CN101161805B - Method for preparing high-qualityparticulate fluorescent whitening agent - Google Patents
Method for preparing high-qualityparticulate fluorescent whitening agent Download PDFInfo
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- CN101161805B CN101161805B CN2007101395249A CN200710139524A CN101161805B CN 101161805 B CN101161805 B CN 101161805B CN 2007101395249 A CN2007101395249 A CN 2007101395249A CN 200710139524 A CN200710139524 A CN 200710139524A CN 101161805 B CN101161805 B CN 101161805B
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- reaction
- heavy metal
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- amount
- triazine
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- 238000000034 method Methods 0.000 title description 4
- 239000006081 fluorescent whitening agent Substances 0.000 title description 2
- 229910001385 heavy metal Inorganic materials 0.000 claims abstract description 18
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical compound C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 239000012065 filter cake Substances 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims description 28
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 11
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 10
- 238000010009 beating Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000000975 dye Substances 0.000 claims description 6
- QPCDCPDFJACHGM-UHFFFAOYSA-N N,N-bis{2-[bis(carboxymethyl)amino]ethyl}glycine Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(=O)O)CCN(CC(O)=O)CC(O)=O QPCDCPDFJACHGM-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000007795 chemical reaction product Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 3
- 239000012745 toughening agent Substances 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 239000003595 mist Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 150000002780 morpholines Chemical class 0.000 claims description 2
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 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 1
- 230000001105 regulatory effect Effects 0.000 claims 1
- 239000000047 product Substances 0.000 abstract description 20
- 239000012535 impurity Substances 0.000 abstract description 6
- 239000000428 dust Substances 0.000 abstract description 4
- 238000005469 granulation Methods 0.000 abstract description 4
- 230000003179 granulation Effects 0.000 abstract description 4
- 239000008187 granular material Substances 0.000 abstract description 2
- 230000008602 contraction Effects 0.000 abstract 2
- 238000010923 batch production Methods 0.000 abstract 1
- 239000007844 bleaching agent Substances 0.000 abstract 1
- 238000005194 fractionation Methods 0.000 abstract 1
- 238000004537 pulping Methods 0.000 abstract 1
- 239000012744 reinforcing agent Substances 0.000 abstract 1
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Chemical compound C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- 238000001914 filtration Methods 0.000 description 4
- 238000004945 emulsification Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229920000191 poly(N-vinyl pyrrolidone) Polymers 0.000 description 3
- 239000011435 rock Substances 0.000 description 3
- 230000002087 whitening effect Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 239000000271 synthetic detergent Substances 0.000 description 2
- 238000004383 yellowing Methods 0.000 description 2
- -1 DSD acid Chemical class 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal 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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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Detergent Compositions (AREA)
Abstract
The invention relates to the preparation method of high quality fluorescent bleaching agent (granular CXT) and is characterized in that an amount of heavy metal remover and triazine remover are added during primary contraction and third contraction; moreover, an amount of granule reinforcing agent is added in an obtained filter cake for mixed pulping; finally, object product is obtained after atomizing granulation, fractionation and standardization. The obtained granular product realizes substantial reduction in triazine impurity content and heavy metal content and greatly increases bulk density, thereby avoiding the dust pollution during processing and use of the product and the harm to human body and the environment caused by heavy metal; moreover, the invention has simple preparation method and is easy to operate, thereby being suitable for batch production.
Description
Affiliated technical field:
The present invention relates to the preparation method of the industrial chemicals that synthetic detergent and dyeing use, is the preparation method of a kind of high-qualityparticulate fluorescent whitening agent (particulate state CXT) specifically.
Background technology:
White dyes CXT is one of most important kind in the two triazines whitening agent structures of toluylene, it has good whitening effect, placed not yellowing for a long time by its product that brightens, and have high temperature resistant typing, alkaline-resisting, oxytolerant floats, anti-chlorine floats, fast light good advantage, is mainly used in synthetic detergent and dyeing.Yet, the present powder-type CXT that comes out according to produced in conventional processes, 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) content and heavy metal content height are produced, are used and pollute shortcomings such as bigger; And amounts of triazine is low, and the environment-friendly type that heavy metal content is low, the granule type CXT that added value is high but because of the technical requirements height, and can not produce, and can't satisfy the demand of domestic and international market.
The powder-type white dyes CXT that traditional processing technology prepares has following defective:
(1) impurity (triazine) content height (〉=2%), (2) heavy metal ion content higher (in iron ion 〉=200ppm), the little (≤360kg/m of (3) product tap density
3), (4) dust easily flies upward, pollutes big.
Summary of the invention:
The objective of the invention is to provide a kind of preparation method of particulate state white dyes for the whitening agent industry, both can reduce because of producing and using the dust pollution that brings, and can make amounts of triazine (≤0.6%), heavy metal content again (in iron ion≤50ppm) and tap density (〉=450kg/m
3) controlled, reach the level of the expensive goods that western countries require.
