CN101823977A - Separating and refining method of 2,5-diarylamine terephthalic acid (DXTA) - Google Patents
Separating and refining method of 2,5-diarylamine terephthalic acid (DXTA) Download PDFInfo
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Abstract
The invention relates to a separating and refining method of 2,5-diarylamine terephthalic acid (DXTA), and a crude 2,5-diarylamine terephthalic acid product is used as a raw material. The method comprises the following steps of: (1) heating and dissolving: adding the raw materials of crude 2,5-diarylamine terephthalic acid product, inorganic base and water into heating and dissolving equipment and simultaneously carrying out a neutralization reaction in the processes of heating and dissolving to generate an aqueous solution of 2,5-diarylamine terephthalic acid salt; (2) adsorbing for removing impurities; (3) carrying out solid-liquid separation; (4) neutralizing and acidifying: adding a refined mother liquor obtained in the step (3) to inorganic acid to obtain crystalline solid of 2,5-diarylamine terephthalic acid; (5) carrying out solid-liquid separation; (6) washing by using water; (7) drying: and obtaining a solid high-purity product of the 2,5-diarylamine terephthalic acid (DXTA) through the steps. The invention has the advantages of simple process, less energy consumption, low cost and good product quality.
Description
Technical field
The present invention relates to a kind of 2, the method of 5-diaryl-amine base terephthalic acid separation and purification, particularly with 2, the crude product of 5-diaryl-amine base terephthalic acid is that raw material recrystallization separation and purification obtains high-purity 2, the method of 5-diaryl-amine base terephthalic acid DXTA product belongs to the fine chemical technology field.
Background technology
2, the molecular structural formula of 5-diaryl-amine base terephthalic acid is:
Arylamine is an aniline, wherein: R=-H ,-CH
3,-Cl or-F etc. is the substituting group on the phenyl ring, can be contraposition or ortho position at anilino.Typical product has:
During R=H, full name 2,5-hexichol amido terephthalic acid (2,5-di-anilinoterephthalic acid), molecular formula is C
20H
16O
4N
2, molecular weight is 348, the red-purple pressed powder abbreviates DATA as.2,5-hexichol amido terephthalic acid is the important intermediate of synthetic senior pigment dyestuff quinacridine ketone pigment.Structural formula is:
During R=Cl, full name 2,5-two (p-Chlorobenzoic acid amide base) terephthalic acid [2,5-di (p-chloroanilino) terephthalic acid], claim 2 again, 5-two p-Chlorobenzoic acid amide bases-1,4-terephthalic acid (2,5-di (p-chloroanlino) terephthalic acid), abbreviate DpCTA as, molecular formula is C
20H
14O
4N
2Cl
2, molecular weight is 417, the bright red pressed powder.2,5-two p-Chlorobenzoic acid amide base terephthalic acids are important intermediate of synthetic senior pigment dyestuff quinacridine ketone pigment.Structural formula is:
R=CH
3The time, full name 2,5-two (para-totuidine base) terephthalic acid (2,5-di-oluidinoterephthalic acid) claims 2 again, two pairs of toluidine terephthalic acids of 5-, molecular formula is C
22H
20O
4N
2, molecular weight is 376, the sorrel pressed powder abbreviates DTTA as.2, two pairs of toluidine terephthalic acids of 5-are important intermediate of synthetic senior pigment dyestuff quinacridine ketone pigment.Structural formula is:
These intermediate general designations DXTA.
Quinacridine ketone pigment belongs to high-grade pigment dyestuff, have good light fastness, fastness to heat, and in various plastics, do not move, thereby be widely used in the painted of high-grade paint, engineering plastics, resin, pigment printing, printing ink, rubber, the fields such as dope dyeing that also are used for synthon are the very important high-grade pigment dyestuff kinds of a class.2,5-diaryl-amine base terephthalic acid is the important intermediate of synthetic quinacridine ketone pigment, 2, and the purity of 5-diaryl-amine base terephthalic acid has significant effects to the character of quinacridine ketone pigment product.Therefore, obtain high-purity 2,5-diaryl-amine base terephthalic acid (mass content＞99.5%) product, perhaps ought prepare 2,5-hexichol amido terephthalate product difficult quality satisfies when quinacridine ketone pigment is synthetic to be required, and needs in a hurry that a kind of technology of exploitation is reasonable, product purity is high, steady quality, separation and refining method is simple, easy to prepare, it is high-purity 2 that the safe and reliable separation and purification of process obtains, the method for 5-diaryl-amine base terephthalate product.
