CN101367770B

CN101367770B - Preparation method for fluorescent whitening agent

Info

Publication number: CN101367770B
Application number: CN2008101414704A
Authority: CN
Inventors: 贺明波
Original assignee: Individual
Current assignee: Individual
Priority date: 2008-09-26
Filing date: 2008-09-26
Publication date: 2012-07-04
Anticipated expiration: 2028-09-26
Also published as: CN101367770A

Abstract

The present invention relates to a preparation method of fluorescence brightening agent. The present invention effectively solves the problems that the emission quantity of acid liquid is large, the dust pollution is serious, the water solubility is poor, the yellowing point is low, the solidness for solarization is poor, and the scope of application is narrow. In the preparation method, 500 to 700 kg ice water of mixed ice and water is added into a reactor, hydrochloric acid is used for adjusting the pH value, 77 to 109 kg of melamine is added when the reaction solution is stirred, 72 to 102 kg of sulfanilic acid is added, sodalye solution is dropped to adjust the pH value and is stopped to be dropped when the pH value can no longer be reduced, simultaneously 2200 to 2600 kg of DSD acid aqueous solution and sodalye solution are added, the sodalye solution is stopped to be dropped when the pH value can no longer be reduced, the reaction solution is added into an acid eduction pot, hydrochloric acid is added to adjust the pH value when the reaction solution is mixed, the reaction solution is transmitted to a pressure filter to be processed through pressure filtration, the filter cake is collected, the filter cake, 100 to 140 kg of diethanolamine and 66 to 94 kg of diglycol are added when the reaction solution is stirred, the sodalye solution is used for adjusting the pH value, and then the product is packaged. The present invention has the advantages that the method is simple, the scope of application is wide, the effects of application are good, and the present invention is a large innovation in the chemical field.

Description

A kind of preparation method of white dyes

One, technical field

The present invention relates to chemical field, particularly a kind of preparation method of white dyes.

Two, background technology

White dyes is widely used in industry such as papermaking, weaving, coating, washing composition; Domestic is main with powder product VBL mostly; Belong to introduce technology the earliest, range of application the widest, the maximum kind of output; But have that acid solution discharging is big, dust pollution is serious, poorly water-soluble, problems such as yellowing point is low, light fastness is poor, narrow in application range, so its improvement is imperative.

Three, summary of the invention

To above-mentioned situation, for overcoming the prior art defective, the present invention's purpose just provides a kind of preparation method of white dyes; Can solve effectively that present white dyes prepares that acid solution discharging is big, dust pollution is serious, poorly water-soluble, yellowing point is low, light fastness is poor, the problem of narrow in application range, the technical scheme of its solution is to add to reaction kettle and ice and water blended frozen water 500-700kg; About ice cube diameter 50mm, using mass concentration is that>=30% hydrochloric acid transfers pH value to be 1.0-3.0, keeps temperature≤5 ℃; Add cyanuric chloride 77-109kg, Sulphanilic Acid 72-102kg while stirring, stirred 15-25 minute, the dropping mass concentration is 42% caustic-soda aqueous solution; The accent pH value is 3.5-4.5, and temperature≤5 ℃ are when treating that pH value no longer descends; Stop to drip caustic-soda aqueous solution, keep and stirred 25-35 minute, the DSD that drips the mass concentration 15% that is become by DSD acid thin up more simultaneously is sour, and (DSD acid full name is 4; 4-diaminobenzil-disulfonic acid) aqueous solution 2200-2600kg and mass concentration be 42% caustic-soda aqueous solution (caustic soda is claimed caustic soda again, sodium hydroxide, molecular formula is NaOH; As follows), holding temperature 55-65 ℃, pH value 3.5-4.5; The DSD aqueous acid added in 2.5-3.5 hour, finished when the DSD aqueous acid is reinforced, when pH value keeps 3.5-4.5 no longer to descend, stopped to drip caustic-soda aqueous solution; Insulation reaction 1.5-2.5 hour, be cooled to then below 30 ℃, get reaction solution; Reaction solution is squeezed into the acid out jar, add mass concentration while stirring and be>=30% hydrochloric acid, the accent pH value is 1.5-2.0; Material (reaction solution) in the acid out jar is pumped into the pressure filter press filtration through dnockout, collects filter cake; Start modulation kettle, add filter cake, diethylolamine 100-140kg, glycol ether 66-94kg then while stirring successively, using mass concentration after 15-25 minute is that 42% caustic-soda aqueous solution transfers pH value to be 7.5-8.0, and blowing is packed after 15-25 minute.The inventive method is simple, reasonable recipe, and applied range, result of use is good, is that one on the chemical field innovated greatly.