Production technique of the present invention: got DSD acid and cyanuric chloride in 1: 2 in molar ratio and put into reactor, add an amount of frozen water, adjusting pH value is 1-3, temperature 0-10 ℃, carries out the reaction of contracting then.In the reaction process, add an amount of heavy metal remover, after the reaction to terminal, add 2 moles of aniline, an amount of Na
2CO
3Carry out two reactions of contracting, until reaction end, then reaction product is gone to three and contract in the reactor, add 2.5 moles of morpholines, an amount of NaOH and triazine remover, carry out three reactions of contracting, after reaction to terminal, change brilliant again, then with the reaction product press filtration, carry out heavy metal, material, liquid separation, filter cake goes to the making beating pot and adds an amount of particle toughener mixing making beating, carries out mist projection granulating, classification, stdn then, finally obtains target compound.
The heavy metal remover is any of heavy metal chelant of ethylenediamine tetraacetic acid (EDTA) (EDTA), diethylene triamine pentacetic acid (DTPA) (DTPA), nitrilotriacetic acid (NTA), and its consumption is 2-5% (mass ratio).The triazine remover is a sulfuric acid, and its consumption is 2.7-5.8% (mass ratio).The particle toughener is an Xylo-Mucine, and its consumption is 0.4-1.0% (mass ratio).
Advantage of the present invention is: by improving production technique; Powdered white dyes is carried out granulating; significantly reduce the triazine impurity and the heavy metal content of product; improve tap density greatly; the dust pollution of having avoided product to produce in processing and use of success, minimizing triazine impurity is to the harm to human body and environment of the influence of quality product yellowing and various heavy.And this preparation method is simple, and is easy to operate, easily produces in batches.
Embodiment
Further specify the present invention by the following examples:
Embodiment 1: coventional type particulate state CXT product:
In reactor, add 1000 liters in water, 800kg on the rocks, transfer PH=1-3, throw cyanuric chloride 100kg, peregal 300g, emulsification 1 hour, under 0-10 ℃, carry out the reaction of contracting, the pure product DSD of the 98kg acid of being dissolved into 10% was knocked down in 2 hours in the same reactor, after the reaction to terminal, again 48.5kg aniline is also knocked down in the same reactor, carry out two reactions of contracting, after the reaction to terminal, will react feed liquid and be transferred to three and contract in the reactor, in alkaline medium, add morpholine 50kg, change brilliant in 130 ℃, with the feed liquid cooling, press filtration separates after the brilliant end of commentaries on classics, the making beating in the making beating pot of resulting filter cake, deliver to prilling tower 250 ℃ of granulations with surge pump then, carry out classification then, stdn obtains qualified product.
Products obtained therefrom is the usual production of the domestic industry standard of a kind of HG/T3675-2000 of meeting.Though reached granulated purpose, fail effectively to remove beavy metal impurity (in iron ion 〉=200ppm), amounts of triazine (〉=2%), and tap density (350-380kg/m
3) all not up to standard.
Embodiment 2: modified version particulate state CXT product:
In reactor, add 1000 liters in water, 800kg on the rocks, transfer PH=1-3, throw cyanuric chloride 100kg, peregal 300g, emulsification 1 hour, under 0-10 ℃, carry out the reaction of contracting, the pure product DSD of the 98kg acid of being dissolved into 10% was knocked down in 2 hours in the same reactor, when reaction nearly finishes, add ethylenediamine tetraacetic acid (EDTA) (EDTA) 25kg, after the reaction to terminal.Again 48.5kg aniline is also knocked down in the same reactor, carried out two reactions of contracting, after the reaction to terminal, to react feed liquid and be transferred to three and contract in the reactor, in alkaline medium, add morpholine 50kg, add sulfuric acid 10kg simultaneously, change brilliant in 130 ℃, with the feed liquid cooling, press filtration separates with heavy metal to carry out feed liquid again after the brilliant end of commentaries on classics, the making beating in the making beating pot of resulting filter cake, deliver to prilling tower 250 ℃ of granulations with surge pump then, carry out classification, stdn then, obtain qualified product.
Products obtained therefrom has effectively been removed heavy metal (so that iron ion≤50ppm), amounts of triazine (≤0.6%) all reaches the level of American-European demand, but its tap density (350-380kg/m
3) still below standard.
Embodiment 3: high-qualityparticulate CXT product:
In reactor, add 1000 liters in water, 800kg on the rocks, transfer PH=1-3, throw cyanuric chloride 100kg, peregal 300g, emulsification 1 hour, under 0-10 ℃, carry out the reaction of contracting, the pure product DSD of the 98kg acid of being dissolved into 10% was knocked down in 2 hours in the same reactor, when reaction finishes, added ethylenediamine tetraacetic acid (EDTA) (EDTA) 25kg nearly, after the reaction to terminal, again 48.5kg aniline is also knocked down in the same reactor, carried out two reactions of contracting, after the reaction to terminal, to react feed liquid is transferred to three and contracts in the reactor, in alkaline medium, add morpholine 50kg, add sulfuric acid 10kg simultaneously, change brilliant in 130 ℃, after changeing brilliant the end feed liquid is cooled off, press filtration separates with heavy metal to carry out feed liquid again, the making beating in the making beating pot of resulting filter cake, and in time add the 10kg Xylo-Mucine, deliver to prilling tower 250 ℃ of granulations with surge pump then, carry out classification then, stdn obtains high-quality product.