Summary of the invention
The purpose of this invention is to provide that a kind of technology is simple, less energy consumption, good product quality, production cost is low and the three wastes produce few, the separation and purification product purity is high 2, the separation and refining method of 5-diaryl-amine base terephthalic acid DXTA.
The technical scheme that realizes above-mentioned purpose is: a kind of 2, the separation and refining method of 5-diaryl-amine base terephthalic acid DXTA, be with 2, the crude product of 5-diaryl-amine base terephthalic acid is that raw material adopts the recrystallization separation and purification to obtain high-purity 2,5-diaryl-amine base terephthalic acid DXTA, described method steps is as follows:
(1) rising temperature for dissolving: with raw material 2, carry out rising temperature for dissolving in the crude product of 5-diaryl-amine base terephthalic acid, mineral alkali and the water adding rising temperature for dissolving equipment, make 2,5-diaryl-amine base terephthalic acid is dissolved in the inorganic alkali solution, neutralization reaction takes place in the rising temperature for dissolving process, generate 2, the aqueous solution of 5-diaryl-amine base terephthalate;
(2) adsorption-edulcoration: in adsorption-edulcoration equipment, with previous step obtain 2, add the operation of adsorption-edulcoration agent carrying out adsorption-edulcoration in the 5-diaryl-amine base terephthalic acid salts solution;
(3) solid-liquid separates: with previous step obtain 2, the material that adds the adsorption-edulcoration agent in the 5-diaryl-amine base terephthalic acid salts solution carries out solid-liquid to be separated, the solid-liquid separation obtains the purified mother liquor and enters next step, and the adsorption-edulcoration agent that solid-phase material obtains after manipulation of regeneration enters previous step and recycles;
(4) in and acidifying: the refinement mother liquor that previous step is obtained adds mineral acid and carries out the acidifying neutralizing treatment, and neutralizing treatment finishes back control pH value 2～6, obtains 2, the crystalline solid of 5-diaryl-amine base terephthalic acid;
(5) solid-liquid separates: separation obtains 2 to the material that previous step is obtained through solid-liquid, the solid materials of 5-diaryl-amine base terephthalic acid enters next step, and the material that liquid phase material is removed behind the inorganic salt through crystallisation by cooling, solid-liquid separation directly recycles as the water and the raw material of the first step;
(6) washing: previous step is obtained 2, and the solid of 5-diaryl-amine base terephthalic acid is washed operation, gets purified 2, and 5-diaryl-amine base terephthalic acid solid, the water cycle of process washing are applied mechanically and used or recycle after treatment;
(7) drying: previous step is obtained 2, and the solid of 5-diaryl-amine base terephthalic acid obtains 2 80 ℃～120 ℃ dryings, 5-diaryl-amine base terephthalic acid DXTA solid high purity product.
Further, the mineral alkali described in the first step rising temperature for dissolving is any one in sodium hydroxide, potassium hydroxide or the ammonia.
Further, the consumption of mineral alkali is with respect in the material quantity 2 in the first step rising temperature for dissolving, the mol ratio of 5-diaryl-amine base terephthalic acid is 2.05～2.2: 1, and the consumption of water is with respect in the material quantity 2 in the system, and the mol ratio of 5-diaryl-amine base terephthalic acid is 100～200: 1.
Further, service temperature is 40 ℃～120 ℃ in the first step rising temperature for dissolving, and the operation absolute pressure is 0.1MPa～0.6MPa.
Further, be in sulfuric acid, hydrochloric acid or the acetic acid any one in the 4th step and described in the acidifying.
