Environment-friendly preparation method of toluylene-based biphenyl type fluorescent brightener

A fluorescent whitening agent and biphenyl-based technology, which is applied in the direction of styrene-based dyes, etc., can solve the problems of difficult handling and large environmental pollution, and achieve the effects of convenient source, low cost, and avoiding waste of heat.

Inactive Publication Date: 2013-02-06
山西青山化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The present invention provides an environmentally friendly preparation method of a distyryl biphenyl type fluorescent whitening agent in order to solve the problems of large environmental pollution and difficult treatment in the prior art

Method used

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  • Environment-friendly preparation method of toluylene-based biphenyl type fluorescent brightener

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Arbuzov reaction: In a dry 300mL reaction kettle, add 45.5g of biphenyl dichlorobenzyl, 60.0g of triethyl phosphite, in N 2 Slowly raise the temperature to 120-125°C within 2-3 hours under the protection of the environment, keep it warm for 4 hours, add 30.0g of triethyl phosphite, then continue to heat up to 145-155°C, keep it warm for 2 hours, add 10.0g of triethyl phosphite , reflux reaction at this temperature for 6-8 hours, stop the reaction, distill under reduced pressure, distill off excess triethyl phosphite and some by-products, lower the temperature to 40°C, and obtain a pale yellow solid ester;

[0041] Condensation reaction: In a dry 500ml reactor, add 200.0g DMF, 31.5g esterified product and 52.5g o-sulfonate sodium benzaldehyde in sequence, start stirring for 0.5 hours to basically dissolve the materials, and then control the temperature between 20-30°C , add 52.0g of sodium methoxide solution dropwise within about 4 hours, then slowly raise the temperatur...

Embodiment 2

[0045] Arbuzov reaction: In a dry 300mL reaction kettle, add 45.5g of biphenyl benzyl dichloride and 50.0g of triethyl phosphite, in N 2 Slowly raise the temperature to 120-125°C within 2-3 hours under the protection of the environment, keep it warm for 4 hours, add 40.0g of triethyl phosphite, then continue to heat up to 145-155°C, keep it warm for 2 hours, add 15.0g of triethyl phosphite , Reflux reaction at this temperature for 6-8 hours, and all the other operations are the same as in Example 1.

[0046] Condensation reaction and aftertreatment are with embodiment 1.

Embodiment 3

[0048] Arbuzov reaction: In a dry 300mL reaction kettle, add 45.5g of biphenyl dichlorobenzyl, 70.0g of triethyl phosphite, in N 2 Slowly raise the temperature to 120-125°C within 2-3 hours under the protection of the environment, keep it warm for 4 hours, add 20.0g of triethyl phosphite, then continue to heat up to 145-155°C, keep it warm for 2 hours, add 20.0g of triethyl phosphite , Reflux reaction at this temperature for 6-8 hours, and all the other operations are the same as in Example 1.

[0049] Condensation reaction and aftertreatment are with embodiment 1.

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Abstract

The invention discloses an environment-friendly preparation method of toluylene-based biphenyl type fluorescent brightener, which belongs to the field of a preparation technique of high-grade fluorescent brightener used for washing powder, detergent, cosmetic and the like, and solves the problems of great pollution to the environment and difficulty in disposal in the prior art. The method comprises the steps of: heating and refluxing 4, 4'-bis(chloromethyl)-1, 1'-biphenyl and triethyl phosphite under the condition of N2, distilling to remove a part of triethyl phosphite and side products through vacuum distillation, condensing, and crushing to obtain an esterified product; reacting the esterified product and benzaldehyde-2-sulfonic acid sodium for 2-15 hours in a strong polar aprotic organic solvent and under the action of organic strong base to obtain a condensate; distilling the condensate, recycling the solvent, and recycling tail gases to obtain a condensed mixture; adding water and salt into the condensed mixture, cooling, performing pressure-filtering to obtain a salting-out filter cake, washing, and refining; and drying the refined cake to obtain the toluylene-based biphenyl type fluorescent brightener. According to the method provided by the invention, the recycling is convenient and the brightener can be used circularly; the problem of environmental pollution is solved and energy is saving and the environment is protected; and the used raw materials is convenient in source and low in cost.

Description

technical field [0001] The invention belongs to the technical field of preparation of high-grade fluorescent whitening agents used in washing powder, detergent, cosmetics, etc., and in particular relates to an environmentally friendly preparation method of a distyryl biphenyl type fluorescent whitening agent. Background technique [0002] Distyryl biphenyl fluorescent whitening agent, because of its good water solubility, has a good whitening effect on cotton fabrics, polyester fibers, protein fibers, acetate fibers, etc., and is also an excellent detergent, laundry detergent, cosmetics Such as whitening additives, are widely used. At present, the most widely used product at home and abroad is CBS-X. [0003] Patent CN 98107403.0 discloses a method for preparing fluorescent whitening agent CBS-X. The method uses biphenyl as raw material, first prepares 4,4-diiodobiphenyl, and then reacts with 2-styrenesulfonic acid to obtain CBS-X . This method effectively avoids the prod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B23/14
Inventor 高飞王运科谌孟晴
Owner 山西青山化工有限公司
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