CN104262990A - Preparation method of suspension of fluorescent whitening agent - Google Patents
Preparation method of suspension of fluorescent whitening agent Download PDFInfo
- Publication number
- CN104262990A CN104262990A CN201410489537.9A CN201410489537A CN104262990A CN 104262990 A CN104262990 A CN 104262990A CN 201410489537 A CN201410489537 A CN 201410489537A CN 104262990 A CN104262990 A CN 104262990A
- Authority
- CN
- China
- Prior art keywords
- formula
- preparation
- suspension
- quality
- fluorescent whitening
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 0 C*c1c(C=C[C@@]2C=CC(NC3=NC(N(CCC(N)=O)CCO)=NC(Nc4ccccc4)N3)=CC2*)ccc(Nc2nc(NCCO)nc(Nc3ccccc3)n2)c1 Chemical compound C*c1c(C=C[C@@]2C=CC(NC3=NC(N(CCC(N)=O)CCO)=NC(Nc4ccccc4)N3)=CC2*)ccc(Nc2nc(NCCO)nc(Nc3ccccc3)n2)c1 0.000 description 3
Abstract
The invention discloses a preparation method of a suspension of a fluorescent whitening agent. The fluorescent whitening agent is a whitening aid for paper, and liquid products of the fluorescent whitening agent are generally used on the market, but because the solubility of the fluorescent whitening agent is low, more than 15% of urea or other cosolvents are added into each product so as to maintain the stability of the product. According to the preparation method disclosed by the invention, by using the characteristics that a disulfonic fluorescent whitening agent has good water solubility at relatively high temperature and relatively low water solubility at low temperature, a suspension protecting agent and an antifreezing agent are added into a high-concentration system with a separated-out disulfonic fluorescent whitening agent, and then the obtained mixture is ground, so that a stable suspension can be obtained.
Description
Technical field
The present invention relates to paper making additive field, specifically a kind of preparation method of disulfonic acid fluorescent whitening agent suspension.
Background technology
White dyes is a kind of paper making additive promoting Paper White Degree, in paper pulp brightens, widely use diphenylethylene disulfonic acid fluorescent whitening agent, but the sulfonation degree of this fluorescent bleaches is low, water-soluble not good at normal temperatures, therefore in the process of preparing product, often need the urea or other solubility promoter that add more than 15%, just can obtain stable liquid product, and urea increases the ammonia-nitrogen content of paper organic waste water, therefore, paper plant needs the certain energy and financial resources of cost to go to administer waste water, can qualified discharge.
EP0884312 discloses a kind of preparation method of fluorescent brightening agent dispersing liquid.The method by acid out, neutralization, evaporate or add ionogen and obtain that there is 4 of specific crystalline form, 4 '-two-triazine radical amido-2,2 '-disulfonic acid stilbene compound, then adds the dispersion liquid that thickening stabilizer homogeneous obtains white dyes.The method needs, by acid out link, be unfavorable for cleaner production, and process to be comparatively complicated.
Summary of the invention
Technical problem to be solved by this invention is the defect overcoming the existence of above-mentioned prior art; a kind of preparation method of disulfonic acid fluorescent whitening agent suspension is provided; low water solubility feature under it utilizes disulfonic acid fluorescent whitening agent to have good water-soluble, lesser temps at relatively high temperatures; in high density and have disulfonic acid fluorescent whitening agent separate out system in add suspension protective material and frostproofer, by grinding can obtain stable suspension.
For this reason, the present invention adopts following technical scheme: a kind of preparation method of disulfonic acid fluorescent whitening agent suspension, and its step is as follows: first, obtains the first step product by DSD acid and cyanuric chloride condensation, then adds aniline condensation and obtain second step product; Then, at reflux, fat primary amine is added or/and fatty primary secondary amine condensation obtains disulfonic acid fluorescent whitening agent; Then, nanofiltration concentrates and obtains the transparent formula A material aqueous solution of high density, and cooling makes formula A material separate out; Finally, in this system, add suspension protective material and frostproofer, obtain the stable white dyes suspension containing formula A material by grinding,
Described formula A material is the material of single structure or the mixture of various structures, in formula A, and M
1, M
2for respective independently Na
+, Li
+, Mg
2+, Al
3+or NH
4 +, in formula A, R
1, R
2, R
3and R
4for respective independently hydrogen, C
1-C
4alkyl, C
1-C
4hydroxyalkyl or C
2-C
4amidoalkyl group.
