CN102718687A - Method for preparing 4B acid - Google Patents
Method for preparing 4B acid Download PDFInfo
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- CN102718687A CN102718687A CN2012101688289A CN201210168828A CN102718687A CN 102718687 A CN102718687 A CN 102718687A CN 2012101688289 A CN2012101688289 A CN 2012101688289A CN 201210168828 A CN201210168828 A CN 201210168828A CN 102718687 A CN102718687 A CN 102718687A
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Abstract
The invention discloses a method for preparing 4B acid. The method comprises the following steps of: putting paratoluidine and sulfuric acid in a certain proportion into a sulfonation reaction kettle, introducing heat transfer oil, heating to 180 DEG C, performing sulfonation reaction, allowing a product obtained by sulfonation reaction to enter a dissolving tank in which caustic soda liquid and water are added, introducing steam and raising the temperature for alkali dissolution at the same time, entering a decolorizing kettle, decolorizing by using activated carbon, allowing a product to enter a reaction kettle in which a hydrochloric acid solution at the concentration of 30 percent is added, performing acid precipitation reaction, filter-pressing and dehydrating by using a filter press, performing interlayer drying by using the heat transfer oil, and finally packaging a product. The product produced by the method for preparing the 4B acid can improve the fluidity, hue and transparency of pigments.
Description
Technical field
The present invention relates to a kind of preparation method of Pigment Intermediates, specifically, relate to a kind of preparation method of 4B acid.
Background technology
4B acid is one of topmost eight kinds of current pigment dyestuff midbody, on pigment industry, is mainly used in to produce C.I. Pigment red 57 serial red pigments.This pigment mainly is widely used in paint, coating, colored ink, rubber and coloring plastic etc., even Different products possibly have different form and aspect requirements to same pigment, this production requirement to pigment is more, and the kind that provides needs more.
Summary of the invention
Technical problem to be solved by this invention provides the method that a kind of preparation can be adjusted the 4B acid of pigment form and aspect.
The present invention solves the scheme that its technical problem takes: a kind of preparation method of 4B acid, and this method may further comprise the steps:
A. in the sulfonation reaction still, slowly in the para-totuidine of melting state, add mass concentration by a certain percentage and be 98% sulfuric acid, and carry out sulfonation reaction after feeding heat-conducting oil heating to 180 ℃, the reaction times is 5h-6h;
B. the sulfonation reaction after product gets into the dissolving vessel that is provided with liquid caustic soda and water, feeds steam simultaneously and heats up, and carries out alkali and dissolves;
C. alkali is dissolved after product entering decolouring still and use decolorizing with activated carbon;
D. the after product that decolours gets into to be provided with in the reaction kettle that mass concentration is 30% hydrochloric acid soln and carries out acid precipitation reaction;
E. the after product of will saltouing uses the thermal oil interlayer dry through the pressure filter filter-press dehydration then, carries out the packing of product at last.
As preferably, para-totuidine and sulfuric acid among the said step a carry out sulfonation reaction with molar mass than the ratio that is 1.07:1.
As optimization, the pressure of press filtration is 0.3MPa-0.6MPa among the said step e, and time of filter pressing is 3h-6h.
The reaction equation of preparation is following:
The invention has the beneficial effects as follows: the product that the preparation method produced of 4B acid provided by the invention can improve the degree of mobilization of pigment, adjustment form and aspect and transparency; And reach 95% loose tide article 4B acid through its solid content of water squeezing and be applied in the pigment, produce that color can be more bright-coloured in the 57 serial red products.
Description of drawings:
Below in conjunction with accompanying drawing the present invention is further specified.
Fig. 1 is preparing method's process flow sheet of 4B acid of the present invention.
Embodiment
Describe the present invention below in conjunction with accompanying drawing and embodiment:
The preparation method of a kind of 4B acid as shown in Figure 1, this method may further comprise the steps:
In the sulfonation reaction still, slowly in the para-totuidine of melting state, add mass concentration by a certain percentage and be 98% sulfuric acid (para-totuidine and sulfuric acid are 1.07:1 with the molar mass ratio); And carry out sulfonation reaction after feeding heat-conducting oil heating to 180 ℃, the reaction times is 5h-6h; The sulfonation reaction after product gets into the dissolving vessel that is provided with liquid caustic soda and water, feeds steam simultaneously and heats up, and carries out alkali and dissolves; Alkali is dissolved after product entering decolouring still use decolorizing with activated carbon; The decolouring after product gets into to be provided with in the reaction kettle that mass concentration is 30% hydrochloric acid soln and carries out acid precipitation reaction; The after product of will saltouing dewaters through pressure filter press filtration (pressure is that 0.3MPa-0.6MPa, time of filter pressing are 3h-6h); Use the thermal oil interlayer dry then; Carry out the packing of product at last, in the 4B acid for preparing, containing 1% different 4B acid is the key factor that 4B acid is applied to can improve in the pigment industry degree of mobilization and adjustment pigment form and aspect.
