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Dicarboxylic acid heavy calcium carbonate powder fluorescent whitening agent as well as preparation method and application thereof

A technology of heavy calcium carbonate powder and fluorescent whitening agent, which is applied in the field of fluorescent whitening agent, can solve the problem of fluorescent whitening material lacking heavy calcium carbonate powder, etc., and achieves strong ultraviolet absorption performance and high bonding firmness. , the effect of good liquidity

Active Publication Date: 2017-04-26
HEZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] There are free calcium ions and hydroxyl groups on the surface of carbonic acid powder. It is difficult for the existing fluorescent whitening agent products on the market to effectively bond or adsorb on the surface of ions or groups on the powder, so they lack the ability to effectively whiten and brighten. Fluorescent whitening material of calcium carbonate powder

Method used

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  • Dicarboxylic acid heavy calcium carbonate powder fluorescent whitening agent as well as preparation method and application thereof
  • Dicarboxylic acid heavy calcium carbonate powder fluorescent whitening agent as well as preparation method and application thereof
  • Dicarboxylic acid heavy calcium carbonate powder fluorescent whitening agent as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Add 20mmol cyanuric chloride to 200mL ice water, ice bath. Then dropwise add a mixture of 10mmol 4,4'-diaminostilbene-2,2'-disulfonic acid (DSD acid) and 200mL distilled water (add an appropriate amount of 20mmol Na 2 CO 3 ), stirred at 0-5°C, and reacted for 2h. Heat up to 30~40℃, add 20mmol Na 2 CO 3 . Then, a mixture of 20 mmol of tetradecyl dimethyl tertiary amine and 10 mL of DMF was added dropwise, and the reaction was carried out under temperature control for 10 h. Heat up to 80-90°C, add 20mmol p-aminobenzoic acid, add dropwise 10% Na 2 CO 3 The solution maintains the pH of the system at 8-9, and the temperature is controlled for 8 hours. Cool to room temperature, add 60 g of sodium chloride, stir, filter with suction, and dry in vacuum to obtain dicarboxylic acid ground calcium carbonate powder fluorescent whitening agent with a yield of 92%.

Embodiment 2

[0036] Add 19mmol cyanuric chloride to 250mL ice water, ice bath. Then dropwise add a mixture of 11mmol 4,4'-diaminostilbene-2,2'-disulfonic acid (DSD acid) and 198mL distilled water (add an appropriate amount of 20mmol Na 2 CO 3 ), stirred at 0-5°C, and reacted for 2h. Heat up to 30~40℃, add 20mmol Na 2 CO 3 . Then, a mixture of 21 mmol of tetradecyl dimethyl tertiary amine and 9 mL of DMF was added dropwise, and the reaction was carried out under temperature control for 10 h. Raise the temperature to 80-90°C, add 22mmol p-aminobenzoic acid, add dropwise 10% Na 2 CO 3 The solution maintains the pH of the system at 8-9, and the temperature is controlled for 8 hours. Cool to room temperature, add 60 g of sodium chloride, stir, filter with suction, and dry in vacuum to obtain dicarboxylic acid ground calcium carbonate powder fluorescent whitening agent with a yield of 91%.

Embodiment 3

[0038] Add 21mmol cyanuric chloride to 225mL ice water, ice bath. Then add dropwise a mixture of 9mmol 4,4'-diaminostilbene-2,2'-disulfonic acid (DSD acid) and 205mL distilled water (add an appropriate amount of 20mmol Na 2 CO 3 ), stirred at 0-5°C, and reacted for 2h. Heat up to 30~40℃, add 20mmol Na 2 CO 3 . Then, a mixture of 18 mmol of tetradecyl dimethyl tertiary amine and 11 mL of DMF was added dropwise, and the reaction was carried out under temperature control for 10 h. Heat up to 80-90°C, add 19mmol p-aminobenzoic acid, drop 10% Na 2 CO 3 The solution maintains the pH of the system at 8-9, and the temperature is controlled for 8 hours. Cool to room temperature, add 60g of sodium chloride, stir, filter with suction, and vacuum-dry to obtain dicarboxylic acid ground calcium carbonate powder fluorescent whitening agent with a yield of 90%.

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Abstract

The invention provides a dicarboxylic acid heavy calcium carbonate powder fluorescent whitening agent. The dicarboxylic acid heavy calcium carbonate powder fluorescent whitening agent is characterized by having a structural formula 1 shown in the specification. The invention aims to provide the dicarboxylic acid heavy calcium carbonate powder fluorescent whitening agent as well as a preparation method and application thereof, the method is simple, the raw materials are low in price, and the process is green and environment-friendly. The heavy calcium carbonate powder treated by adopting the fluorescent whitening agent provided by the invention has relatively high whiteness and brightness, and relatively good fluidity and dispersity, so that the dicarboxylic acid heavy calcium carbonate powder fluorescent whitening agent is an excellent multifunctional fluorescent whitening agent.

Description

technical field [0001] The invention relates to the technical field of fluorescent whitening agents, in particular to a dicarboxylic acid heavy calcium carbonate powder fluorescent whitening agent and a preparation method and application thereof. Background technique [0002] In my country's "12th Five-Year" new material development plan, the development of new materials that are coordinated with resources and the environment is taken as the main assessment index, and the problem of resource shortage is solved through the development of new materials. my country has formed a relatively complete material science and technology system, and has obvious resource advantages and technological advantages in some new material fields, but the overall independent innovation capability is still relatively weak, and there are still relatively few new material products and technologies with independent intellectual property rights. Especially in terms of ground calcium carbonate powder fl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D251/70C09K11/06C09C1/02C09C3/08
CPCC01P2006/60C07D251/70C09C1/021C09C3/08C09K11/06C09K2211/1007C09K2211/1059
Inventor 万茂生画莉曾一文莫福旺
Owner HEZHOU UNIV
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