CN104262999A - Highly dispersive fluorescent brightener for whitening in printing and dyeing and preparation method thereof - Google Patents
Highly dispersive fluorescent brightener for whitening in printing and dyeing and preparation method thereof Download PDFInfo
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- CN104262999A CN104262999A CN201410495946.XA CN201410495946A CN104262999A CN 104262999 A CN104262999 A CN 104262999A CN 201410495946 A CN201410495946 A CN 201410495946A CN 104262999 A CN104262999 A CN 104262999A
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Abstract
The invention belongs to a fluorescent brightener and a preparation method thereof and specifically relates to a highly dispersive fluorescent brightener for whitening in printing and dyeing and a preparation method thereof. The highly dispersive fluorescent brightener for whitening in printing and dyeing is mainly used for solving the technical problems of complex process and high energy consumption of an existing fluorescent brightener and difficult adjustment of the value of a granular fluorescent brightener. The highly dispersive fluorescent brightener for whitening in printing and dyeing is prepared from the following components in percentage by weight: 80-95% of C.I. fluorescent brightener 71, 2-8% of wetting agent, 2-10% of inorganic salt and 0.5-5% of water. The highly dispersive fluorescent brightener for whitening in printing and dyeing has the advantages of good wettability and easy dispersion, and the preparation method of the brightener is simple and low in energy consumption; and besides, the value of the fluorescent brightener can be adjusted according to the use requirements of customers anytime.
Description
Technical field
The invention belongs to white dyes and preparation method thereof, being specifically related to a kind of high dispersive type white dyes brightened for printing and dyeing and preparation method thereof.
Background technology
Most of fluorescent whitening dyes is water insoluble or is insoluble in the organic compound of water, there is wettability difference, the problem that difficulty or ease are disperseed in water.Particularly printing and dyeing white dyes, because powder-type product has, effective component content is high, stable storing, packed and transported advantage easily, most enterprises choice of powder type white dyes, but powder-type white dyes is comparatively thin because of its powder, the problem that existence not easily soaks, jitter time is long of easily uniting in water.Therefore solve the problem that white dyes wettability is poor, not easily disperse, become a great problem of printing and dyeing white dyes.
The evaluation method of white dyes wettability---settling time index, white dyes, as dyeing and printing auxiliary, needs the aqueous solution first white dyes being dissolved as high density, then joins in dye liquor, carry out brightening of fabric.If the wettability of white dyes is poor, not easily disperseing, then can extend dissolving jitter time, also likely there is the staining problem of white dyes on fabric in serious.We evaluate a method for quick of white dyes wettability at dyeing for this reason, namely the settling time is detected, namely 1g white dyes sample is claimed, add in the beaker of the 250ml filling 100ml tap water, the record settling time, standard is under static state, and material sank to completely in water in 30 seconds, shows that the wettability of material is good.
In order to the problem solving white dyes wettability difference and not easily disperse, Authorization Notice No. be CN101760048 B patent discloses a kind of granule type white dyes with polymolecularity for washing industry, but product is in preparation process, the coarse filtration cake used again need add water to pull an oar and disperse, spraying dry is carried out again through sand milling, there is complex process and the high technical problem of energy consumption, and granule type white dyes score value not easily adjusts, can not carry out according to the service requirements of client the problem that adjusts at any time.
Summary of the invention
The object of the invention is to solve existing white dyes and there is the technical problem that the high and granule type white dyes score value of complex process, energy consumption not easily adjusts, a kind of high dispersive type white dyes brightened for printing and dyeing and preparation method thereof is provided.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
The high dispersive type white dyes brightened for printing and dyeing, it is made up of the component of following weight percent:
Prepare a method for the described high dispersive type white dyes brightened for printing and dyeing, it comprises the following steps:
1) prepare C.I. white dyes 71: by 4,4 ,-diaminobenzil-disulfonic acid and cyanuric chloride, according to the mol ratio of 1:1, obtain single step reaction condensated liquid through a step condensation reaction at the temperature of 0-10 DEG C; Single step reaction condensated liquid and aniline, according to the mol ratio of 1:2, obtain two step reaction condensated liquids through two step condensation reactions at the temperature of 30-50 DEG C; Two steps reaction condensated liquids and morpholine, according to the mol ratio of 1:2, through three step condensation reactions at the temperature of 80-90 DEG C, and turn crystalline substance through high temperature and obtain the three-step reaction condensated liquid that C.I. white dyes 71 content is 9 ~ 15% at the temperature of 130-140 DEG C;
2) until step 1) the three-step reaction condensated liquid prepared proceeds to transfer pot when 120-110 DEG C;
3) when feed temperature is down to 90-80 DEG C in transfer pot, add in transfer pot by wetting agent under the state stirred, wetting agent add-on is the 2-8% of C.I. white dyes 71 amount of giving money as a gift in three-step reaction condensated liquid, continues to stir 25-35 minute;
4) when feed temperature is down to 80-65 DEG C in transfer pot, it is the filter cake of 45-70% that the feed liquid press filtration in transfer pot is obtained C.I. white dyes 71 content;
5) be finally that namely 80-95% obtains the high dispersive type white dyes brightened for printing and dyeing by C.I. white dyes 71 filter cake through expansion drying to C.I. white dyes 71 content.
