CN101429343A

CN101429343A - Process for producing fluorescent whitening agent 5BM

Info

Publication number: CN101429343A
Application number: CNA2008100800514A
Authority: CN
Inventors: 张成才; 李钢
Original assignee: SHANXI KINGSUN CHEMICAL CO Ltd
Current assignee: SHANXI KINGSUN CHEMICAL CO Ltd
Priority date: 2008-12-04
Filing date: 2008-12-04
Publication date: 2009-05-13

Abstract

The invention relates to a method for preparing a synthetic detergent and a ring whitening agent for printing industry, in particular to a method for preparing a fluorescent whitening agent 5BM. The method solves the problem that the product obtained through the prior method for processing and preparing the fluorescent whitening agent 5BM has low quality. The method comprises the following steps: cyanuric chloride and DSD acid are put into a reaction kettle and are added with ice water; the PH value of the mixture of the ice water, the cyanuric chloride and the DSD acid is regulated to between 1 and 1.5; the hydrochloric acid generated in the reaction is neutralized; the PH value is regulated to between 6 and 6.5; after the amido value of the DSD acid disappears, the hydrochloric acid is added with aniline; after the aniline disappears, N-methylethanolamine is added to the mixture; the PH value is finally regulated to between 10 and 12; the mixture is cooled to the temperature of 5 DEG C through the ice water so that a target product is precipitated out; and the target product is filtered, dried and pulverized to obtain the 5BM product.

Description

The preparation method of white dyes 5BM

Technical field

The present invention relates to the preparation method of the ring whitening agent that a kind of synthetic detergent and dyeing use, the preparation method of specifically a kind of white dyes 5BM.

Background technology

White dyes 5BM belongs to the two triazine structures of toluylene, molecular formula C ₃₈H ₃₈N ₁₂O ₈S ₂Na ₂,

Because of its superior performance, be widely used in industries such as papermaking, printing and dyeing, washing.The present 5BM that produces according to external solvent production method, exist triazine impurity (mainly to refer to 2-hydroxyl-4 always, 6-hexichol amido-s-triazine, 2-morpholinyl-4,6-hexichol amido-s-triazine and 2-anilino-4,6-dimorpholine base-s-triazine) shortcomings such as bigger are polluted in content and heavy metal content height, production, use; And amounts of triazine is low, the environment-friendly type that heavy metal content is low, the granule type 5BM that added value is high, and but because of the technical requirements height, domestic manufacturer can not produce at present, can't satisfy the demand of domestic and international market.

Summary of the invention

The low problem of product quality that the present invention obtains for the method that solves prior art processing and preparing white dyes 5BM and the preparation method of a kind of white dyes 5BM is provided.

The present invention is realized by following technical scheme, the preparation method of a kind of white dyes 5BM, step is: get cyanuric chloride and reactor is put in DSD acid, add frozen water, the pH value of re-adjustment frozen water, cyanuric chloride, DSD acid mixture is 1-1.5, the hydrochloric acid that generates of neutralization reaction then, regulating pH value is 6-6.5, treat that the amino value of DSD acid disappears after, adding aniline, treat to add the N-Mono Methyl Ethanol Amine after aniline disappears, adjusting the pH value at last is 10-12, makes target product with the frozen water cooling then, separates out, filtration, dry, pulverizing obtain the 5BM product.

Regulate the pH value of frozen water, cyanuric chloride, DSD acid mixture and use hydrochloric acid,

The hydrochloric acid that neutralization reaction generates can use carbonate, as yellow soda ash, and lime carbonate, magnesiumcarbonate etc.

Regulate last pH value and use NaOH.

More than provided concrete step, specifically how to have determined consumption aborning, then grasped flexibly according to producing needs, according to the structure of participating in reactive material, the concrete data of using in theory are as follows: (umber is the ratio of molar weight)

The preparation method of a kind of white dyes 5BM, step is: get 2 parts cyanuric chloride and 1 part DSD acid and put into reactor, add frozen water, the pH value of re-adjustment frozen water, cyanuric chloride, DSD acid mixture is 1-1.5, the hydrochloric acid that generates of neutralization reaction then, regulating pH value is 6-6.5, after treating that the amino value of DSD acid disappears, the aniline that adds 2 parts treats that aniline disappearance back adds 2 parts N-Mono Methyl Ethanol Amine, and adjusting the pH value at last is 10-12, be cooled to 5 ℃ with frozen water then and make target product, separate out, filtration, dry, pulverizing obtain the 5BM product.

The product that the technical scheme of putting down in writing according to the application obtains both can reduce because of producing and using the dust pollution that brings, and can make the cold water-dispersible of product improve 21.5% than like product again, met and exceeded the level of the expensive goods of western countries' requirement.

Advantage of the present invention is: do not have high-temperature high-pressure craft in the production process, trace heavy metals, iron and triazine impurity have been removed, the product cold water-dispersible is good, be suitable for cold washing especially, the dust pollution of having avoided product in processing and use, to produce of success, and various heavy is to the harm of human body and environment, and the preparation method is simple, easy to operate, easily produce in batches.

Embodiment

Embodiment 1: the preparation method of a kind of shape white dyes 5BM, step is: get cyanuric chloride and reactor is put in DSD acid according to the ratio of mol ratio 2:1, (consumption rises the amount interpolation of frozen water according to the corresponding 2000-2200 of DSD acid of every 200-250 kilogram to add an amount of frozen water, cyanuric chloride is not dissolved in water, purpose is the ice mill), regulating the pH value is 1-1.5, add the hydrochloric acid that the yellow soda ash neutralization reaction generates then, regulating pH value is 6-6.5, after treating that the amino value of DSD acid disappears, the adding mol ratio is 2 aniline, treats that aniline disappearance back adds 2 moles N-Mono Methyl Ethanol Amine, making the pH value by adding NaOH is 10-12, be cooled to 5 ℃ of cold analysis with frozen water then and go out product, filter then, dry, pulverize, obtain the 5BM product.