The preferred structural formula of formula A has:
As preferably, M
1, M
2for Na
+, fat primary amine is or/and fatty primary secondary amine is one or more the mixture in 3-[(2-hydroxyethyl) is amino] propionic acid amide, Monoethanolamine MEA BASF, diethanolamine.
As preferably, the thickening temperature adopted when nanofiltration concentrates is 65-80 DEG C.
As preferably, the quality that nanofiltration concentrates containing formula A material in the formula A material aqueous solution obtained is 10-40%, is more preferably 20-30%.
As preferably, it is 8.0-11.0 that nanofiltration concentrates the formula A material pH value of water solution obtained.
As preferably, described suspension protective material is glue class thickening material, cellulose thickener, mineral-type thickening material or polymerization macromolecule class thickening material, and the suspension protective material quality that it adds is the 0.1-6% of formula A material mass; Described suspension protective material be more preferably in wilkinite, Walocel MT 20.000PV, polyvinyl alcohol, guar gum, xanthan gum, gelatin one or more, the suspension protective material quality that it adds is more preferably the 0.5-3.5% of formula A material mass.
As preferably, the frostproofer quality added is the 1-10% of the quality of formula A material.
As preferably, described frostproofer is one or more in ethylene glycol, propylene glycol, glycerol, and its quality is the 3-5% of the quality of formula A material.
As preferably, the mass concentration of white dyes suspension Chinese style A material is 5-35%.
Present invention utilizes disulfonic acid fluorescent whitening agent there is good water-soluble, lesser temps at relatively high temperatures under low water solubility feature; in high density and have disulfonic acid fluorescent whitening agent separate out system in add suspension protective material and frostproofer, finally by grinding can obtain stable suspension.Preparation process easily controls, and reaches the object of cleaner production.
Embodiment
Embodiment 1
(1) in four-hole bottle, 3000ml mixture of ice and water is added.
(2) add 0.650mol cyanuric chloride and 0.319mol DSD acid, control temperature≤2 DEG C, pH value≤2.5, obtain a step product.
(3) add 0.650mol aniline, control temperature 20-30 DEG C, pH value 4-5, obtain secondary product.
(4) add 0.715mol 3-[(2-hydroxyethyl) is amino] propionic acid amide, control temperature 100 DEG C backflow, pH value 8-11, obtains (A1) solution.
(5) the concentrated concentrated solution obtained containing (A1) 26.2% of nanofiltration.
(6) be cooled to 20 DEG C, obtain the saturated solution of separating out containing (A1).
Embodiment 2
Take embodiment 1 (A1) saturated solution 100g, add 0.5g Walocel MT 20.000PV and 1g ethylene glycol, grinding obtains containing (A1) suspension.
Embodiment 3
Take embodiment 1 (A1) saturated solution 100g, add 0.4g polyvinyl alcohol and 1g ethylene glycol, grinding obtains containing (A1) suspension.
Embodiment 4
Take embodiment 1 (A1) saturated solution 100g, add 0.27g gelatin and 1g propylene glycol, grinding obtains containing (A1) suspension.
Embodiment 5
(1) in four-hole bottle, 3000ml mixture of ice and water is added.
(2) add 0.650mol cyanuric chloride and 0.319mol DSD acid, control temperature≤2 DEG C, pH value≤2.5, obtain a step product.
(3) add 0.650mol aniline, control temperature 20-30 DEG C, pH value 4-5, obtain secondary product.
(4) add the mixture of 0.715mol 3-[(2-hydroxyethyl) is amino] propionic acid amide and Monoethanolamine MEA BASF, control temperature 100 DEG C backflow, pH value 8-10.5, obtains (A1) (A2) (A3) solution.