The feed postition of described wetting agent evenly added in 10-20 minute under the state stirred.
Described wetting agent is Nekal BX or OP-10.
The high dispersive type white dyes wettability that the powder-type that the present invention adopts above-mentioned preparation method to obtain brightens for printing and dyeing is good, easy dispersion, within settling time can reach 30 seconds, have more than 2 minutes than traditional powder-type white dyes settling time and improved greatly, and preparation method is simple, energy consumption is low, and white dyes score value can adjust according to the service requirements of client at any time.Therefore, compared with background technology, the present invention has wettability advantage that is good and that easily disperse, and preparation method is simple, and energy consumption is low, and white dyes score value can adjust according to the service requirements of client at any time.
Embodiment
Embodiment 1
A kind of high dispersive type white dyes brightened for printing and dyeing in the present embodiment, it is made up of the component of following weight percent:
Prepare a method for the high dispersive type white dyes brightened for printing and dyeing described in the present embodiment, it comprises the following steps:
1) prepare C.I. white dyes 71: by 4,4 ,-diaminobenzil-disulfonic acid and cyanuric chloride, according to the mol ratio of 1:1, obtain single step reaction condensated liquid through a step condensation reaction at the temperature of 0-10 DEG C; Single step reaction condensated liquid and aniline, according to the mol ratio of 1:2, obtain two step reaction condensated liquids through two step condensation reactions at the temperature of 30-50 DEG C; Two steps reaction condensated liquids and morpholine, according to the mol ratio of 1:2, through three step condensation reactions at the temperature of 80-90 DEG C, and turn crystalline substance through high temperature and obtain the three-step reaction condensated liquid that C.I. white dyes 71 content is 15% at the temperature of 130-140 DEG C;
2) until step 1) the three-step reaction condensated liquid prepared proceeds to transfer pot 120 DEG C time;
3) when feed temperature is down to 90 DEG C in transfer pot, under the state stirred, Nekal BX was evenly sprinkled in transfer pot in 10 minutes, Nekal BX add-on is 8% of C.I. white dyes 71 amount of giving money as a gift in three-step reaction condensated liquid, continues stirring 25 minutes;
4) when feed temperature is down to 80 DEG C in transfer pot, it is the filter cake of 45% that the feed liquid press filtration in transfer pot is obtained C.I. white dyes 71 content;
5) be finally 80% namely obtain the high dispersive type white dyes brightened for printing and dyeing by C.I. white dyes 71 filter cake through expansion drying to C.I. white dyes 71 content.
Embodiment 2
A kind of high dispersive type white dyes brightened for printing and dyeing in the present embodiment, it is made up of the component of following weight percent:
Prepare a method for the high dispersive type white dyes brightened for printing and dyeing described in the present embodiment, it comprises the following steps:
1) prepare C.I. white dyes 71: by 4,4 ,-diaminobenzil-disulfonic acid and cyanuric chloride, according to the mol ratio of 1:1, obtain single step reaction condensated liquid through a step condensation reaction at the temperature of 0-10 DEG C; Single step reaction condensated liquid and aniline, according to the mol ratio of 1:2, obtain two step reaction condensated liquids through two step condensation reactions at the temperature of 30-50 DEG C; Two steps reaction condensated liquids and morpholine, according to the mol ratio of 1:2, through three step condensation reactions at the temperature of 80-90 DEG C, and turn crystalline substance through high temperature and obtain the three-step reaction condensated liquid that C.I. white dyes 71 content is 9% at the temperature of 130-140 DEG C;
2) until step 1) the three-step reaction condensated liquid prepared proceeds to transfer pot 110 DEG C time;
3) when feed temperature is down to 80 DEG C in transfer pot, under the state stirred, Nekal BX was evenly sprinkled in transfer pot in 20 minutes, Nekal BX add-on is 2% of C.I. white dyes 71 amount of giving money as a gift in three-step reaction condensated liquid, continues stirring 35 minutes;
4) when feed temperature is down to 65 DEG C in transfer pot, it is the filter cake of 70% that the feed liquid press filtration in transfer pot is obtained C.I. white dyes 71 content;
5) be finally 95% namely obtain the high dispersive type white dyes brightened for printing and dyeing by C.I. white dyes 71 filter cake through expansion drying to C.I. white dyes 71 content.