Further, the service temperature of the second step adsorption-edulcoration is 40 ℃～120 ℃, and working pressure is 0.1MPa～0.6MPa.
Further, the described adsorption-edulcoration agent of second step in the adsorption-edulcoration is the mixture of any one or any two kinds or any three kinds of components in molecular sieve or activated carbon or the diatomite.
Further, the first step rising temperature for dissolving equipment and the second step adsorption-edulcoration equipment and in the 4th step and acidizing unit be that the still formula stirs any one in chemical reactor, tubular chemical reactor or the static mixer.
Further, the 3rd step and described solid-liquid tripping device of the 5th step are any one in decanter type or press filter type or centrifugal or the vane-type solid-liquid tripping device.
Realize that the main technique equipment that the present invention needs is: rising temperature for dissolving equipment, adsorption-edulcoration equipment, in and acidizing unit and solid-liquid separating device etc.
The present invention 2, and the principle of the separation and purification of 5-diaryl-amine base terephthalic acid is:
(1) utilize 2,5-diaryl-amine base terephthalate is dissolved in the alkaline aqueous solution easily, and along with the rising solubleness of temperature becomes big characteristic fast, with 2,5-diaryl-amine base terephthalic acid is dissolved in the alkaline aqueous solution;
(2) utilize 2, the indissoluble liquid of 5-diaryl-amine base terephthalic acid is in acidic aqueous solution, and the characteristics of difficult hydrolysis, promptly utilize 2,5-diaryl-amine base terephthalate and 2, the deliquescent difference of 5-diaryl-amine base terephthalic acid, by with 2,5-diaryl-amine base terephthalic acid is dissolved in alkaline aqueous solution other the insoluble impurity that neutralizes to be separated, and further adopts the adsorption-edulcoration agent to carry out the adsorption-edulcoration operation and prepares 2,5-diaryl-amine base terephthalate refined soln, then with 2, the crystallization in acidic aqueous solution of 5-diaryl-amine base terephthalate is separated out, and obtains making with extra care 2,5-diaryl-amine base terephthalate product;
(3) utilize 2, in the 5-diaryl-amine base terephthalate treating process, the solubleness of by product inorganic acid salt in the aqueous solution is bigger, and along with variation of temperature changes in solubility bigger characteristics and easy crystalline characteristics, the employing cooling crystallization method is removed, and the aqueous solution in the process is recycled, by the refrigerative method, make 2,5-diaryl-amine base terephthalic acid solution refining.
The present invention adopts the benefit of technique scheme to be:
(1) makes full use of 2,5-diaryl-amine base terephthalate is in the alkaline aqueous solution that solubility with temperature raises and increases characteristic rapidly, adopt the recrystallization separation and purification to obtain high-purity 2,5-diaryl-amine base terephthalic acid DXTA, make operational path of the present invention short, technology is simple, consuming little energy, and production cost is low;
(2) make full use of the singularity of product, the no three wastes produce in the sepn process, cleaning, environmental protection, and various by products can be recycled, and this has saved cost greatly, is convenient to suitability for industrialized production;
(3) product 2 of employing processing method separation and purification of the present invention, 5-diaryl-amine base terephthalate product quality is good, yield height, purity height;
Preparation technology of the present invention is simple, less energy consumption, and good product quality, production cost is low and three wastes generation is few, separation and purification product purity height.
Description of drawings
Accompanying drawing is a process flow sheet of the present invention.
Embodiment
The present invention is further detailed explanation below in conjunction with drawings and Examples.
Embodiment one
Main technique equipment is: rising temperature for dissolving equipment, adsorption-edulcoration equipment and in and acidizing unit be that the still formula stirs chemical reactor, filter plant is centrifugal solid-liquid tripping device.