Four, embodiment

Elaborate below in conjunction with the practical situation specific embodiments of the invention.

Provided by technical scheme, the inventive method at first is to add with water and ice cube blended frozen water 500-700kg, about the diameter 50mm of ice cube to reaction kettle; Using mass concentration is that>=30% hydrochloric acid transfers pH value to be 1.0-3.0, keeps temperature≤5 ℃, adds cyanuric chloride 77-109kg, Sulphanilic Acid 72-102kg while stirring; Stirred 15-25 minute, the dropping mass concentration is 42% caustic-soda aqueous solution, and the accent pH value is 3.5-4.5; Temperature≤5 ℃ are kept and were stirred 25-35 minute; The DSD aqueous acid 2480kg and the mass concentration that drip the mass concentration 15% that is become by DSD acid thin up more simultaneously are 42% caustic-soda aqueous solution, holding temperature 55-65 ℃, and pH value 3.5-4.5; The DSD aqueous acid added in 2.5-3.5 hour; Finish when the DSD aqueous acid is reinforced, when pH value no longer descends, stop to drip caustic-soda aqueous solution, insulation reaction 1.5-2.5 hour; Be cooled to then below 30 ℃, get reaction solution; Reaction solution is squeezed into the acid out jar, add mass concentration while stirring and be>=30% hydrochloric acid, accents pH value is 1.5-2.0, and material (reaction solution) in the acid out jar is got into the pressure filter press filtration through the dnockout pump, the collection filter cake; In modulation kettle, add filter cake, diethylolamine 100-140kg, glycol ether 66-94kg then while stirring successively, using mass concentration after 15-25 minute is that 42% caustic-soda aqueous solution transfers pH value to be 7.5-8.0, blowing packing after 15-25 minute.

The DSD acid that said DSD acid is mass content >=99%; Said Sulphanilic Acid is the Sulphanilic Acid of mass content >=99%; Said cyanuric chloride is the cyanuric chloride of mass content >=99%; Said diethylolamine is the diethylolamine of mass content >=99%; Said glycol ether is the glycol ether of mass content >=99%; The mixing of said water and ice cube, the two add-on need different situations to add, and when temperature was high, the ice cube add-on was many, when temperature is hanged down; The ice cube add-on is few, in order to keep temperature, adds about ice cube diameter 50mm, and be because ice cube is too little; Thawing speed is fast, and is too big, is difficult for melting, and temperature is wayward.

Embodiment 1

The said method of the present invention is, at first adds entry and ice cube blended frozen water 600kg to reaction kettle, and using mass concentration is that to transfer pH value be 1.0 for 30% hydrochloric acid; Keep 4 ℃ of temperature, add cyanuric chloride 93kg, Sulphanilic Acid 87kg more while stirring, stirred 20 minutes; The dropping mass concentration is 42% caustic-soda aqueous solution, and transferring pH value is 4.0,4 ℃ of temperature; When treating that pH value no longer descends, stop to drip caustic-soda aqueous solution, keep and stirred 30 minutes; The DSD aqueous acid 2480kg and the mass concentration that drip the mass concentration 15% that is become by DSD acid thin up more simultaneously are 42% caustic-soda aqueous solution, 60 ℃ of holding temperatures, pH value 4.0; The DSD aqueous acid added in 3 hours; Finish when the DSD aqueous acid is reinforced, when pH value keeps 4.0 no longer to descend, stop to drip caustic-soda aqueous solution, insulation reaction 2 hours; Be cooled to 25 ℃ then, get reaction solution; Reaction solution is squeezed into the acid out jar, add mass concentration while stirring and be 30% hydrochloric acid, making pH value is 1.5; Using the dnockout pump again is that 1.5 reaction solution material is squeezed into the pressure filter press filtration with pH value, collects filter cake; In modulation kettle, add filter cake, diethylolamine 120kg, glycol ether 80kg then while stirring successively, the use mass concentration is that 42% caustic-soda aqueous solution accent pH value is a blowing packing after 7.5,20 minutes after 20 minutes.

