CN102718688A - Method for preparing 2B acid - Google Patents
Method for preparing 2B acid Download PDFInfo
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- CN102718688A CN102718688A CN2012101689135A CN201210168913A CN102718688A CN 102718688 A CN102718688 A CN 102718688A CN 2012101689135 A CN2012101689135 A CN 2012101689135A CN 201210168913 A CN201210168913 A CN 201210168913A CN 102718688 A CN102718688 A CN 102718688A
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- sulfonation reaction
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Abstract
The invention discloses a method for preparing 2B acid. The method comprises the following steps of: putting 2B oil and sulfuric acid into a sulfonation reaction kettle according to a certain proportion; introducing heat conductive oil, and heating to 200 DEG C for performing sulfonation reaction; introducing the sulfonation reaction product to a dissolving tank in which caustic soda liquid and water are held; introducing steam for raising the temperature and performing alkaline dissolution; entering a decoloring kettle for decoloring by using active carbon; entering the decolored product to a reaction kettle holding 30 percent of hydrochloric acid solution for acid analysis reaction; performing filter-pressing and dewatering by a pressure filter; drying by the heat conductive oil in an interlayer mode; and finally packaging the product. By utilizing the product produced by using the method for preparing 2B acid, the fluidity of a pigment can be improved, and the hue and the transparency are regulated.
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 2B acid.
Background technology
2B 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 48 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 regulated the 2B acid of pigment form and aspect.
The present invention solves the scheme that its technical problem takes: a kind of preparation method of 2B acid, and this method may further comprise the steps:
A. in the sulfonation reaction still, slowly adding mass concentration by a certain percentage to the 2B of melting state oil is 98% sulfuric acid, carries out sulfonation reaction after feeding heat-conducting oil heating to 200 ℃;
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 and to be provided with the reaction of saltouing in the reaction kettle that mass concentration is 30% hydrochloric acid soln;
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, 2B oil and sulfuric acid among the said step a carry out sulfonation reaction with molar mass than the ratio that is 1.41:1.The reaction equation of preparation is following:
As preferably, the pressure of press filtration is 0.3MPa-0.6MPa among the said step e, and time of filter pressing is 3h-6h.
The invention has the beneficial effects as follows: the product application that the preparation method produced of 2B acid provided by the invention can improve the degree of mobilization of pigment, adjustment form and aspect and transparency in pigment; And reach 90% loose tide article 2B acid through its solid content of water squeezing and be applied in the pigment, produce that color can be more bright-coloured in the 48 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 2B 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 2B acid as shown in Figure 1, this method may further comprise the steps: in the sulfonation reaction still, slowly adding mass concentration by a certain percentage to the 2B of melting state oil is 98% sulfuric acid (2B oil and sulfuric acid are 1.41:1 with the molar mass ratio); Carry out sulfonation reaction after feeding heat-conducting oil heating to 200 ℃; 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 2B acid for preparing, containing 1% different 2B acid is the key factor that 2B 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 application that the preparation method produced of 2B acid provided by the invention can improve the degree of mobilization of pigment, adjustment form and aspect and transparency in pigment; And reach 90% loose tide article 2B acid through its solid content of water squeezing and be applied in the pigment, produce that color can be more bright-coloured in the 48 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 technical scheme of the present invention any simple modification, equivalent variations and modification that above embodiment did.
Claims (3)
1. the preparation method of 2B acid, it is characterized in that: this method may further comprise the steps:
A. in the sulfonation reaction still, slowly in the 2B of melting state oil, add mass concentration by a certain percentage and be 98% sulfuric acid, and carry out sulfonation reaction after feeding heat-conducting oil heating to 200 ℃;
B. the product after the sulfonation reaction gets into the dissolving vessel that is added 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 will decolour 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 2B acid according to claim 1 is characterized in that: 2B oil and sulfuric acid among the said step a carry out sulfonation reaction with molar mass than the ratio that is 1.41:1.
3. 2B 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 |
|---|---|---|---|
| CN2012101689135A CN102718688A (en) | 2012-05-29 | 2012-05-29 | Method for preparing 2B acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101689135A CN102718688A (en) | 2012-05-29 | 2012-05-29 | Method for preparing 2B acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102718688A true CN102718688A (en) | 2012-10-10 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012101689135A Pending CN102718688A (en) | 2012-05-29 | 2012-05-29 | Method for preparing 2B acid |
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| CN (1) | CN102718688A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109180537A (en) * | 2018-08-24 | 2019-01-11 | 浙江友联化学工业有限公司 | A kind of method that liquid phase baking process prepares 3- chlorine para-totuidine -6- sulfonic acid |
| CN114716351A (en) * | 2022-04-28 | 2022-07-08 | 镇江市宝利科技有限公司 | Method for producing 2-amino-4-chloro-5-methylbenzenesulfonic 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 CN2012101689135A patent/CN102718688A/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 (4)
| 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》 * |
| 尤乃禄: "2B酸生产新工艺", 《江苏化工》 * |
| 施志荣等: "2B酸的合成改进", 《安徽化工》 * |
| 杨明荣: "在煤油溶剂中合成2B酸的研究", 《浙江化工》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109180537A (en) * | 2018-08-24 | 2019-01-11 | 浙江友联化学工业有限公司 | A kind of method that liquid phase baking process prepares 3- chlorine para-totuidine -6- sulfonic acid |
| CN109180537B (en) * | 2018-08-24 | 2021-07-20 | 浙江友联化学工业有限公司 | Method for preparing 3-chloro-p-toluidine-6-sulfonic acid by liquid phase baking method |
| CN114716351A (en) * | 2022-04-28 | 2022-07-08 | 镇江市宝利科技有限公司 | Method for producing 2-amino-4-chloro-5-methylbenzenesulfonic acid |
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Application publication date: 20121010 |