As shown in the figure, a kind of 2, the separation and refining method of 5-diaryl-amine base terephthalic acid DXTA, be with 2, it is high-purity 2 that the crude product of 5-diaryl-amine base terephthalic acid is that raw material adopts the recrystallization separation and purification to prepare, 5-diaryl-amine base terephthalic acid DXTA, and described method steps is as follows:
(1) rising temperature for dissolving: it is the lass lining stirred autoclave that the still formula of employing stirs chemical reactor, and with raw material 2, the crude product 10.0kg of 5-hexichol amido terephthalic acid, 2.4kg sodium hydroxide (NaOH) solid and 79.0kg water add the 0.128m of strap clamp cover
3In the lass lining stirred autoclave, the NaOH and 2 that adds, the mol ratio of 5-hexichol amido terephthalic acid crude product is 2.05: 1, the amount of water is with respect in the material quantity 2 in the system, and the mol ratio of 5-hexichol amido terephthalic acid crude product is 157: 1, and service temperature is 90 ℃, the operation absolute pressure is 0.1MPa, neutralization reaction takes place in the rising temperature for dissolving process, generates 2, the aqueous solution of 5-hexichol amido para-phthalic sodium;
(2) adsorption-edulcoration: the 91.4kg 2 that in the previous step glassed steel reaction vessels, obtains, in the 5-hexichol amido para-phthalic sodium solution, add adsorption-edulcoration agent activated carbon 1.0kg and carry out the adsorption-edulcoration operation, the consumption of adsorption-edulcoration agent be the solution body quality 1% (consumption of sorbent material is that the quality of sorbent material and the volume ratio of system are 10kg: 1m
3), the adsorption operations temperature is 90 ℃, working pressure is 0.1MPa;
(3) solid-liquid separates: with previous step obtain 2, the material that adds the adsorption-edulcoration agent in the 5-hexichol amido para-phthalic sodium solution adopts centrifugal solid-liquid tripping device to carry out the solid-liquid separation, the solid-liquid separation obtains the purified mother liquor and enters next step, and the adsorption-edulcoration agent that solid-phase material obtains after the water vapor desorption and regeneration is handled enters previous step, and agent recycles as adsorption-edulcoration;
(4) in and acidifying: the refinement mother liquor that previous step is obtained adds 98% industrial sulphuric acid 2.9kg, and the pH value in the regulation system is 2.Carry out the acidifying neutralizing treatment, material is carried out obtaining 2, the crystalline solid of 5-hexichol amido terephthalic acid about cooling operation to 20 ℃ simultaneously;
(5) solid-liquid separates: the material that previous step is obtained adopts centrifugal solid-liquid tripping device to carry out the solid-liquid separation, separation obtains 2 through solid-liquid, the solid materials of 5-hexichol amido terephthalic acid enters next step, the concentration of salt acquires a certain degree the time in the liquid phase material, and liquid phase material separates the material that removes after desalting through but crystallization, solid-liquid and directly recycles as the water and the raw material of the first step;
(6) washing: previous step is obtained 2, and the solid of 5-hexichol amido terephthalic acid is washed operation, gets purified 2, and 5-hexichol amido terephthalic acid solid, the water cycle of process washing are applied mechanically and used or recycle after treatment;
(7) drying: previous step is obtained 2, and the solid of 5-hexichol amido terephthalic acid obtains 2 120 ℃ of dryings, 5-hexichol amido terephthalic acid (DATA) solid high purity product.
Embodiment two
Main technique equipment is: rising temperature for dissolving equipment, adsorption-edulcoration equipment and in and acidizing unit be tubular chemical reactor, filter plant is a vane-type solid-liquid tripping device.