Embodiment 3
A kind of high dispersive type white dyes brightened for printing and dyeing in the present embodiment, it is made up of the component of following weight percent:
Prepare a method for the high dispersive type white dyes brightened for printing and dyeing described in the present embodiment, it comprises the following steps:
1) prepare C.I. white dyes 71: by 4,4 ,-diaminobenzil-disulfonic acid and cyanuric chloride, according to the mol ratio of 1:1, obtain single step reaction condensated liquid through a step condensation reaction at the temperature of 0-10 DEG C; Single step reaction condensated liquid and aniline, according to the mol ratio of 1:2, obtain two step reaction condensated liquids through two step condensation reactions at the temperature of 30-50 DEG C; Two steps reaction condensated liquids and morpholine, according to the mol ratio of 1:2, through three step condensation reactions at the temperature of 80-90 DEG C, and turn crystalline substance through high temperature and obtain the three-step reaction condensated liquid that C.I. white dyes 71 content is 12% at the temperature of 130-140 DEG C;
2) until step 1) the three-step reaction condensated liquid prepared proceeds to transfer pot 115 DEG C time;
3) when feed temperature is down to 85 DEG C in transfer pot, under the state stirred, Nekal BX was evenly sprinkled in transfer pot in 15 minutes, Nekal BX add-on is 5.5% of C.I. white dyes 71 amount of giving money as a gift in three-step reaction condensated liquid, continues stirring 30 minutes;
4) when feed temperature is down to 70 DEG C in transfer pot, it is the filter cake of 50% that the feed liquid press filtration in transfer pot is obtained C.I. white dyes 71 content;
5) be finally 90% namely obtain the high dispersive type white dyes brightened for printing and dyeing by C.I. white dyes 71 filter cake through expansion drying to C.I. white dyes 71 content.
Embodiment 4
A kind of high dispersive type white dyes brightened for printing and dyeing in the present embodiment, it is made up of the component of following weight percent:
Prepare a method for the high dispersive type white dyes brightened for printing and dyeing described in the present embodiment, it comprises the following steps:
1) prepare C.I. white dyes 71: by 4,4 ,-diaminobenzil-disulfonic acid and cyanuric chloride, according to the mol ratio of 1:1, obtain single step reaction condensated liquid through a step condensation reaction at the temperature of 0-10 DEG C; Single step reaction condensated liquid and aniline, according to the mol ratio of 1:2, obtain two step reaction condensated liquids through two step condensation reactions at the temperature of 30-50 DEG C; Two steps reaction condensated liquids and morpholine are according to the mol ratio of 1:2, and through three step condensation reactions at the temperature of 80-90 DEG C, and at the temperature of 130-140 DEG C, turning crystalline substance through high temperature, to obtain C.I. white dyes 71 content be 10% three-step reaction condensated liquid;
2) until step 1) the three-step reaction condensated liquid prepared proceeds to transfer pot 120 DEG C time;
3) when feed temperature is down to 90 DEG C in transfer pot, under the state stirred, Nekal BX was evenly sprinkled in transfer pot in 10 minutes, Nekal BX add-on is 3% of C.I. white dyes 71 amount of giving money as a gift in three-step reaction condensated liquid, continues stirring 25 minutes;
4) when feed temperature is down to 80 DEG C in transfer pot, it is the filter cake of 60% that the feed liquid press filtration in transfer pot is obtained C.I. white dyes 71 content;
5) be finally 89% namely obtain the high dispersive type white dyes brightened for printing and dyeing by C.I. white dyes 71 filter cake through expansion drying to C.I. white dyes 71 content.
