CN103468017A - Preparation method of ultrawhite high-efficiency low-impurity fluorescent whitening agent - Google Patents
Preparation method of ultrawhite high-efficiency low-impurity fluorescent whitening agent Download PDFInfo
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- CN103468017A CN103468017A CN2013103926483A CN201310392648A CN103468017A CN 103468017 A CN103468017 A CN 103468017A CN 2013103926483 A CN2013103926483 A CN 2013103926483A CN 201310392648 A CN201310392648 A CN 201310392648A CN 103468017 A CN103468017 A CN 103468017A
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- Prior art keywords
- diaminobenzil
- disulfonic acid
- whitening agent
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- preparation
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- 239000012535 impurity Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000006081 fluorescent whitening agent Substances 0.000 title abstract 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 40
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- 239000002253 acid Substances 0.000 claims abstract description 24
- 238000001914 filtration Methods 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000012065 filter cake Substances 0.000 claims abstract description 12
- 239000007787 solid Substances 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims abstract description 6
- 239000000975 dye Substances 0.000 claims description 27
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 16
- 230000001105 regulatory effect Effects 0.000 claims description 15
- 238000010009 beating Methods 0.000 claims description 8
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 8
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 8
- 230000000694 effects Effects 0.000 claims description 7
- 150000003839 salts Chemical class 0.000 claims description 3
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Chemical compound C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 abstract description 16
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 abstract description 12
- 230000002087 whitening effect Effects 0.000 abstract description 9
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical compound C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 abstract description 6
- 238000001035 drying Methods 0.000 abstract description 6
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 238000004043 dyeing Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000000034 method Methods 0.000 abstract description 2
- 238000007639 printing Methods 0.000 abstract description 2
- 238000005406 washing Methods 0.000 abstract description 2
- 238000006068 polycondensation reaction Methods 0.000 abstract 3
- 238000011085 pressure filtration Methods 0.000 abstract 2
- 239000012752 auxiliary agent Substances 0.000 abstract 1
- 239000013078 crystal Substances 0.000 abstract 1
- 239000005457 ice water Substances 0.000 abstract 1
- 230000009466 transformation Effects 0.000 abstract 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 10
- 239000000047 product Substances 0.000 description 7
- 101100118680 Caenorhabditis elegans sec-61.G gene Proteins 0.000 description 5
- 239000010813 municipal solid waste Substances 0.000 description 5
- 238000005507 spraying Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000004744 fabric Substances 0.000 description 3
- 238000004383 yellowing Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000271 synthetic detergent Substances 0.000 description 1
- PJANXHGTPQOBST-VAWYXSNFSA-N trans-stilbene Chemical group C=1C=CC=CC=1/C=C/C1=CC=CC=C1 PJANXHGTPQOBST-VAWYXSNFSA-N 0.000 description 1
- 150000003918 triazines Chemical class 0.000 description 1
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Abstract
The invention belongs to the technical field of auxiliary agents specially for washing and printing and dyeing, and particularly relates to a preparation method of an ultrawhite high-efficiency low-impurity fluorescent whitening agent. The preparation method mainly solves the problems of high impurity content, poor whitening effect, and the like of the traditional method for producing a fluorescent whitening agent. The preparation method of the ultrawhite high-efficiency low-impurity fluorescent whitening agent comprises the following steps of: firstly adding ice water to a reaction kettle, carrying out first polycondensation reaction on cyanuric chloride and a 4,4'-diaminobenzil-disulfonic acid solution; filtering by using a filter screen; transferring materials which pass through the filter screen into the reaction kettle; adding aniline for a second polycondensation reaction; increasing temperature to 80-90 DEG C; acting for 1-1.5 hours, then carrying out pressure filtration to obtain a filter cake, then uniformly stirring in a high-pressure kettle added with deionized water, and then increasing the temperature to 60-70 DEG C; adding morpholine and sodium hydroxide solids for a third polycondensation reaction; carrying out crystal transformation and pressure filtration, and drying to obtain the fluorescent whitening agent. The method disclosed by the invention has the advantages of low triazine impurity content, high stacking density, ultrawhite appearance of whitening agent, good whitening effect, and the like.