As shown in the figure, a kind of 2, the separation and refining method of 5-diaryl-amine base terephthalic acid DXTA, be with 2, it is high-purity 2 that the crude product of 5-diaryl-amine base terephthalic acid is that raw material adopts the recrystallization separation and purification to prepare, 5-diaryl-amine base terephthalic acid DXTA, and described method steps is as follows:
(1) rising temperature for dissolving: with raw material 2, the crude product 10.0kg of 5-two p-Chlorobenzoic acid amide base terephthalic acids, 2.8kg potassium hydroxide (KOH) solid and 80kg water add in the tubular chemical reactor, the KOH and 2 that adds, the mol ratio of 5-two p-Chlorobenzoic acid amide base terephthaldehyde acid crudes is 2.2: 1, the amount of water is with respect in the material quantity 2 in the system, the mol ratio water of 5-two p-Chlorobenzoic acid amide base terephthaldehyde acid crudes is 193: 1, service temperature is 120 ℃, the operation absolute pressure is 0.3MPa, neutralization reaction takes place in the rising temperature for dissolving process, generate 2, the aqueous solution of 5-two p-Chlorobenzoic acid amide base potassium terephthalates;
(2) adsorption-edulcoration: the 92.8kg2 that in the previous step tubular chemical reactor, obtains, in the 5-two p-Chlorobenzoic acid amide base terephthalic acid potassium solutions, add adsorption-edulcoration agent molecule sieve 3.0kg and carry out the adsorption-edulcoration operation, the consumption of adsorption-edulcoration agent be the solution body quality 3% (consumption of sorbent material is that the quality of sorbent material and the volume ratio of system are 30kg: 1m
3), the adsorption operations temperature is 98 ℃, working pressure is 0.3MPa;
(3) solid-liquid separates: with previous step obtain 2, the material that adds the adsorption-edulcoration agent in the 5-two p-Chlorobenzoic acid amide base terephthalic acid potassium solutions adopts vane-type solid-liquid tripping device to carry out the solid-liquid separation, the solid-liquid separation obtains the purified mother liquor and enters next step, and the adsorption-edulcoration agent that solid-phase material obtains after the water vapor desorption and regeneration is handled enters previous step, and agent recycles as adsorption-edulcoration;
(4) in and acidifying: the refinement mother liquor that previous step is obtained adds 37% technical hydrochloric acid 4.8kg, and the pH value in the regulation system is 4.Carry out the acidifying neutralizing treatment, material is carried out obtaining 2, the crystalline solid of 5-two p-Chlorobenzoic acid amide base terephthalic acids about cooling operation to 20 ℃ simultaneously;
(5) solid-liquid separates: the material that previous step is obtained adopts vane-type solid-liquid tripping device to carry out the solid-liquid separation, separation obtains 2 through solid-liquid, the solid materials of 5-two p-Chlorobenzoic acid amide base terephthalic acids enters next step, the concentration of salt acquires a certain degree the time in the liquid phase material, and liquid phase material separates the material that removes after desalting through but crystallization, solid-liquid and directly recycles as the water and the raw material of the first step;
(6) washing: previous step is obtained 2, and the solid of 5-two p-Chlorobenzoic acid amide base terephthalic acids is washed operation, gets purified 2, and 5-two p-Chlorobenzoic acid amide base terephthalic acid solid, the water cycle of process washing are applied mechanically and used or recycle after treatment;
(7) drying: previous step is obtained 2, and the solid of 5-two p-Chlorobenzoic acid amide base terephthalic acid acid obtains 2 100 ℃ of dryings, 5-two p-Chlorobenzoic acid amide base terephthalic acid (DpCTA) solid high purity products.
Embodiment three
Main technique equipment is: rising temperature for dissolving equipment, adsorption-edulcoration equipment and in and acidizing unit be static mixer, filter plant is a press filter type solid-liquid tripping device.