With the high-qualityparticulate product of this explained hereafter gained, quality had both surpassed domestic industry standard level, and its 10 heavy metal species element (in iron ion≤50ppm), amounts of triazine (≤0.6%), and bulk density (450-500kg/m
3), also all reach American-European countries's required standard, satisfy export requirement fully.
Claims (1)
1. the preparation method of a particulate state white dyes, it is characterized in that: got 4 in 1: 2 in molar ratio, 4 '-diaminobenzil-2,2 '-disulfonic acid and cyanuric chloride put into reactor, add an amount of frozen water, regulating pH value is 1～3,5～10 ℃ of temperature are carried out the reaction of contracting, in the reaction process then, add heavy metal remover ethylenediamine tetraacetic acid (EDTA) or diethylene triamine pentacetic acid (DTPA) or nitrilotriacetic acid, mass ratio is 2～5%; After the reaction to terminal, add 2 moles of aniline, an amount of Na
2CO
3Carry out two reactions of contracting, until reaction end; Then reaction product is gone to three and contract in the reactor, add 2.5 moles of morpholines, an amount of NaOH and mass ratio and be 2.7～2.8% triazine remover sulfuric acid, carry out three reactions of contracting, after reaction to terminal, change brilliant again, then reaction product is filtered, carry out heavy metal, material, liquid separation; Filter cake goes to the making beating pot, adds the particle toughener Xylo-Mucine mixing making beating of mass ratio 0.4～1.0%, carries out mist projection granulating, classification, stdn then, finally obtains target compound.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101395249A CN101161805B (en) | 2007-09-28 | 2007-09-28 | Method for preparing high-qualityparticulate fluorescent whitening agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101395249A CN101161805B (en) | 2007-09-28 | 2007-09-28 | Method for preparing high-qualityparticulate fluorescent whitening agent |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101161805A CN101161805A (en) | 2008-04-16 |
| CN101161805B true CN101161805B (en) | 2010-06-23 |
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ID=39296790
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2007101395249A Active CN101161805B (en) | 2007-09-28 | 2007-09-28 | Method for preparing high-qualityparticulate fluorescent whitening agent |
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| CN (1) | CN101161805B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101367770B (en) * | 2008-09-26 | 2012-07-04 | 贺明波 | Preparation method for fluorescent whitening agent |
| CN102911127B (en) * | 2012-10-26 | 2014-12-03 | 山西青山化工有限公司 | Preparation method for low-triazine fluorescent whitening agent |
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2007
- 2007-09-28 CN CN2007101395249A patent/CN101161805B/en active Active
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| Publication number | Publication date |
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| CN101161805A (en) | 2008-04-16 |
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| ASS | Succession or assignment of patent right |
Owner name: WANG XIANG Free format text: FORMER OWNER: SHANXI KINGSUN CHEMICAL CO., LTD. Effective date: 20100326 |
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| C41 | Transfer of patent application or patent right or utility model | ||
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Inventor after: Wang Xiang Inventor before: Yang Yu Inventor before: Wang Xinliang |
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| COR | Change of bibliographic data |
Free format text: CORRECT: INVENTOR; FROM: YANG YU WANG XINLIANG TO: WANG XIANG Free format text: CORRECT: ADDRESS; FROM: 044102 NO.888, HIGH-TCH INDUSTRIAL PARK, LINYI COUNTY, YUNCHENG CITY, SHANXI PROVINCE TO: 044100 EAST OF FLOOR 1, UNIT 3, BUILDING 7, AREA 4, FERTILIZER FACTORY, LINYI COUNTY, YUNCHENG CITY, SHANXI PROVINCE |
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Effective date of registration: 20100326 Address after: Yuncheng City, Shanxi province 044100 Chemical Fertilizer Factory Linyi County four District 7 building three unit on the first floor of the East Applicant after: Wang Xiang Address before: Hi tech Industrial Park, 044102 Shanxi city of Yuncheng Province Linyi County No. 888 Applicant before: Shanxi Kingsun Chemical Co., Ltd. |
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Effective date of registration: 20180314 Address after: 044100 Shanxi city of Yuncheng Province Linyi hi tech Industrial Park, No. 888 Patentee after: Shanxi Jinguang Chemical Co., Ltd. Address before: Yuncheng City, Shanxi province 044100 Chemical Fertilizer Factory Linyi County District Four 7 floor three unit on the first floor of the East Patentee before: Wang Xiang |
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| TR01 | Transfer of patent right |