Description
Technical field
The invention belongs to washing and printing and dyeing special assistant technical field, be specifically related to the efficiently preparation method of low impurity white dyes of a kind of ultrawhite.
Background technology
White dyes 71# is one of most important white dyes in the two triazines whitening agent structures of toluylene, it has good whitening effect, the product brightened by it can keep long-time the placement and not yellowing, and have that high temperature resistant, alkaline-resisting, anti-chlorine floats, oxytolerant floats, the fast light advantage such as shine, be mainly used in synthetic detergent and dyeing.And the 71# white dyes that traditional processing technology is produced has following shortcoming:
(1) impurity (triazine) content high (>=1%),
Refer to following structure:
(2) the little (≤400Kg/m of the tap density of product
3), (3) cold water-dispersible can poor (≤40%).(4), due to poorly water-soluble, yellowing point is not very high.(5) 71# white dyes outward appearance is not very white, and whitening effect neither be fine.
Summary of the invention
The present invention, mainly for the problem that the method for traditional mode of production white dyes exists that impurity (triazine) content tap density high, product is little, cold water-dispersible can be poor, dissolubility is poor, whitening effect is bad, provides the efficiently preparation method of low impurity white dyes of a kind of ultrawhite.
The present invention addresses the above problem the technical scheme of taking to be:
A kind of ultrawhite is the preparation method of low impurity white dyes efficiently, in molar ratio 1:2 get massfraction be 10～15% 4, 4 '-diaminobenzil-disulfonic acid solution and cyanuric chloride, first to the frozen water that adds 10～15 times of cyanuric chloride weight in reactor, with the salt acid for adjusting pH value, be 1～2, add cyanuric chloride making beating 1～2h again in reactor, then drip 4, 4 '-diaminobenzil-disulfonic acid solution, it is 0～5 ℃ that temperature is controlled, it is 4～6 that the sodium carbonate solution that is 10～20% with massfraction is regulated the pH value, carrying out a contracting reaction to amino value disappears, with 130～150 mesh filter screens, filtered, the material passed through from filter screen proceeds in reactor again, then add 1.95～2.1 times 4 in reactor, 4 '-aniline of diaminobenzil-disulfonic acid molar weight, it is 7～9 that the sodium hydroxide solution that is 20～30% with massfraction is regulated pH, carrying out two contracting reactions to amino value disappears, heat up 80～90 ℃, press filtration after effect 1～1.5h, the filter cake obtained adds in the autoclave of deionized water of 10～15 times of cyanuric chloride weight again, stir evenly 60～70 ℃ of rear intensifications, add 2.3～2.6 times 4, 4 '-morpholine of diaminobenzil-disulfonic acid molar weight, 2.1～2.3 times 4, 4 '-sodium hydrate solid of diaminobenzil-disulfonic acid molar weight carries out three contracting reactions, 1.5 after～2h, turned brilliant, press filtration, dry, obtain white dyes.
The present invention adopts above-mentioned preparation method, by intensification press filtration after filtration, two sheepshank bundles after a sheepshank bundle, removes by product and impurity; By heating up 60～70 ℃, add morpholine, optimize three contracting reaction conditionss, make that produced 71# white dyes has that the triazine foreign matter content is low, the tap density of product is large, the dispersing property of product in water is good, high, the whitening agent outward appearance ultrawhite of yellowing point and the characteristics such as whitening effect is good while dying cloth.