Embodiment 2: solvent method is made particulate state 5BM product (contrast):

In the flask of the 2000mL that is furnished with stirring, pH meter, thermometer, reflux exchanger and dropping funnel, add 375g trash ice and 300g butanone, be cooled to-7 ℃ after mixing.Add the 50g cyanuric chloride then, under vigorous stirring, add 50gDSD acid, (full name is 4,4`-diaminobenzil-disulfonic acid) ice bath keeps the temperature≤5 ℃ while to drip the 195mL15% sodium carbonate solution in 30-40 minute time down, make reacting liquid pH value at first remain on 3-4, then to 5-6.After treating that DSD acid disappears, the yellow homogeneous phase soup compound of the tea that is easily stirred.Be warming up to 20 ℃ then, drip 25.2g aniline in 5 minutes time, drip 22g50%NaOH solution down at 27-30 ℃ simultaneously, make reacting liquid pH value at first remain on 4-5, then to 8.0-8.5.After treating that aniline disappears, obtain yellow homogeneous phase soup compound.Be warming up to 50 ℃ again, disposable adding 22.9gN-Mono Methyl Ethanol Amine, and reflux.At first reacting liquid pH value is 10, descends rapidly then, by dripping 24.5g50%NaOH solution to keep pH value 10-11.Finish, continued stirring and refluxing 1.5 hours.Add 80gNaCl then, restir refluxed 15 minutes.Slowly distilled at 73 ℃ of butanone, obtain an adhesive reaction liquid when temperature is 75 ℃, this adhesive reaction liquid disappears and obtains light yellow product after about 1 hour.When temperature was 100 ℃, butanone is all steamed removed and obtains the sand product.Be cooled to 30 ℃, filter, drain 100 ℃ of vacuum-dryings.Obtain the 5BM finished product.This process adopts solvent method, whole process of preparation complicated operation, supplementary material and processing unit cost height.

Embodiment 3: the non-solvent method that with the present invention is example is made particulate state 5BM product

In the beaker of 2000mL, add 100g trash ice and 100g water, stirring well the back adds between the 10% hydrochloric acid accent pH to 1-1.5, add 10g cyanuric chloride making beating 0.5 hour, (strength of solution is in 100-120g/L) scope to add 9.75gDSD acid then under vigorous stirring, under keeping 5 ℃, the yellow soda ash liquid that drips simultaneously 2.78g (0.026mol) 10% in 30-40 minutes time makes pH remain on 5-5.5 earlier, be transferred to 6-6.5 then, after treating that amino value disappears, add 5.2g aniline, drip 2.95g (0.028mol) 10% yellow soda ash liquid down at 20-35 ℃ simultaneously pH is remained between 7-7.5, treat the disposable adding 4.8gN-methyl-ethanolamine in aniline disappearance back, and be heated to 80 ℃, be incubated 1.5 hours, it is earlier 10 for the reaction solution pH value, descends rapidly then

By dripping 2.2g (0.055mol) 20%NaOH liquid to keep pH value 10-12, heat up 100 ℃ then, be incubated 0.5 hour.Stop heating, after mixing water is cooled to 30 degrees centigrade, continue to be cooled to 5 ℃ with frozen water, filtration, dry, pulverizing obtain the 5BM product.This preparation process adopts non-solvent method, and whole process of preparation is convenient to operation than solvent method, and has saved butanone and reclaimed and recycle, and adopts non-solvent method can save the raw material and the processing unit cost of butanone.

Claims

1, the preparation method of a kind of white dyes 5BM, it is characterized in that: step is, get cyanuric chloride and reactor is put in DSD acid, add frozen water, the pH value of re-adjustment frozen water, cyanuric chloride, DSD acid mixture is 1-1.5, the hydrochloric acid that generates of neutralization reaction then, regulating pH value is 6-6.5, treat that the amino value of DSD acid disappears after, adding aniline, treat to add the N-Mono Methyl Ethanol Amine after aniline disappears, adjusting the pH value at last is 10-12, makes target product with the frozen water cooling then, separates out, filtration, dry, pulverizing obtain the 5BM product.

2, the preparation method of white dyes 5BM according to claim 1, it is characterized in that: step is: get 2 parts cyanuric chloride and 1 part DSD acid and put into reactor, add frozen water, the re-adjustment frozen water, cyanuric chloride, the pH value of DSD acid mixture is 1-1.5, the hydrochloric acid that generates of neutralization reaction then, regulating pH value is 6-6.5, after treating that the amino value of DSD acid disappears, the aniline that adds 2 parts treats that aniline disappearance back adds 2 parts N-Mono Methyl Ethanol Amine, and adjusting the pH value at last is 10-12, be cooled to 5 ℃ with frozen water then and make target product, separate out, filter, dry, pulverize, obtain the 5BM product.

3, the preparation method of white dyes 5BM according to claim 1 and 2 is characterized in that: the pH value of regulating frozen water, cyanuric chloride, DSD acid mixture is used hydrochloric acid.

4, the preparation method of white dyes 5BM according to claim 1 and 2 is characterized in that: the hydrochloric acid that neutralization reaction generates uses the carbonate neutralization.

5, the preparation method of white dyes 5BM according to claim 1 and 2 is characterized in that: regulate last pH value and use NaOH.