and various characteristics of the obtained nigrosine are shown in Table 2.

[0144] The nigrosine black that embodiment 2~4 obtains, carries out FT-IR measurement by KBr tablet method, at 1070~1030cm -1 There was a peak nearby, and the presence of a sulfo group was confirmed.

Embodiment 5

[0163] 1.5 g of nigrosine obtained in Example 1 and 48.5 g of polyvinyl chloride resin powder 103EP8D (Zeon Corporation) were weighed, put into a 100 cc polyethylene beaker, and mixed well with a spatula to obtain a mixed powder.

[0164] Add 0.5g of calcium stearate to the obtained mixed powder and mix, set the gap of the hot roller heated to 160°C to 0.2mm, knead the above mixed powder in the roller little by little, and continue kneading The resin composition was peeled off from the roll until the resin composition was integrated, and used as a raw material for a colored resin sheet.

[0165] Next, the above-mentioned resin composition was sandwiched between surface-ground stainless steel plates, placed in a hot press heated to 180°C, and heated at 1 ton / cm 2 The pressure was press-molded to obtain a colored resin sheet with a thickness of 1 mm.

[0166] The obtained colored resin sheet had an L* value of 7.2 and a dispersion state of 5.

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Abstract

Provided are: an aniline black that contains no harmful substances such as chromium or copper, exhibits an excellent black color, and has a high resistance; and a black resin composition, aqueous dispersion, and solvent dispersion that are colored with said aniline black and exhibit high dispersivity. The sulfur content of this aniline black is 0.2% to 6.0% by weight, and the average major-axis length of the primary particles of said aniline black is 0.05 to 0.80 [mu]m.

Description

technical field [0001] The present invention provides nigrosine containing sulfur derived from a sulfo group and having excellent blackness. [0002] The present invention also provides a resin composition having excellent dispersibility and an aqueous or solvent-based dispersion colored by the nigrosine. Background technique [0003] Aniline black is a black dye and pigment obtained by oxidative condensation of aromatic amines such as aniline, toluidine, and phenylenediamine. , printing inks, drawing tools, poster colors, plastics, thermal transfer inks, etc. As the oxidizing agent used in the production of nigrosine, the method of using dichromate is most suitable. [0004] However, the chromium ion contained in dichromate is an extremely harmful pollution substance to the human body (although it is now confirmed that the chromium contained in nigrosine is coordinated with the pigment, does not contain harmful hexavalent chromium, and is safe) , and copper ions derived ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B17/02C08K5/34C08L101/00C09B67/46C09B67/48C09D11/00C08L79/02
CPCC09D5/028C09D11/037C09D11/322C09B67/0086C09B67/009C09B68/22C08K5/0041C09D7/67C09D7/68Y10T428/2982C08K5/3465C09D11/00C08L79/02C08L101/00C09D11/328
Inventor 下畑祐介上原高平志茂伸哉青木功荘
Owner TODA IND
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