For further showing preparation method's of the present invention effect, done following simultaneous test:
Simultaneous test 1: the white dyes that traditional technology is produced:
Add water 500L in reactor, add trash ice 800Kg, with hydrochloric acid adjust pH 1～2, throw cyanuric chloride 100Kg, pull an oar 1 hour, carry out a contracting reaction under 0～5 ℃, the 98Kg4 that is 10% by massfraction, 4 '-add in same reactor in diaminobenzil-disulfonic acid solution 2.5 hours, it is 6 that the sodium carbonate solution that is simultaneously 10% with massfraction is regulated pH, reaction to terminal, again 50.5Kg aniline is also dropped in same reactor, it is 8 that the sodium hydroxide solution that is simultaneously 20% with massfraction is regulated pH, after carrying out two contracting reactions to terminal, reaction mass is gone in three contracting reactors, add the 56.69Kg morpholine, the 23Kg sodium hydrate solid, turn brilliant under 135 ℃, turn brilliant rear press filtration, carry out spraying drying after the filter cake making beating, after aftertreatment is synthetic, obtain white dyes.
Simultaneous test 2: adopt after a sheepshank bundle and filter the white dyes of producing:
Add water 500L in reactor, add trash ice 800Kg, with hydrochloric acid adjust pH 1～2, throw cyanuric chloride 100Kg, pull an oar 1 hour, carry out a contracting reaction under 0～5 ℃, the 100Kg4 that is 10% by massfraction, 4 '-add in same reactor in diaminobenzil-disulfonic acid solution 2.5 hours, it is 6 that the sodium carbonate solution that is simultaneously 10% with massfraction is regulated pH, reaction to terminal, after filtration, again 50.5Kg aniline is also dropped in same reactor, it is 8 that the sodium hydroxide solution that is simultaneously 20% with massfraction is regulated pH, after carrying out two contracting reactions to terminal, reaction mass is gone in three contracting reactors, add the 56.69Kg morpholine, the 23Kg sodium hydrate solid, turn brilliant under 110-135 ℃, turn brilliant rear press filtration, carry out spraying drying after the filter cake making beating, after aftertreatment is synthetic, obtain white dyes.
Simultaneous test 3: adopt a sheepshank beam filter, the white dyes that two sheepshank bundle press filtrations are produced:
Add water 500L in reactor, add trash ice 800Kg, with hydrochloric acid adjust pH 1～2, throw cyanuric chloride 100Kg, pull an oar 1 hour, carry out a contracting reaction under 0～5 ℃, the 100Kg4 that is 10% by massfraction, 4 '-add in same reactor in diaminobenzil-disulfonic acid solution 2.5 hours, it is 6 that the sodium carbonate solution that is simultaneously 10% with massfraction is regulated pH, reaction to terminal, after filtration, again 50.5Kg aniline is also dropped in same reactor, it is 8 that the sodium hydroxide solution that is simultaneously 20% with massfraction is regulated pH, after carrying out two contracting reactions to terminal, heat up 80～90 ℃, press filtration after effect 1h, the filter cake obtained adds in the autoclave that the 1300L deionized water is arranged again, after stirring evenly 30～40 ℃ of rear intensifications, add the 56.69Kg morpholine, the 23Kg sodium hydrate solid, turn brilliant under 110～135 ℃, turn brilliant rear press filtration, carry out spraying drying after the filter cake making beating, after aftertreatment is synthetic, obtain white dyes.
Simultaneous test 4: adopt a sheepshank beam filter, two sheepshank bundle press filtrations, heat up after 60～70 ℃ and add morpholine, the white dyes of production:
Add water 500L in reactor, add trash ice 800Kg, with hydrochloric acid adjust pH 1～2, throw cyanuric chloride 100Kg, pull an oar 1 hour, carry out a contracting reaction under 0～5 ℃, the 100Kg4 that is 10% by massfraction, 4 '-add in same reactor in diaminobenzil-disulfonic acid solution 2.5 hours, the sodium carbonate solution that is simultaneously 10% with massfraction regulate pH be 6 reactions to terminal, after filtration, again 50.5Kg aniline is also dropped in same reactor, it is 8 that the sodium hydroxide solution that is simultaneously 20% with massfraction is regulated pH, after carrying out two contracting reactions to terminal, heat up 80～90 ℃, press filtration after effect 1h, the filter cake obtained adds in the autoclave that the 1300L deionized water is arranged again, after stirring evenly 60～70 ℃ of rear intensifications, add the 56.69Kg morpholine, add the 23Kg sodium hydrate solid, turn brilliant under 110～135 ℃, turn brilliant rear press filtration, carry out spraying drying after the filter cake making beating, after aftertreatment is synthetic, obtain white dyes.
