CN103540448B - Preparation method for pasty stilbene biphenyl sodium disulfonate (CBS) fluorescent whitening agent - Google Patents
Preparation method for pasty stilbene biphenyl sodium disulfonate (CBS) fluorescent whitening agent Download PDFInfo
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Abstract
The invention belongs to a preparation method of a fluorescent whitening agent and particularly relates to a preparation method of a pasty stilbene biphenyl sodium disulfonate (CBS) fluorescent whitening agent. The fluorescent whitening agent disclosed by the invention is mainly used for solving the technical problem that existing CBS pasty fluorescent whitening agents are short in stable storage time. According to the technical scheme, the pasty CBS fluorescent whitening agent comprises the following raw materials in percentage by weight: 30-40% of 4, 4'-bis (2-sodium sulfonate styryl) biphenyl, 0.2-5% of dispersing agent, 0.1-2.0% of thickening agent, 0.2-5% of industrial salt, 0-5% of antifreeze agent, 0-0.5% of bactericide and 42.5-69.5% of deionized water. The preparation method of the pasty CBS fluorescent whitening agent comprises the four steps of crystal transformation, adding of auxiliaries, homogenizing and defoaming. The pasty CBS fluorescent whitening agent disclosed by the invention can be stably stored for at least 6 months and is simple in preparation process, low in cost and can be easily put into industrial production.
Description
Technical field
The invention belongs to the preparation method of white dyes, be specifically related to a kind of preparation method of pulpous state CBS white dyes.
Background technology
CBS white dyes, chemical name is 4, and 4 '-bis-(2-sodium sulfonate styryl) biphenyl, belongs to Stilbene-based Fluorescent Brighteners, dissolve rapidly because it has in cold water, fast light, resistance to drift and the easy advantage such as degraded, be widely used in brightening of the washing composition series products such as washing powder.At present, the formulation of CBS white dyes product is divided into four kinds, is powder, particle, liquid and pulpous state respectively; Wherein powder or particle CBS white dyes in use, all can produce certain dust pollution; Liquid and pulpous state CBS white dyes no dust pollution, use more environmental protection, realize Cemented filling by pump, be easy to automatic production, but liquid-type CBS fluorescent brightener levels generally can only accomplish 20%, and the amount of auxiliary of adding is large, and production cost is high.And pulpous state type CBS white dyes overcomes the above-mentioned shortcoming of liquid product, working substance content can be accomplished higher, reaches more than 30%, and the auxiliary agent cost of interpolation is much lower compared with liquid product.But there is certain problem in the technological development of pulpous state CBS white dyes at present.
Publication number be CN1802465A patent describes the two triazines white dyes of a kind of and another kind of toluylene in the two triazines white dyes of toluylene or with a kind of formula mixing soup compound of stilbene biphenyl white dyes and preparation method, white dyes stable storing prepared by this technology, but this patent does not relate to the soup compound of one-component fluorescent brightener CBS.
Publication number is the slurries that patent describes by direct high speed dispersion CBS filter cake of CN102408957B; add a certain proportion of protective colloid, frostproofer, defoamer again; obtain the CBS pasty products of working substance content 30%; only two months this product Absorbable organic halogens shelf-time, exist and stablize shelf-time short problem.