(5) the concentrated concentrated solution obtained containing (A1) (A2) (A3) 24% of nanofiltration.
(6) be cooled to 10 DEG C, obtain the saturated solution of separating out containing (A1) (A2) (A3).
Embodiment 6
Take embodiment 5 (A1) (A2) (A3) saturated solution 100g, add 0.8g Walocel MT 20.000PV and 1.0g glycerol, grinding obtains containing (A1) (A2) (A3) suspension.
Embodiment 7
Take embodiment 5 (A1) (A2) (A3) saturated solution 100g, add 0.7g wilkinite and 2.0g propylene glycol, grinding obtains containing (A1) (A2) (A3) suspension.
Embodiment 8
(1) in four-hole bottle, 3000ml mixture of ice and water is added.
(2) add 0.650mol cyanuric chloride and 0.319mol DSD acid, control temperature≤2 DEG C, pH value≤2.5, obtain a step product.
(3) add 0.650mol aniline, control temperature 20-30 DEG C, pH value 4-5, obtain secondary product.
(4) add the mixture of 0.715mol diethanolamine, control temperature 100 DEG C backflow, pH value 9-10, obtains (A5) solution.
(5) the concentrated concentrated solution obtained containing (A5) 25% of nanofiltration.
(6) be cooled to 15 DEG C, obtain the saturated solution of separating out containing (A5).
Embodiment 9
Take embodiment 8 (A5) saturated solution 100g, add 0.6g Walocel MT 20.000PV and 1.0g propylene glycol, grinding obtains containing (A5) suspension.
Embodiment 10
Take embodiment 8 (A5) saturated solution 100g, add 0.24g gelatin and 1.2g ethylene glycol, grinding obtains containing (A5) suspension.
Embodiment 11
Take embodiment 5 (A1) (A2) (A3) saturated solution 33g and embodiment 8 (A5) saturated solution 67g to mix, add 0.24g guar gum and 1.0g ethylene glycol, grinding obtains containing (A1) (A2) (A3) (A5) suspension.
Embodiment 12
Take embodiment 5 (A1) (A2) (A3) saturated solution 34g and embodiment 8 (A5) saturated solution 66g to mix, add 0.6g hydroxylmethyl cellulose and 1.2g propylene glycol, homogeneous obtains containing (A1) (A2) (A3) (A5) suspension.
Embodiment 13
(1) in four-hole bottle, 3000ml mixture of ice and water is added.
(2) add 0.650mol cyanuric chloride and 0.319mol DSD acid, control temperature≤2 DEG C, pH value≤2.5, obtain a step product.
(3) add 0.650mol aniline, control temperature 20-30 DEG C, pH value 4-5, obtain secondary product.
(4) add the mixture of 0.715mol 3-[(2-hydroxyethyl) is amino] propionic acid amide and diethanolamine, control temperature 100 DEG C backflow, pH value 8-10, obtains (A1) (A4) (A5) solution.
(5) the concentrated concentrated solution obtained containing (A1) (A4) (A5) 28% of nanofiltration.
(6) be cooled to 20 DEG C, obtain the saturated solution of separating out containing (A1) (A4) (A5).
Embodiment 14
Take embodiment 13 (A1) (A4) (A5) saturated solution 100g, add 0.6g wilkinite and 1.0g propylene glycol, homogeneous obtains containing (A1) (A4) (A5) suspension.
Stability is tested
Application performance
The above is only preferred embodiment of the present invention, not does any pro forma restriction to technical scheme of the present invention.Every above embodiment is done according to technical spirit of the present invention any simple modification, equivalent variations and modification, all fall within the scope of protection of the present invention.