The target product of four groups of simultaneous tests has been carried out to percentage ratio, the WICIE value of dying cloth under 5 ‰ concentration and WG value that triazine impurity, tap density, cold water-dispersible 0.02g material dissolve in 1L water and tested, concrete outcome is in Table 1.
Four groups of group simultaneous test products therefroms of table 1, the applied analysis data under identical conditions are as following table:
By table 1, can be drawn, the white dyes that preparation method of the present invention produces, index: WICIE value, WG value after triazine impurity, tap density, cold water disperse to go, dye cloth all are better than the white dyes that traditional technology is produced.
Embodiment
Embodiment 1
Add water 500L in reactor, add trash ice 800Kg, with the hydrochloric acid adjust pH, be 1.5, throw cyanuric chloride 100Kg, pull an oar 1 hour, then the 100Kg4 that is 10% by massfraction, 4 '-add in same reactor in diaminobenzil-disulfonic acid solution 2.5 hours, it is 3 ℃ that temperature is controlled, it is 6 that the sodium carbonate solution that is 15% with massfraction is regulated the pH value, carrying out a contracting reaction to amino value disappears, with 130 order stainless steel filtering nets, filtered, the material passed through from filter screen proceeds in reactor again, again 50.5Kg aniline is also dropped in same reactor, it is 8 that the sodium hydroxide solution that is simultaneously 25% with massfraction is regulated pH, carrying out two contracting reactions to amino value disappears, heat up 85 ℃, press filtration after effect 1h, the filter cake obtained adds in the autoclave that the 1300L deionized water is arranged again, after stirring evenly 65 ℃ of rear intensifications, add the 56.69Kg morpholine, add the 23Kg sodium hydrate solid, carry out three contracting reactions, 1.5h after, turn brilliant under 120 ℃, turn brilliant rear press filtration, carry out spraying drying after the filter cake making beating, obtain white dyes.
The present invention can also be according to the arbitrary proportion value in following ranges:
A kind of ultrawhite is the preparation method of low impurity white dyes efficiently, in molar ratio 1:2 get massfraction be 10～15% 4, 4 '-diaminobenzil-disulfonic acid solution and cyanuric chloride, first to the frozen water that adds 10～15 times of cyanuric chloride weight in reactor, with the salt acid for adjusting pH value, be 1～2, add cyanuric chloride making beating 1～2h again in reactor, then drip 4, 4 '-diaminobenzil-disulfonic acid solution, it is 0～5 ℃ that temperature is controlled, it is 4～6 that the sodium carbonate solution that is 10～20% with massfraction is regulated the pH value, carrying out a contracting reaction to amino value disappears, with 130～150 mesh filter screens, filtered, the material passed through from filter screen proceeds in reactor again, then add 1.95～2.1 times 4 in reactor, 4 '-aniline of diaminobenzil-disulfonic acid molar weight, it is 7～9 that the sodium hydroxide solution that is 20～30% with massfraction is regulated pH, carrying out two contracting reactions to amino value disappears, heat up 80～90 ℃, press filtration after effect 1～1.5h, the filter cake obtained adds in the autoclave of deionized water of 10～15 times of cyanuric chloride weight again, stir evenly 60～70 ℃ of rear intensifications, add 2.3～2.6 times 4, 4 '-morpholine of diaminobenzil-disulfonic acid molar weight, 2.1～2.3 times 4, 4 '-sodium hydrate solid of diaminobenzil-disulfonic acid molar weight carries out three contracting reactions, 1.5 after～2h, turned brilliant, press filtration, dry, obtain white dyes.