The reaction equation of preparation is following:
The invention has the beneficial effects as follows: the product that the preparation method produced of 4B acid provided by the invention can improve the degree of mobilization of pigment, adjustment form and aspect and transparency; And reach 95% loose tide article 4B acid through its solid content of water squeezing and be applied in the pigment, produce that color can be more bright-coloured in the 57 serial red products.
It is emphasized that: above only is preferred embodiment of the present invention; Be not that the present invention is done any pro forma restriction; Every foundation technical spirit of the present invention all still belongs in the scope of this technical scheme any simple modification, equivalent variations and modification that above embodiment did.
Claims (3)
1. the preparation method of 4B acid, it is characterized in that: this method may further comprise the steps:
A. in the sulfonation reaction still, slowly in the para-totuidine of melting state, add mass concentration by a certain percentage and be 98% sulfuric acid, and carry out sulfonation reaction after feeding heat-conducting oil heating to 180 ℃, the reaction times is 5h-6h;
B. the sulfonation reaction after product gets into the dissolving vessel that is provided with liquid caustic soda and water, feeds steam simultaneously and heats up, and carries out alkali and dissolves;
C. alkali is dissolved after product entering decolouring still and use decolorizing with activated carbon;
D. the after product that decolours gets into to be provided with in the reaction kettle that mass concentration is 30% hydrochloric acid soln and carries out acid precipitation reaction;
E. the after product of will saltouing uses the thermal oil interlayer dry through the pressure filter filter-press dehydration then, carries out the packing of product at last.
2. the preparation method of 4B acid according to claim 1, it is characterized in that: para-totuidine and sulfuric acid among the said step a carry out sulfonation reaction with molar mass than the ratio that is 1.07:1.
3. 4B according to claim 1 acid the preparation method, it is characterized in that: the pressure of press filtration is 0.3MPa-0.6MPa among the said step e, time of filter pressing is 3h-6h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101688289A CN102718687A (en) | 2012-05-29 | 2012-05-29 | Method for preparing 4B acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101688289A CN102718687A (en) | 2012-05-29 | 2012-05-29 | Method for preparing 4B acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102718687A true CN102718687A (en) | 2012-10-10 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012101688289A Pending CN102718687A (en) | 2012-05-29 | 2012-05-29 | Method for preparing 4B acid |
Country Status (1)
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| CN (1) | CN102718687A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105968033A (en) * | 2016-05-12 | 2016-09-28 | 嘉兴市正大化工有限公司 | Production method of 3,4-dichloroaniline-6-sulfonic acid |
| CN109053500A (en) * | 2018-09-10 | 2018-12-21 | 宜宾市南溪区红源化工有限公司 | A kind of method of liquid alkaline purification 4B acid |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1130624A (en) * | 1995-09-07 | 1996-09-11 | 深州市景明化工厂 | Synthetic method and purifying technique for high-purity p-toluidine-3-sulfonic acid (4B acid) |
-
2012
- 2012-05-29 CN CN2012101688289A patent/CN102718687A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1130624A (en) * | 1995-09-07 | 1996-09-11 | 深州市景明化工厂 | Synthetic method and purifying technique for high-purity p-toluidine-3-sulfonic acid (4B acid) |
Non-Patent Citations (6)
| Title |
|---|
| 史沈明: "4-氨基甲苯-3-磺酸的合成工艺研究及设计", 《中国优秀硕士学位论文全文数据库工程科技I辑》 * |
| 夏天喜等: "液相磺化合成高纯4B酸的研究", 《染料工业》 * |
| 张雪梅等: "4B酸的合成", 《精细石油化工》 * |
| 张雪梅等: "对甲基苯胺-邻磺酸合成新工艺", 《化工进展》 * |
| 王鸿等: "用浓硫酸磺化苯胺制备对氨基苯磺酸生产工艺浅析", 《湖北化工》 * |
| 苏砚溪等: "对甲苯胺-2-磺酸的合成研究", 《精细石油化工》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105968033A (en) * | 2016-05-12 | 2016-09-28 | 嘉兴市正大化工有限公司 | Production method of 3,4-dichloroaniline-6-sulfonic acid |
| CN105968033B (en) * | 2016-05-12 | 2018-02-16 | 浙江正大新材料科技有限公司 | A kind of production method of the sulfonic acid of 3,4 dichloroaniline 6 |
| CN109053500A (en) * | 2018-09-10 | 2018-12-21 | 宜宾市南溪区红源化工有限公司 | A kind of method of liquid alkaline purification 4B acid |
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Application publication date: 20121010 |