Claims (10)
1. a preparation method for disulfonic acid fluorescent whitening agent suspension, its step is as follows: first, obtains the first step product by DSD acid and cyanuric chloride condensation, then adds aniline condensation and obtain second step product; Then, at reflux, fat primary amine is added or/and fatty primary secondary amine condensation obtains disulfonic acid fluorescent whitening agent; Then, nanofiltration concentrates and obtains the transparent formula A material aqueous solution of high density, and cooling makes formula A material separate out; Finally, in this system, add suspension protective material and frostproofer, obtain the stable white dyes suspension containing formula A material by grinding,
Described formula A material is the material of single structure or the mixture of various structures, in formula A, and M
1, M
2for respective independently Na
+, Li
+, Mg
2+, Al
3+or NH
4 +, in formula A, R
1, R
2, R
3and R
4for respective independently hydrogen, C
1-C
4alkyl, C
1-C
4hydroxyalkyl or C
2-C
4amidoalkyl group.
2. preparation method according to claim 1, is characterized in that, the thickening temperature adopted when nanofiltration concentrates is 65-80 DEG C.
3. preparation method according to claim 1, is characterized in that, the quality that nanofiltration concentrates containing formula A in the formula A material aqueous solution obtained is 10-40%.
4. preparation method according to claim 3, is characterized in that, the quality that nanofiltration concentrates containing formula A material in the formula A material aqueous solution obtained is 20-30%.
5. preparation method according to claim 1, is characterized in that, it is 8.0-11.0 that nanofiltration concentrates the formula A material pH value of water solution obtained.
6. preparation method according to claim 1; it is characterized in that; described suspension protective material is glue class thickening material, cellulose thickener, mineral-type thickening material or polymerization macromolecule class thickening material, and the suspension protective material quality that it adds is the 0.1-6% of formula A material mass.
7. preparation method according to claim 6; it is characterized in that; described suspension protective material is one or more in wilkinite, Walocel MT 20.000PV, polyvinyl alcohol, guar gum, xanthan gum, gelatin, and the suspension protective material quality that it adds is the 0.5-3.5% of formula A material mass.
8. preparation method according to claim 1, is characterized in that, the frostproofer quality added is the 1-10% of the quality of formula A material.
9. preparation method according to claim 8, it is characterized in that, described frostproofer is one or more in ethylene glycol, propylene glycol, glycerol, and its add-on is the 3-5% of formula A quality.
10. preparation method according to claim 1, is characterized in that, the mass concentration of white dyes suspension Chinese style A material is 5-35%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410489537.9A CN104262990A (en) | 2014-09-23 | 2014-09-23 | Preparation method of suspension of fluorescent whitening agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410489537.9A CN104262990A (en) | 2014-09-23 | 2014-09-23 | Preparation method of suspension of fluorescent whitening agent |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104262990A true CN104262990A (en) | 2015-01-07 |
Family
ID=52154581
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410489537.9A Pending CN104262990A (en) | 2014-09-23 | 2014-09-23 | Preparation method of suspension of fluorescent whitening agent |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104262990A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110857418A (en) * | 2018-08-25 | 2020-03-03 | 山西晋光化工有限公司 | Novel liquid fluorescent whitening agent |
| CN113463368A (en) * | 2021-08-02 | 2021-10-01 | 浙江宏达化学制品有限公司 | CXT liquid fluorescent whitening agent and preparation method thereof |