Claims (1)
1. a ultrawhite is efficiently hanged down the preparation method of impurity white dyes, it is characterized in that: in molar ratio 1:2 get massfraction be 10～15% 4, 4 '-diaminobenzil-disulfonic acid solution and cyanuric chloride, first to the frozen water that adds 10～15 times of cyanuric chloride weight in reactor, with the salt acid for adjusting pH value, be 1～2, add cyanuric chloride making beating 1～2h again in reactor, then drip 4, 4 '-diaminobenzil-disulfonic acid solution, it is 0～5 ℃ that temperature is controlled, it is 4～6 that the sodium carbonate solution that is 10～20% with massfraction is regulated the pH value, carrying out a contracting reaction to amino value disappears, with 130～150 mesh filter screens, filtered, the material passed through from filter screen proceeds in reactor again, then add 1.95～2.1 times 4 in reactor, 4 '-aniline of diaminobenzil-disulfonic acid molar weight, it is 7～9 that the sodium hydroxide solution that is 20～30% with massfraction is regulated pH, carrying out two contracting reactions to amino value disappears, heat up 80～90 ℃, press filtration after effect 1～1.5h, the filter cake obtained adds in the autoclave of deionized water of 10～15 times of cyanuric chloride weight again, stir evenly 60～70 ℃ of rear intensifications, add 2.3～2.6 times 4, 4 '-morpholine of diaminobenzil-disulfonic acid molar weight, 2.1～2.3 times 4, 4 '-sodium hydrate solid of diaminobenzil-disulfonic acid molar weight carries out three contracting reactions, 1.5 after～2h, turned brilliant, press filtration, dry, obtain white dyes.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310392648.3A CN103468017B (en) | 2013-09-02 | 2013-09-02 | Preparation method of ultrawhite high-efficiency low-impurity fluorescent whitening agent |
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| CN201310392648.3A CN103468017B (en) | 2013-09-02 | 2013-09-02 | Preparation method of ultrawhite high-efficiency low-impurity fluorescent whitening agent |
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| CN103468017B CN103468017B (en) | 2015-04-01 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109776757A (en) * | 2019-01-15 | 2019-05-21 | 陕西科技大学 | A kind of preparation method and applications of the paper surface polyurethane fluorescent brightening lotion containing benzophenone |
| CN111809443A (en) * | 2020-07-22 | 2020-10-23 | 浙江传化华洋化工有限公司 | Modified fluorescent whitening agent aqueous solution and preparation method thereof |
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| CN102911127A (en) * | 2012-10-26 | 2013-02-06 | 山西青山化工有限公司 | Preparation method for low-triazine fluorescent whitening agent |
| CN102993110A (en) * | 2011-06-30 | 2013-03-27 | 上海安诺其纺织化工股份有限公司 | Intermediate of 4,4'-diaminostilbene-2,2'-disulfonic acid derivative |
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2013
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102993110A (en) * | 2011-06-30 | 2013-03-27 | 上海安诺其纺织化工股份有限公司 | Intermediate of 4,4'-diaminostilbene-2,2'-disulfonic acid derivative |
| CN102911127A (en) * | 2012-10-26 | 2013-02-06 | 山西青山化工有限公司 | Preparation method for low-triazine fluorescent whitening agent |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109776757A (en) * | 2019-01-15 | 2019-05-21 | 陕西科技大学 | A kind of preparation method and applications of the paper surface polyurethane fluorescent brightening lotion containing benzophenone |
| CN109776757B (en) * | 2019-01-15 | 2021-06-08 | 陕西科技大学 | Preparation method and application of benzophenone-containing paper surface polyurethane fluorescent whitening emulsion |
| CN111809443A (en) * | 2020-07-22 | 2020-10-23 | 浙江传化华洋化工有限公司 | Modified fluorescent whitening agent aqueous solution and preparation method thereof |
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