CN103468017B - 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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- CN103468017B CN103468017B CN201310392648.3A CN201310392648A CN103468017B CN 103468017 B CN103468017 B CN 103468017B CN 201310392648 A CN201310392648 A CN 201310392648A CN 103468017 B CN103468017 B CN 103468017B
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- diaminobenzil
- whitening agent
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- massfraction
- impurity
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- 239000012535 impurity Substances 0.000 title claims abstract description 17
- 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 43
- 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 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Chemical compound C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 claims abstract description 22
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 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 5
- 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
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 16
- 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
- NGNBDVOYPDDBFK-UHFFFAOYSA-N 2-[2,4-di(pentan-2-yl)phenoxy]acetyl chloride Chemical class CCCC(C)C1=CC=C(OCC(Cl)=O)C(C(C)CCC)=C1 NGNBDVOYPDDBFK-UHFFFAOYSA-N 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- 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
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 238000004043 dyeing 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
- 238000001035 drying Methods 0.000 abstract 1
- 239000005457 ice water Substances 0.000 abstract 1
- 230000009466 transformation Effects 0.000 abstract 1
- 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
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 239000004744 fabric Substances 0.000 description 3
- 238000004383 yellowing Methods 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000004061 bleaching 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
- 239000006185 dispersion Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 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 preparation method of the efficient 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 structure of toluylene, it has good whitening effect, can be kept placing and not yellowing for a long time by its product brightened, and there is the advantages such as high temperature resistant, alkaline-resisting, chlorine-resistant drift, resistance to oxygen bleaching, resistance to illumination, 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%),
Namely following structure is referred to:
(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
Mainly for the method for traditional mode of production white dyes, the present invention exists that impurity (triazine) content tap density that is high, product is little, cold water-dispersible can poor, dissolubility is poor, whitening effect is bad problem, provides the preparation method of the efficient low impurity white dyes of a kind of ultrawhite.
The present invention is the technical scheme taked that solves the problem:
The preparation method of the efficient low impurity white dyes of a kind of ultrawhite, in molar ratio 1:2 get that massfraction is 10 ~ 15% 4, 4 '-diaminobenzil-disulphonic acid and cyanuric chloride, in reactor, first add the frozen water of 10 ~ 15 times of cyanuric chloride weight, be 1 ~ 2 with salt acid for adjusting pH value, cyanuric chloride making beating 1 ~ 2h is added again in reactor, then 4 are dripped, 4 '-diaminobenzil-disulphonic acid, it is 0 ~ 5 DEG C that temperature controls, be 4 ~ 6 by the sodium carbonate solution adjust ph that massfraction is 10 ~ 20%, carry out a contracting reaction to disappear to amino value, filter with 130 ~ 150 mesh filter screens, the material passed through from filter screen proceeds in reactor again, then 1.95 ~ 2.1 times 4 is added in a kettle., the aniline of 4 '-diaminobenzil-disulfonic acid molar weight, pH is regulated to be 7 ~ 9 with the sodium hydroxide solution that massfraction is 20 ~ 30%, carry out two contracting reactions to disappear to amino value, heat up 80 ~ 90 DEG C, press filtration after effect 1 ~ 1.5h, the filter cake obtained adds in the autoclave of the deionized water of 10 ~ 15 times of cyanuric chloride weight again, stir evenly rear intensification 60 ~ 70 DEG C, add 2.3 ~ 2.6 times 4, the morpholine of 4 '-diaminobenzil-disulfonic acid molar weight, 2.1 ~ 2.3 times 4, the sodium hydrate solid of 4 '-diaminobenzil-disulfonic acid molar weight carries out three contracting reactions, after 1.5 ~ 2h, carry out turning brilliant, press filtration, dry, obtain white dyes.
The present invention adopts above-mentioned preparation method, removes by product and impurity by the press filtration that heats up after filtration, two sheepshank bundles after a sheepshank bundle; By heating up 60 ~ 70 DEG C, add morpholine, optimize three contracting reaction conditionss, produced 71# white dyes is had triazine impurity content is low, the tap density of product greatly, the dispersing property of product in water be good, high, the whitening agent outward appearance ultrawhite of yellowing point and the feature such as whitening effect is good when dying cloth.