Summary of the invention
The object of the invention is to solve stable shelf-time that existing CBS pulpous state white dyes exists short technical problem, a kind of preparation method of pulpous state CBS white dyes is provided, pulpous state CBS white dyes Absorbable organic halogens prepared by the present invention deposits at least six months, and preparation technology is simple, cost is low, is easy to suitability for industrialized production.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
A kind of preparation method of pulpous state CBS white dyes, it is made up of the raw material of following weight percents: 4,4 '-bis-(2-sodium sulfonate styryl) biphenyl 30 ~ 40%, dispersion agent 0.2 ~ 5%, thickening material 0.1 ~ 2.0%, Industrial Salt 0.2 ~ 5%, antifreezing agent 0 ~ 5%, sterilant 0 ~ 0.5%, deionized water 42.5 ~ 69.5%; Comprise a turn crystalline substance, add auxiliary agent, homogenize and deaeration four steps, its preparation process is:
(1) turn brilliant and first add to turning in brilliant equipment the deionized water that weight percent is 42.5 ~ 69.5%, when stirring heating is warming up to 50 ~ 60 DEG C, then add that weight percent is 30 ~ 40% 4, 4 '-bis-(2-sodium sulfonate styryl) biphenyl, continue to be heated to 95 ~ 100 DEG C dissolve and be incubated 1 ~ 2h, ON cycle water coolant is down to 60 ~ 65 DEG C temperature of charge again, and be incubated 1 ~ 2h at this temperature, continue to pass into recirculated cooling water after insulation terminates, temperature of charge is slowly down to 30 ~ 35 DEG C, and be incubated more than 2h at this temperature, until use biomicroscope 160 times under observe crystal form major part for laminar crystallization till,
(2) add auxiliary agent to complete turn brilliant slurry in add successively weight percent be 0.2 ~ 5% dispersion agent, the weight percent thickening material that is 0.1 ~ 2.0%, the weight percent Industrial Salt that is 0.2 ~ 5%, weight percent be 0 ~ 5% antifreezing agent and weight percent be the sterilant of 0 ~ 0.5%, stir 30 minutes;
(3) homogenize and the slurry that with the addition of auxiliary agent is added in high speed beating equipment, pull an oar 30 ~ 60 minutes under mixing speed is 2500 ~ 3000rpm condition;
(4) slurry after above-mentioned homogenizing adds in vacuum defoamation machine and carries out deaeration 1h by deaeration, and deaeration is complete, and obtain pulpous state CBS white dyes product, product is put in the plastic tank of cleaning, keeps in Dark Place.
Above-mentioned dispersion agent is one or more mixtures in beta-naphthalenesulfonic-acid salt, NNO, MF or lignin sulfonate.
Above-mentioned thickening material is one or more mixtures in xanthan gum, carboxymethyl cellulose, cyclodextrin or polyvinylpyrrolidone.
Above-mentioned antifreezing agent is one or more mixtures in 1,2-PD, ethylene glycol or glycerol.
Above-mentioned sterilant is the one in CMIT or MIT.
The present invention adopts above technical scheme, the polymorphism characteristic utilizing CBS intrinsic: CBS has needle-like, the crystalline form such as bar-shaped and laminar, in preparation process, by the key factor such as strict temperature control and stirring velocity, guide CBS to turn brilliant, obtain and be conducive to the fluorescent brightener CBS that slurries stablize non-setting laminar crystalline form; Add dispersion agent and stablizer in fluorescent brightener CBS, utilize dispersion agent to the parcel stabilization of fine particle, prevent serous granule from forming macrobead because of cohesion and precipitating; In addition, the present invention additionally uses vacuum defoamation technology, decreases the input of auxiliary material, reduces production cost.Compared with background technology, pulpous state CBS white dyes prepared by the present invention has the advantage that Absorbable organic halogens is deposited at least six months, and preparation technology is simple, cost is low, is easy to suitability for industrialized production.
Embodiment
Embodiment 1
Pulpous state CBS white dyes in the present embodiment, it is made up of the raw material of following weight percents:
The preparation method of above-mentioned pulpous state CBS white dyes, comprise a turn crystalline substance, add auxiliary agent, homogenize and deaeration four steps, its preparation method is:
(1) turn crystalline substance and first add 626Kg deionized water to turning in brilliant equipment, when stirring heating is warming up to 50 ~ 60 DEG C, then 300Kg 4 is added, 4 '-bis-(2-sodium sulfonate styryl) biphenyl, continue to be heated to 95 ~ 100 DEG C dissolve and be incubated 1h, ON cycle water coolant is down to 60 ~ 65 DEG C temperature of charge again, and be incubated 1h at this temperature, continue to pass into recirculated cooling water after insulation terminates, temperature of charge is slowly down to 30 ~ 35 DEG C, and be incubated 6h at this temperature, observing crystal form major part under using biomicroscope 160 times is laminar crystallization,
(2) add auxiliary agent and add sodiumβ-naphthalenesulfonate 1.0Kg, NNO 1.0Kg, xanthan gum 20Kg, Industrial Salt 2Kg, ethylene glycol 25Kg and 1 successively to completing in turn brilliant slurry, 2-propylene glycol 25Kg, stir 30 minutes, ethylene glycol and 1,2-propylene glycol addition adjusts according to the change of weather, can add during temperature height in summer;
(3) homogenize and the slurry that with the addition of auxiliary agent is added in high speed beating equipment, pull an oar 30 minutes under mixing speed is 2500 ~ 3000rpm condition;
(4) slurry after above-mentioned homogenizing adds in vacuum defoamation machine and carries out deaeration 1h by deaeration, and deaeration is complete, and obtain pulpous state CBS white dyes product, product is put in the plastic tank of cleaning, keeps in Dark Place.