Embodiment 5
A kind of high dispersive type white dyes brightened for printing and dyeing in the present embodiment, it is made up of the component of following weight percent:
Prepare a method for the high dispersive type white dyes brightened for printing and dyeing described in the present embodiment, it comprises the following steps:
1) prepare C.I. white dyes 71: by 4,4 ,-diaminobenzil-disulfonic acid and cyanuric chloride, according to the mol ratio of 1:1, obtain single step reaction condensated liquid through a step condensation reaction at the temperature of 0-10 DEG C; Single step reaction condensated liquid and aniline, according to the mol ratio of 1:2, obtain two step reaction condensated liquids through two step condensation reactions at the temperature of 30-50 DEG C; Two steps reaction condensated liquids and morpholine are according to the mol ratio of 1:2, and through three step condensation reactions at the temperature of 80-90 DEG C, and at the temperature of 130-140 DEG C, turning crystalline substance through high temperature, to obtain C.I. white dyes 71 content be 12% three-step reaction condensated liquid;
2) until step 1) the three-step reaction condensated liquid prepared proceeds to transfer pot 110 DEG C time;
3) when feed temperature is down to 80 DEG C in transfer pot, under the state stirred, Nekal BX was evenly sprinkled in transfer pot in 20 minutes, Nekal BX add-on is 6% of C.I. white dyes 71 amount of giving money as a gift in three-step reaction condensated liquid, continues stirring 35 minutes;
4) when feed temperature is down to 65 DEG C in transfer pot, it is the filter cake of 65% that the feed liquid press filtration in transfer pot is obtained C.I. white dyes 71 content;
5) be finally 86% namely obtain the high dispersive type white dyes brightened for printing and dyeing by C.I. white dyes 71 filter cake through expansion drying to C.I. white dyes 71 content.
Nekal BX in above-described embodiment can also replace with OP-10.
The high dispersive type white dyes brightened for printing and dyeing in above-described embodiment can also be made up of the component arbitrary combination of following weight percent:
Protection scope of the present invention is not by the restriction of above embodiment.
Claims (4)
1. the high dispersive type white dyes brightened for printing and dyeing, is characterized in that: it is made up of the component of following weight percent:
2. preparing a method for the high dispersive type white dyes brightened for printing and dyeing according to claim 1, it is characterized in that: comprise the following steps:
1) prepare C.I. white dyes 71: by 4,4 ,-diaminobenzil-disulfonic acid and cyanuric chloride, according to the mol ratio of 1:1, obtain single step reaction condensated liquid through a step condensation reaction at the temperature of 0-10 DEG C; Single step reaction condensated liquid and aniline, according to the mol ratio of 1:2, obtain two step reaction condensated liquids through two step condensation reactions at the temperature of 30-50 DEG C; Two steps reaction condensated liquids and morpholine, according to the mol ratio of 1:2, through three step condensation reactions at the temperature of 80-90 DEG C, and turn crystalline substance through high temperature and obtain the three-step reaction condensated liquid that C.I. white dyes 71 content is 9 ~ 15% at the temperature of 130-140 DEG C;
2) until step 1) the three-step reaction condensated liquid prepared proceeds to transfer pot when 120-110 DEG C;
3) when feed temperature is down to 90-80 DEG C in transfer pot, add in transfer pot by wetting agent under the state stirred, wetting agent add-on is the 2-8% of C.I. white dyes 71 amount of giving money as a gift in three-step reaction condensated liquid, continues to stir 25-35 minute;
4) when feed temperature is down to 80-65 DEG C in transfer pot, it is the filter cake of 45-70% that the feed liquid press filtration in transfer pot is obtained C.I. white dyes 71 content;
5) be finally that namely 80-95% obtains the high dispersive type white dyes brightened for printing and dyeing by C.I. white dyes 71 filter cake through expansion drying to C.I. white dyes 71 content.
3. a kind of method for the preparation of the high dispersive type white dyes brightened of printing and dyeing according to claim 2, is characterized in that: the feed postition of described wetting agent evenly added in 10-20 minute under the state stirred.
4. a kind of method for the preparation of the high dispersive type white dyes brightened of printing and dyeing according to Claims 2 or 3, is characterized in that: described wetting agent is Nekal BX or OP-10.
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| CN201410495946.XA CN104262999A (en) | 2014-09-25 | 2014-09-25 | Highly dispersive fluorescent brightener for whitening in printing and dyeing and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106349752A (en) * | 2016-08-25 | 2017-01-25 | 山西青山化工有限公司 | Stilbene bis triazine liquid whitener and preparation method thereof |
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| CN101760048A (en) * | 2009-11-30 | 2010-06-30 | 山西青山化工有限公司 | High-dispersivity fluorescent whitening agent and preparation method thereof |
| 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 |
| CN102924972A (en) * | 2012-11-16 | 2013-02-13 | 山西青山化工有限公司 | Highly water-soluble disulfonic acid fluorescent whitening agent composition |
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| WO2004111330A1 (en) * | 2003-06-11 | 2004-12-23 | Ciba Specialty Chemicals Holding Inc. | Storage-stable fluorescent whitener formulations |
| CN101429343A (en) * | 2008-12-04 | 2009-05-13 | 山西青山化工有限公司 | Process for producing fluorescent whitening agent 5BM |
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| CN106349752A (en) * | 2016-08-25 | 2017-01-25 | 山西青山化工有限公司 | Stilbene bis triazine liquid whitener and preparation method thereof |
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Application publication date: 20150107 |