For showing the effect of preparation method of the present invention further, do 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, a contracting reaction is carried out at 0 ~ 5 DEG C, be the 98Kg4 of 10% by massfraction, 4 '-diaminobenzil-disulphonic acid adds in 2.5 hours in same reactor, regulate pH to be 6 with the sodium carbonate solution that massfraction is 10% simultaneously, reaction to terminal, again 50.5Kg aniline is also dropped in same reactor, regulate pH to be 8 with the sodium hydroxide solution that massfraction is 20% simultaneously, after carrying out two contracting reactions to terminal, reaction mass is gone in three contracting reactors, add 56.69Kg morpholine, 23Kg sodium hydrate solid, turn brilliant at 135 DEG C, turn brilliant rear press filtration, spraying dry is carried out after filter cake making beating, after aftertreatment synthesis, obtain white dyes.
Simultaneous test 2: the white dyes filtering production after adopting a sheepshank bundle:
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, a contracting reaction is carried out at 0 ~ 5 DEG C, be the 100Kg4 of 10% by massfraction, 4 '-diaminobenzil-disulphonic acid adds in 2.5 hours in same reactor, regulate pH to be 6 with the sodium carbonate solution that massfraction is 10% simultaneously, reaction to terminal, after filtration, again 50.5Kg aniline is also dropped in same reactor, regulate pH to be 8 with the sodium hydroxide solution that massfraction is 20% simultaneously, after carrying out two contracting reactions to terminal, reaction mass is gone in three contracting reactors, add 56.69Kg morpholine, 23Kg sodium hydrate solid, turn brilliant at 110-135 DEG C, turn brilliant rear press filtration, spraying dry is carried out after filter cake making beating, after aftertreatment synthesis, 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, a contracting reaction is carried out at 0 ~ 5 DEG C, be the 100Kg4 of 10% by massfraction, 4 '-diaminobenzil-disulphonic acid adds in 2.5 hours in same reactor, regulate pH to be 6 with the sodium carbonate solution that massfraction is 10% simultaneously, reaction to terminal, after filtration, again 50.5Kg aniline is also dropped in same reactor, regulate pH to be 8 with the sodium hydroxide solution that massfraction is 20% simultaneously, after carrying out two contracting reactions to terminal, heat up 80 ~ 90 DEG C, press filtration after effect 1h, the filter cake obtained adds in the autoclave having 1300L deionized water again, after stirring evenly rear intensification 30 ~ 40 DEG C, add 56.69Kg morpholine, 23Kg sodium hydrate solid, turn brilliant at 110 ~ 135 DEG C, turn brilliant rear press filtration, spraying dry is carried out after filter cake making beating, after aftertreatment synthesis, obtain white dyes.
Simultaneous test 4: adopt a sheepshank beam filter, two sheepshank bundle press filtrations, heat up after 60 ~ 70 DEG C 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, a contracting reaction is carried out at 0 ~ 5 DEG C, be the 100Kg4 of 10% by massfraction, 4 '-diaminobenzil-disulphonic acid adds in 2.5 hours in same reactor, simultaneously with massfraction be 10% sodium carbonate solution regulate pH be 6 reactions to terminal, after filtration, again 50.5Kg aniline is also dropped in same reactor, regulate pH to be 8 with the sodium hydroxide solution that massfraction is 20% simultaneously, after carrying out two contracting reactions to terminal, heat up 80 ~ 90 DEG C, press filtration after effect 1h, the filter cake obtained adds in the autoclave having 1300L deionized water again, after stirring evenly rear intensification 60 ~ 70 DEG C, add 56.69Kg morpholine, add 23Kg sodium hydrate solid, turn brilliant at 110 ~ 135 DEG C, turn brilliant rear press filtration, spraying dry is carried out after filter cake making beating, after aftertreatment synthesis, obtain white dyes.
Carried out triazine impurity to the target product of four groups of simultaneous tests, tap density, cold water-dispersible 0.02g expect that the percentage ratio dissolved in 1L water, the WICIE value of dying cloth under 5 ‰ concentration and WG value are tested, concrete outcome is in table 1.
Table 1 four groups of group simultaneous test products therefroms, the applied analysis data under identical conditions are as following table:
Can be drawn by table 1, the white dyes that preparation method of the present invention produces, index: triazine impurity, tap density, cold water dispersion row, dye cloth after WICIE value, WG value be all better than the white dyes of traditional technology production.
Embodiment
Embodiment 1
Add water 500L in reactor, add trash ice 800Kg, be 1.5 with hydrochloric acid adjust pH, throw cyanuric chloride 100Kg, pull an oar 1 hour, then be the 100Kg4 of 10% by massfraction, 4 '-diaminobenzil-disulphonic acid adds in 2.5 hours in same reactor, it is 3 DEG C that temperature controls, be 6 by the sodium carbonate solution adjust ph that massfraction is 15%, carry out a contracting reaction to disappear to amino value, filter with 130 order stainless steel filtering nets, the material passed through from filter screen proceeds in reactor again, again 50.5Kg aniline is also dropped in same reactor, regulate pH to be 8 with the sodium hydroxide solution that massfraction is 25% simultaneously, carry out two contracting reactions to disappear to amino value, heat up 85 DEG C, press filtration after effect 1h, the filter cake obtained adds in the autoclave having 1300L deionized water again, after stirring evenly rear intensification 65 DEG C, add 56.69Kg morpholine, add 23Kg sodium hydrate solid, carry out three contracting reactions, 1.5h after, turn brilliant at 120 DEG C, turn brilliant rear press filtration, spraying dry is carried out after filter cake making beating, obtain white dyes.