After depositing 205 days under room temperature, through observing slurries, there is not obvious demixing phenomenon.
Embodiment 2
Pulpous state CBS white dyes in the present embodiment, it is made up of the raw material of following weight percents:
The preparation method of above-mentioned pulpous state CBS white dyes, comprise a turn crystalline substance, add auxiliary agent, homogenize and deaeration four steps, its preparation method is:
(1) turn crystalline substance and first add 593Kg deionized water to turning in brilliant equipment, when stirring heating is warming up to 50 ~ 60 DEG C, then 350Kg4 is added, 4 '-bis-(2-sodium sulfonate styryl) biphenyl, continue to be heated to 95 ~ 100 DEG C dissolve and be incubated 1.5h, ON cycle water coolant is down to 60 ~ 65 DEG C temperature of charge again, and be incubated 1.5h at this temperature, continue to pass into recirculated cooling water after insulation terminates, temperature of charge is slowly down to 30 ~ 35 DEG C, and be incubated 4h at this temperature, observing crystal form major part under using biomicroscope 160 times is laminar crystallization,
(2) add auxiliary agent and add sodiumβ-naphthalenesulfonate 10Kg, MF 5.0Kg, cyclodextrin 12Kg, Industrial Salt 25Kg and CMIT 5.0Kg successively to completing in turn brilliant slurry, stir 30 minutes, CMIT addition, according to the situation of weather, can adjust in right amount;
(3) homogenize and the slurry that with the addition of auxiliary agent is added in high speed beating equipment, pull an oar 40 minutes under mixing speed is 2500 ~ 3000rpm condition;
(4) slurry after above-mentioned homogenizing adds in vacuum defoamation machine and carries out deaeration 1h by deaeration, and deaeration is complete, and obtain pulpous state CBS white dyes product, product is put in the plastic tank of cleaning, keeps in Dark Place.
After depositing 230 days under room temperature, through observing slurries, there is not obvious demixing phenomenon.
Embodiment 3
Pulpous state CBS white dyes in the present embodiment, it is made up of the raw material of following weight percents:
The preparation method of above-mentioned pulpous state CBS white dyes, comprise a turn crystalline substance, add auxiliary agent, homogenize and deaeration four steps, its preparation method is:
(1) turn crystalline substance and first add 498Kg deionized water to turning in brilliant equipment, when stirring heating is warming up to 50 ~ 60 DEG C, then 400Kg 4 is added, 4 '-bis-(2-sodium sulfonate styryl) biphenyl, continue to be heated to 95 ~ 100 DEG C dissolve and be incubated 2h, ON cycle water coolant is down to 60 ~ 65 DEG C temperature of charge again, and be incubated 2h at this temperature, continue to pass into recirculated cooling water after insulation terminates, temperature of charge is slowly down to 30 ~ 35 DEG C, and be incubated 8h at this temperature, observing crystal form major part under using biomicroscope 160 times is laminar crystallization,
(2) add auxiliary agent and add sodium lignosulfonate 30.0Kg, NNO20.0Kg, carboxymethyl cellulose 0.5Kg, PVP 0.5Kg, Industrial Salt 50.0Kg and MIT 2.0Kg successively to completing in turn brilliant slurry, stir 30 minutes, MIT addition, according to the situation of weather, can adjust in right amount;
(3) homogenize and the slurry that with the addition of auxiliary agent is added in high speed beating equipment, pull an oar 60 minutes under mixing speed is 2500 ~ 3000rpm condition;
(4) slurry after above-mentioned homogenizing adds in vacuum defoamation machine and carries out deaeration 1h by deaeration, and deaeration is complete, and obtain pulpous state CBS white dyes product, product is put in the plastic tank of cleaning, keeps in Dark Place.