Embodiment 2

The said method of the present invention is, at first adds entry and ice cube blended frozen water 650kg to reaction kettle, use mass concentration be 40% hydrochloric acid to transfer pH value be 2.0, agitator; Keep 3 ℃ of temperature, add cyanuric chloride 100kg, Sulphanilic Acid 94kg while stirring, stirred 25 minutes; The dropping mass concentration is 42% caustic-soda aqueous solution, and transferring pH value is 4.5,3 ℃ of temperature; When treating that pH value 4.5 does not descend, stop to drip caustic-soda aqueous solution, keep and stirred 35 minutes; The DSD aqueous acid 2580kg and the mass concentration that drip the mass concentration 15% that is become by DSD acid thin up more simultaneously are 42% caustic-soda aqueous solution, 55 ℃ of holding temperatures, pH value 4.5; The DSD aqueous acid added in 2.5 hours; Finish when the DSD aqueous acid is reinforced, when pH value keeps 4.5 not descend, stop to drip caustic-soda aqueous solution, insulation reaction 2.5 hours; Be cooled to 20 ℃ then, get reaction solution; Reaction solution is squeezed into the acid out jar, add mass concentration while stirring and be 40% hydrochloric acid, making pH value is 2.0; Material (reaction solution) in the acid out jar is got into the pressure filter press filtration through the dnockout pump, collect filter cake; Start modulation kettle, in modulation kettle, add filter cake, diethylolamine 130kg, glycol ether 90kg while stirring successively, the use mass concentration is that 42% caustic-soda aqueous solution accent pH value is a blowing packing after 8.0,25 minutes after 25 minutes.

The present invention is the red-brown transparent liquid; PH value: 7.5-8.0; Solid content: 40%, through test and practical application, stable in properties, quality is good; Wide accommodation can be useful on industrial circles such as papermaking, weaving, coating, washing composition, and cost is low, and save energy is more than 25%; Pollution-free, good water solubility, inclusion-free and throw out, degree of brightening improves more than 40%; Can't compare for existing whitening agent, be that one on the white dyes created greatly, and economic and social benefit is huge.

Claims

1. the preparation method of a white dyes is characterized in that, at first adds ice and water blended frozen water 500-700kg to reaction kettle, about ice cube diameter 50mm; Using mass concentration is that>=30% hydrochloric acid transfers pH value to be 1.0-3.0, keeps temperature≤5 ℃, adds cyanuric chloride 77-109kg, Sulphanilic Acid 72-102kg more while stirring, stirs 15-25 minute; Drip mass concentration and be 42% caustic-soda aqueous solution, the accent pH value is 3.5-4.5, temperature≤5 ℃; Keep and stirred 25-35 minute, drip simultaneously again, 4 of the mass concentration 15% that 4-diaminobenzil-disulfonic acid thin up becomes by 4; 4-diaminobenzil-disulfonic acid aqueous solution 2200-2600kg and mass concentration are 42% caustic-soda aqueous solution, holding temperature 55-65 ℃, and pH value 3.5-4.5; When 4,4-diaminobenzil-disulfonic acid aqueous solution added in 2.5-3.5 hour, and pH value 3.5-4.5 stops to drip caustic-soda aqueous solution; Insulation reaction 1.5-2.5 hour, be cooled to then below 30 ℃, get reaction solution; Reaction solution is squeezed into the acid out jar, add mass concentration while stirring and be>=30% hydrochloric acid, the accent pH value is 1.5-2.0; Material in the acid out jar is pumped into the pressure filter press filtration through dnockout, collects filter cake, start modulation kettle then and add filter cake, diethylolamine 100-140kg, glycol ether 66-94kg while stirring successively; The use mass concentration is 42% caustic-soda aqueous solution accent pH value: 7.5-8.0 after 15-25 minute, solid content: 40%, and blowing packing after 15-25 minute.