| CN113638219A (en) * | 2021-08-20 | 2021-11-12 | 奥仕集团有限公司 | Preparation method of low-temperature-resistant fluorescent whitening slurry |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3012971A (en) * | 1959-04-07 | 1961-12-12 | Du Pont | Whitening composition for paper |
| CN1802465A (en) * | 2003-06-11 | 2006-07-12 | 西巴特殊化学品控股有限公司 | Storage-stable fluorescent whitener formulations |
| CN101372819A (en) * | 2007-08-23 | 2009-02-25 | 南通丽思化学助剂有限公司 | Method for producing fluorescent whitening agent |
| CN103254660A (en) * | 2013-05-20 | 2013-08-21 | 浙江传化华洋化工有限公司 | Preparation method of carbamide-free disulfonic acid triazinyl fluorescent whitening agent liquid |
-
2014
- 2014-09-23 CN CN201410489537.9A patent/CN104262990A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3012971A (en) * | 1959-04-07 | 1961-12-12 | Du Pont | Whitening composition for paper |
| CN1802465A (en) * | 2003-06-11 | 2006-07-12 | 西巴特殊化学品控股有限公司 | Storage-stable fluorescent whitener formulations |
| CN101372819A (en) * | 2007-08-23 | 2009-02-25 | 南通丽思化学助剂有限公司 | Method for producing fluorescent whitening agent |
| CN103254660A (en) * | 2013-05-20 | 2013-08-21 | 浙江传化华洋化工有限公司 | Preparation method of carbamide-free disulfonic acid triazinyl fluorescent whitening agent liquid |
Non-Patent Citations (1)
| Title |
|---|
| 吴飞 等: "双三嗪氨基二苯乙烯类液体荧光增白剂的合成与应用研究", 《中华纸业》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110857418A (en) * | 2018-08-25 | 2020-03-03 | 山西晋光化工有限公司 | Novel liquid fluorescent whitening agent |
| CN113463368A (en) * | 2021-08-02 | 2021-10-01 | 浙江宏达化学制品有限公司 | CXT liquid fluorescent whitening agent and preparation method thereof |
| CN113463368B (en) * | 2021-08-02 | 2023-09-26 | 浙江宏达化学制品有限公司 | CXT liquid fluorescent whitening agent and preparation method thereof |
| CN113638219A (en) * | 2021-08-20 | 2021-11-12 | 奥仕集团有限公司 | Preparation method of low-temperature-resistant fluorescent whitening slurry |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104262990A (en) | Preparation method of suspension of fluorescent whitening agent | |
| NZ578582A (en) | Electrochemical process for the preparation of halo amines such as monochloroamine | |
| CN102531991A (en) | Novel multi-amino functionalized ionic liquid and preparation method thereof | |
| AR106955A1 (en) | SYSTEMS AND METHODS TO IMPROVE THE RECOVERY OF CO-PRODUCTS FROM GRAINS AND / OR GRAIN COMPONENTS USED FOR BIOCHEMICAL AND / OR BIOFUEL PRODUCTION USING AGENTS THAT BREAK EMULSION | |
| CN102597374A (en) | Disulfo-type fluorescent whitening agents | |
| CN103265820B (en) | Method for preparing azo dye with alkalescent arylamine serving as diazotization ingredient | |
| RU2603392C2 (en) | Fluorescent whitening agent composition | |
| CN101309978B (en) | Liquid direct dye formulations | |
| CN103265223A (en) | Cement grinding aid | |
| DE19706238B4 (en) | Process for the preparation of substituted 4,4'-diaminostilbene-2,2'-disulfonic acids | |
| ES2254813T3 (en) | USE OF ETER-CARBOXILIC ACIDS WITH A LOW POINT OF SOLIDIFICATION. | |
| CN103865660A (en) | Enzymatic laundry powder | |
| MX2010005094A (en) | Nucleic acid complex and nucleic acid delivery composition. | |
| CN102806046A (en) | Green preparation method of quaternary ammonium salt surfactant | |
| CN103865669A (en) | Heavy-duty laundry detergent | |
| CN104940036B (en) | The preparation method of environment-friendly type large arch dam moisturizer | |
| DE102018201831A1 (en) | Detergent composition with yield value | |
| CN103923486A (en) | Toluylenetriazine pasty fluorescent brightener and preparation method thereof | |
| RU2564815C2 (en) | Method of production of white paper | |
| CN110950701A (en) | Production process of water flush fertilizer anticaking agent | |
| CN106609482A (en) | Packaging paper made of bamboo fiber | |
| RU2012124799A (en) | WATER DISPERSIONS | |
| CN107652196A (en) | A kind of removal technique of the glycine zine crystallization water | |
| CN108559103B (en) | Preparation method of nitro-straw extract and product | |
| CN104447448B (en) | The novel crystal forms and its crystallization preparation method of antioxidant 1035 |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20150107 |
|
| RJ01 | Rejection of invention patent application after publication |