After depositing 250 days under room temperature, through observing slurries, there is not obvious demixing phenomenon.
1,2-PD in above-described embodiment and ethylene glycol can also replace by glycerol.
Raw material in above-described embodiment can also by following weight percents arbitrary combination:
Protection scope of the present invention is not by the restriction of above embodiment.
Claims (5)
1. the preparation method of a pulpous state CBS white dyes, it is characterized in that: it is made up of the raw material of following weight percents: 4,4 '-bis-(2-sodium sulfonate styryl) biphenyl 30 ~ 40%, dispersion agent 0.2 ~ 5%, thickening material 0.1 ~ 2.0%, Industrial Salt 0.2 ~ 5%, antifreezing agent 0 ~ 5%, sterilant 0 ~ 0.5%, deionized water 42.5 ~ 69.5%; Comprise a turn crystalline substance, add auxiliary agent, homogenize and deaeration four steps, its preparation process is:
(1) turn brilliant and first add to turning in brilliant equipment the deionized water that weight percent is 42.5 ~ 69.5%, when stirring heating is warming up to 50 ~ 60 DEG C, then add that weight percent is 30 ~ 40% 4, 4 '-bis-(2-sodium sulfonate styryl) biphenyl, continue to be heated to 95 ~ 100 DEG C dissolve and be incubated 1 ~ 2h, ON cycle water coolant is down to 60 ~ 65 DEG C temperature of charge again, and be incubated 1 ~ 2h at this temperature, continue to pass into recirculated cooling water after insulation terminates, temperature of charge is slowly down to 30 ~ 35 DEG C, and be incubated more than 2h at this temperature, until use biomicroscope 160 times under observe crystal form major part for laminar crystallization till,
(2) add auxiliary agent to complete turn brilliant slurry in add successively weight percent be 0.2 ~ 5% dispersion agent, the weight percent thickening material that is 0.1 ~ 2.0%, the weight percent Industrial Salt that is 0.2 ~ 5%, weight percent be 0 ~ 5% antifreezing agent and weight percent be the sterilant of 0 ~ 0.5%, stir 30 minutes;
(3) homogenize and the slurry that with the addition of auxiliary agent is added in high speed beating equipment, pull an oar 30 ~ 60 minutes under mixing speed is 2500 ~ 3000rpm condition;
(4) slurry after above-mentioned homogenizing adds in vacuum defoamation machine and carries out deaeration 1h by deaeration, and deaeration is complete, obtains pulpous state CBS white dyes product.
2. the preparation method of a kind of pulpous state CBS white dyes according to claim 1, is characterized in that: described dispersion agent is one or more mixtures in beta-naphthalenesulfonic-acid salt, NNO, MF or lignin sulfonate.
3. the preparation method of a kind of pulpous state CBS white dyes according to claim 1, is characterized in that: described thickening material is one or more mixtures in xanthan gum, carboxymethyl cellulose, cyclodextrin or polyvinylpyrrolidone.
4. the preparation method of a kind of pulpous state CBS white dyes according to claim 1, is characterized in that: described antifreezing agent is one or more mixtures in 1,2-PD, ethylene glycol or glycerol.
5. the preparation method of a kind of pulpous state CBS white dyes according to claim 1, is characterized in that: described sterilant is the one in CMIT or MIT.
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| CN103923486A (en) * | 2014-04-03 | 2014-07-16 | 山西青山化工有限公司 | Toluylenetriazine pasty fluorescent brightener and preparation method thereof |
| TWI568801B (en) * | 2016-01-28 | 2017-02-01 | Teh Fong Min International Co Ltd | A fluorescent whitening agent composition |
| CN110857418A (en) * | 2018-08-25 | 2020-03-03 | 山西晋光化工有限公司 | Novel liquid fluorescent whitening agent |
| CN113736579A (en) * | 2021-09-29 | 2021-12-03 | 浙江宏达化学制品有限公司 | Fluorescent whitening agent composition with low salt content and preparation method thereof |
| CN114163834A (en) * | 2021-12-13 | 2022-03-11 | 陕西省石油化工研究设计院 | CBS-351 liquid whitening agent and preparation method thereof |
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