2. the preparation method of white dyes according to claim 1 is characterized in that, and is said 4, and 4-diaminobenzil-disulfonic acid is 4 of mass content >=99%, 4-diaminobenzil-disulfonic acid; Said Sulphanilic Acid is the Sulphanilic Acid of mass content >=99%; Said cyanuric chloride is the cyanuric chloride of mass content >=99%; Said diethylolamine is the diethylolamine of mass content >=99%; Said glycol ether is the glycol ether of mass content >=99%.

3. the preparation method of white dyes according to claim 1 is characterized in that, at first adds said water and ice cube blended frozen water 600kg to reaction kettle, and using mass concentration is that to transfer pH value be 1.0 for 30% hydrochloric acid; At 4 ℃, add cyanuric chloride 93kg, Sulphanilic Acid 87kg while stirring, stirred 20 minutes, the dropping mass concentration is 42% caustic-soda aqueous solution; Transferring pH value is 4.0, and 4 ℃ of temperature are kept and stirred 30 minutes, drip simultaneously by 4 again; 4 of the mass concentration 15% that 4-diaminobenzil-disulfonic acid thin up becomes, 4-diaminobenzil-disulfonic acid aqueous solution 2480kg and mass concentration are 42% caustic-soda aqueous solution, 60 ℃ of holding temperatures; PH value 4.0,4,4-diaminobenzil-disulfonic acid aqueous solution added in 3 hours; When 4,4-diaminobenzil-disulfonic acid aqueous solution is reinforced to finish, pH value keeps 4.0, stops to drip caustic-soda aqueous solution; Insulation reaction 2 hours is cooled to 25 ℃ then, gets reaction solution; Reaction solution is squeezed into the acid out jar, add mass concentration while stirring and be 30% hydrochloric acid, making pH value is 1.5; Using the dnockout pump again is that 1.5 reaction solution material is squeezed into the pressure filter press filtration with pH value, collects filter cake, restarts modulation kettle; Add filter cake, diethylolamine 120kg, glycol ether 80kg while stirring successively, the use mass concentration is that 42% caustic-soda aqueous solution accent pH value is a blowing packing after 7.5,20 minutes after 20 minutes.

4. the preparation method of white dyes according to claim 1 is characterized in that, at first adds said water and ice cube blended frozen water 650kg to reaction kettle, and using mass concentration is that to transfer pH value be 2.0 for 40% hydrochloric acid; Keep 3 ℃ of temperature, add cyanuric chloride 100kg, Sulphanilic Acid 94kg while stirring, stirred 25 minutes, the dropping mass concentration is 42% caustic-soda aqueous solution; Transferring pH value is 4.5, and 3 ℃ of temperature are kept and stirred 35 minutes, drip simultaneously by 4 again; 4 of the mass concentration 15% that 4-diaminobenzil-disulfonic acid thin up becomes, 4-diaminobenzil-disulfonic acid aqueous solution 2580kg and mass concentration are 42% caustic-soda aqueous solution, 55 ℃ of holding temperatures; PH value 4.5,4,4-diaminobenzil-disulfonic acid aqueous solution added in 2.5 hours; When 4,4-diaminobenzil-disulfonic acid aqueous solution is reinforced to finish, pH value keeps 4.5, stops to drip caustic-soda aqueous solution; Insulation reaction 2.5 hours is cooled to 20 ℃ then, gets reaction solution; Reaction solution is squeezed into the acid out jar, add mass concentration while stirring and be 40% hydrochloric acid, making pH value is 2.0; Then material in the acid out jar is pumped into the pressure filter press filtration through dnockout, collects filter cake, start modulation kettle; In modulation kettle, add filter cake, diethylolamine 130kg, glycol ether 90kg while stirring successively, the use mass concentration is that 42% caustic-soda aqueous solution accent pH value is a blowing packing after 8.0,25 minutes after 25 minutes.