The present invention can also according to arbitrary proportion value in following ranges:
The preparation method of the efficient low impurity white dyes of a kind of ultrawhite, in molar ratio 1:2 get that massfraction is 10 ~ 15% 4, 4 '-diaminobenzil-disulphonic acid and cyanuric chloride, in reactor, first add the frozen water of 10 ~ 15 times of cyanuric chloride weight, be 1 ~ 2 with salt acid for adjusting pH value, cyanuric chloride making beating 1 ~ 2h is added again in reactor, then 4 are dripped, 4 '-diaminobenzil-disulphonic acid, it is 0 ~ 5 DEG C that temperature controls, be 4 ~ 6 by the sodium carbonate solution adjust ph that massfraction is 10 ~ 20%, carry out a contracting reaction to disappear to amino value, filter with 130 ~ 150 mesh filter screens, the material passed through from filter screen proceeds in reactor again, then 1.95 ~ 2.1 times 4 is added in a kettle., the aniline of 4 '-diaminobenzil-disulfonic acid molar weight, pH is regulated to be 7 ~ 9 with the sodium hydroxide solution that massfraction is 20 ~ 30%, carry out two contracting reactions to disappear to amino value, heat up 80 ~ 90 DEG C, press filtration after effect 1 ~ 1.5h, the filter cake obtained adds in the autoclave of the deionized water of 10 ~ 15 times of cyanuric chloride weight again, stir evenly rear intensification 60 ~ 70 DEG C, add 2.3 ~ 2.6 times 4, the morpholine of 4 '-diaminobenzil-disulfonic acid molar weight, 2.1 ~ 2.3 times 4, the sodium hydrate solid of 4 '-diaminobenzil-disulfonic acid molar weight carries out three contracting reactions, after 1.5 ~ 2h, carry out turning brilliant, press filtration, dry, obtain white dyes.
Claims (1)
1. the preparation method of the efficient low impurity white dyes of ultrawhite, it is characterized in that: in molar ratio 1:2 get that massfraction is 10 ~ 15% 4, 4 '-diaminobenzil-disulphonic acid and cyanuric chloride, in reactor, first add the frozen water of 10 ~ 15 times of cyanuric chloride weight, be 1 ~ 2 with salt acid for adjusting pH value, cyanuric chloride making beating 1 ~ 2h is added again in reactor, then 4 are dripped, 4 '-diaminobenzil-disulphonic acid, it is 0 ~ 5 DEG C that temperature controls, be 4 ~ 6 by the sodium carbonate solution adjust ph that massfraction is 10 ~ 20%, carry out a contracting reaction to disappear to amino value, filter with 130 ~ 150 mesh filter screens, the material passed through from filter screen proceeds in reactor again, then 1.95 ~ 2.1 times 4 is added in a kettle., the aniline of 4 '-diaminobenzil-disulfonic acid molar weight, pH is regulated to be 7 ~ 9 with the sodium hydroxide solution that massfraction is 20 ~ 30%, carry out two contracting reactions to disappear to amino value, heat up 80 ~ 90 DEG C, press filtration after effect 1 ~ 1.5h, the filter cake obtained adds in the autoclave of the deionized water of 10 ~ 15 times of cyanuric chloride weight again, stir evenly rear intensification 60 ~ 70 DEG C, add 2.3 ~ 2.6 times 4, the morpholine of 4 '-diaminobenzil-disulfonic acid molar weight, 2.1 ~ 2.3 times 4, the sodium hydrate solid of 4 '-diaminobenzil-disulfonic acid molar weight carries out three contracting reactions, after 1.5 ~ 2h, carry out turning brilliant, press filtration, dry, obtain white dyes.
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| 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 |
| CN111809443B (en) * | 2020-07-22 | 2022-11-04 | 浙江传化华洋化工有限公司 | Modified fluorescent whitening agent aqueous solution and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (3)
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| 浅谈荧光增白剂CXT的生产工艺过程;宋玮等;《第九届全国染料与染色学术研讨会暨信息发布会论文集》;20041130;103-105 * |
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