As shown in the figure, as shown in the figure, a kind of 2, the separation and refining method of 5-diaryl-amine base terephthalic acid DXTA is with 2, and the crude product of 5-diaryl-amine base terephthalic acid is that raw material adopts the recrystallization separation and purification to prepare high-purity 2,5-diaryl-amine base terephthalic acid DXTA, described method steps is as follows:
(1) rising temperature for dissolving: with raw material 2, two couples of toluidine terephthaldehydes of 5-acid crude 10.0kg and 95.5kg water and 1.0kg liquefied ammonia add in the static mixer, the liquefied ammonia and 2 that adds, the mol ratio of two couples of toluidine terephthaldehydes of 5-acid crude is 2.1: 1, the amount of water is with respect in the material quantity 2 in the system, the mol ratio of 5-two p-Chlorobenzoic acid amide base terephthaldehyde acid crudes is 200: 1, service temperature is 100 ℃, the operation absolute pressure is 0.6MPa, neutralization reaction takes place in the rising temperature for dissolving process, generate 2, the aqueous solution of 5-two (to toluidine) terephthalic acid ammonium;
(2) adsorption-edulcoration: the 100.5kg2 that in the previous step static mixer, obtains, in 5-two (to toluidine) the terephthaldehyde acid ammonium solution, add adsorption-edulcoration agent diatomite 10.0kg and carry out the adsorption-edulcoration operation, the consumption of adsorption-edulcoration agent be the solution body quality 5% (consumption of sorbent material is that the quality of sorbent material and the volume ratio of system are 100kg: 1m
3), the adsorption operations temperature is 120 ℃, working pressure is 0.6MPa;
(3) solid-liquid separates: with previous step obtain 2, the material that adds the adsorption-edulcoration agent in two couples of toluidine terephthaldehydes of 5-acid ammonium solution adopts the press filter type tripping device to carry out the solid-liquid separation, the solid-liquid separation obtains the purified mother liquor and enters next step, and the adsorption-edulcoration agent that solid-phase material obtains after the water vapor desorption and regeneration is handled enters previous step, and agent recycles as adsorption-edulcoration;
(4) in and acidifying: the refinement mother liquor that previous step is obtained adds 28% industrial acetic acid 12.8kg, pH value in the regulation system is 5, carries out the acidifying neutralizing treatment, material is cooled to about 20 ℃ simultaneously, obtain 2, the crystalline solid of two pairs of toluidine terephthalic acids of 5-;
(5) solid-liquid separates: the material that previous step is obtained adopts press filter type solid-liquid tripping device to carry out the solid-liquid separation, separation obtains 2 through solid-liquid, the solid materials of two pairs of toluidine terephthalic acids of 5-enters next step, and liquid phase material separates the material that removes after desalting through crystallisation by cooling, solid-liquid and directly recycles as the water and the raw material of the first step;
(6) washing: previous step is obtained 2, and the solid of two pairs of toluidine terephthalic acids of 5-is washed operation, gets purified 2, and two pairs of toluidine terephthalic acid solid of 5-, the water cycle of process washing are applied mechanically and used or recycle after treatment;
(7) drying: previous step is obtained 2, and the solid of two pairs of toluidine terephthalic acids of 5-obtains 2 80 ℃ of dryings, two pairs of toluidine terephthalic acids of 5-(DTTA) solid high purity product.
Embodiment four
Main technique equipment is: rising temperature for dissolving equipment, adsorption-edulcoration equipment and in and acidizing unit be that the still formula stirs chemical reactor, filter plant is a decanter type solid-liquid tripping device.
As shown in the figure, a kind of 2, the separation and refining method of 5-diaryl-amine base terephthalic acid DXTA, be with 2, it is high-purity 2 that the crude product of 5-diaryl-amine base terephthalic acid is that raw material adopts the recrystallization separation and purification to prepare, 5-diaryl-amine base terephthalic acid DXTA, and described method steps is as follows:
(1) rising temperature for dissolving: it is the lass lining stirred autoclave that the still formula of employing stirs chemical reactor, and with raw material 2, the crude product 10.0kg of 5-hexichol amido terephthalic acid, 2.4kg potassium hydroxide (KOH) solid and 79.0kg water add the 0.128m of strap clamp cover
3In the lass lining stirred autoclave, the KOH and 2 that adds, the mol ratio of 5-hexichol amido terephthalic acid crude product is 2.0: 1, the amount of water is with respect in the material quantity 2 in the system, and the mol ratio of 5-hexichol amido terephthalic acid crude product is 100: 1, and service temperature is 40 ℃, the operation absolute pressure is 0.2MPa, neutralization reaction takes place in the rising temperature for dissolving process, generates 2, the aqueous solution of 5-hexichol amido potassium terephthalate;
(2) adsorption-edulcoration: the 91.4kg 2 that in the previous step glassed steel reaction vessels, obtains, in the 5-hexichol amido potassium terephthalate solution, add adsorption-edulcoration agent activated carbon and diatomite 1.0kg and carry out the adsorption-edulcoration operation, the consumption of adsorption-edulcoration agent be the solution body quality 4% (consumption of sorbent material is that the quality of sorbent material and the volume ratio of system are 50kg: 1m
3), the adsorption operations temperature is 40 ℃, working pressure is 0.2MPa;
(3) solid-liquid separates: with previous step obtain 2, the material that adds the adsorption-edulcoration agent in the 5-hexichol amido potassium terephthalate solution adopts decanter type solid-liquid tripping device to carry out the solid-liquid separation, the solid-liquid separation obtains the purified mother liquor and enters next step, and the adsorption-edulcoration agent that solid-phase material obtains after the water vapor desorption and regeneration is handled enters previous step, and agent recycles as adsorption-edulcoration;
(4) in and acidifying: the refinement mother liquor that previous step is obtained adds 37% technical hydrochloric acid 2.9kg, and the pH value in the regulation system is 3.Carry out the acidifying neutralizing treatment, material is carried out obtaining 2, the crystalline solid of 5-hexichol amido terephthalic acid about cooling operation to 20 ℃ simultaneously;
(5) solid-liquid separates: the material that previous step is obtained adopts decanter type solid-liquid tripping device to carry out the solid-liquid separation, separation obtains 2 through solid-liquid, the solid materials of 5-hexichol amido terephthalic acid enters next step, the concentration of salt acquires a certain degree the time in the liquid phase material, and liquid phase material separates the material that removes after desalting through but crystallization, solid-liquid and directly recycles as the water and the raw material of the first step;
(6) washing: previous step is obtained 2, and the solid of 5-hexichol amido terephthalic acid is washed operation, gets purified 2, and 5-hexichol amido terephthalic acid solid, the water cycle of process washing are applied mechanically and used or recycle after treatment;
(7) drying: previous step is obtained 2, and the solid of 5-hexichol amido terephthalic acid obtains 2 110 ℃ of dryings, 5-hexichol amido terephthalic acid (DATA) solid high purity product.
Embodiment five
Main technique equipment is: rising temperature for dissolving equipment, adsorption-edulcoration equipment and in and acidizing unit be tubular chemical reactor, filter plant is a vane-type solid-liquid tripping device.
As shown in the figure, a kind of 2, the separation and refining method of 5-diaryl-amine base terephthalic acid DXTA, be with 2, it is high-purity 2 that the crude product of 5-diaryl-amine base terephthalic acid is that raw material adopts the recrystallization separation and purification to prepare, and 5-diaryl-amine base terephthalic acid DXTA is characterized in that described method steps is as follows:
(1) rising temperature for dissolving: with raw material 2, the crude product 10.0kg of 5-two p-Chlorobenzoic acid amide base terephthalic acids, 2.8kg sodium hydroxide (NaOH) solid and 80kg water add in the tubular chemical reactor, the NaOH and 2 that adds, the mol ratio of 5-two p-Chlorobenzoic acid amide base terephthaldehyde acid crudes is 2.15: 1, the amount of water is with respect in the material quantity 2 in the system, the mol ratio water of 5-two p-Chlorobenzoic acid amide base terephthaldehyde acid crudes is 128: 1, service temperature is 60 ℃, the operation absolute pressure is 0.5MPa, neutralization reaction takes place in the rising temperature for dissolving process, generate 2, the aqueous solution of 5-two p-Chlorobenzoic acid amide base para-phthalic sodiums;
(2) adsorption-edulcoration: the 92.8kg2 that in the previous step tubular chemical reactor, obtains, add adsorption-edulcoration agent molecule sieve and activated carbon and diatomite 3.0kg in the 5-two p-Chlorobenzoic acid amide base terephthalic acid sodium solutions and carry out the adsorption-edulcoration operation, the consumption of adsorption-edulcoration agent be the solution body quality 2% (consumption of sorbent material is that the quality of sorbent material and the volume ratio of system are 80kg: 1m
3), the adsorption operations temperature is 60 ℃, working pressure is 0.5MPa;
(3) solid-liquid separates: with previous step obtain 2, the material that adds the adsorption-edulcoration agent in the 5-two p-Chlorobenzoic acid amide base terephthalic acid sodium solutions adopts vane-type solid-liquid tripping device to carry out the solid-liquid separation, the solid-liquid separation obtains the purified mother liquor and enters next step, and the adsorption-edulcoration agent that solid-phase material obtains after the water vapor desorption and regeneration is handled enters previous step, and agent recycles as adsorption-edulcoration;
(4) in and acidifying: the refinement mother liquor that previous step is obtained adds acetic acid 4.8kg, and the pH value in the regulation system is 6.Carry out the acidifying neutralizing treatment, material is carried out obtaining 2, the crystalline solid of 5-two p-Chlorobenzoic acid amide base terephthalic acids about cooling operation to 20 ℃ simultaneously;
(5) solid-liquid separates: the material that previous step is obtained adopts vane-type solid-liquid tripping device to carry out the solid-liquid separation, separation obtains 2 through solid-liquid, the solid materials of 5-two p-Chlorobenzoic acid amide base terephthalic acids enters next step, the concentration of salt acquires a certain degree the time in the liquid phase material, and liquid phase material separates the material that removes after desalting through but crystallization, solid-liquid and directly recycles as the water and the raw material of the first step;
(6) washing: previous step is obtained 2, and the solid of 5-two p-Chlorobenzoic acid amide base terephthalic acids is washed operation, gets purified 2, and 5-two p-Chlorobenzoic acid amide base terephthalic acid solid, the water cycle of process washing are applied mechanically and used or recycle after treatment;
(7) drying: previous step is obtained 2, and the solid of 5-two p-Chlorobenzoic acid amide base terephthalic acid acid obtains 2 95 ℃ of dryings, 5-two p-Chlorobenzoic acid amide base terephthalic acid (DpCTA) solid high purity products.
Embodiment six
Main technique equipment is: rising temperature for dissolving equipment, adsorption-edulcoration equipment and in and acidizing unit be static mixer, filter plant is a press filter type solid-liquid tripping device.
As shown in the figure, as shown in the figure, a kind of 2, the separation and refining method of 5-diaryl-amine base terephthalic acid DXTA is with 2, and the crude product of 5-diaryl-amine base terephthalic acid is that raw material adopts the recrystallization separation and purification to prepare high-purity 2,5-diaryl-amine base terephthalic acid DXTA, described method steps is as follows:
(1) rising temperature for dissolving: with raw material 2, two couples of toluidine terephthaldehydes of 5-acid crude 10.0kg and 95.5kg water and 1.0kg liquefied ammonia add in the static mixer, the liquefied ammonia and 2 that adds, the mol ratio of two couples of toluidine terephthaldehydes of 5-acid crude is 2.08: 1, the amount of water is with respect in the material quantity 2 in the system, the mol ratio of 5-two p-Chlorobenzoic acid amide base terephthaldehyde acid crudes is 140: 1, service temperature is 80 ℃, the operation absolute pressure is 0.4MPa, neutralization reaction takes place in the rising temperature for dissolving process, generate 2, the aqueous solution of two pairs of toluidine terephthalic acids of 5-ammonium;
(2) adsorption-edulcoration: the 100.5kg2 that in the previous step static mixer, obtains, in two couples of toluidine terephthaldehydes of 5-acid ammonium solution, add adsorption-edulcoration agent activated carbon 10.0kg and carry out the adsorption-edulcoration operation, the consumption of adsorption-edulcoration agent be the solution body quality 3% (consumption of sorbent material is that the quality of sorbent material and the volume ratio of system are 20kg: 1m
3), the adsorption operations temperature is 80 ℃, working pressure is 0.4MPa;
(3) solid-liquid separates: with previous step obtain 2, the material that adds the adsorption-edulcoration agent in two couples of toluidine terephthaldehydes of 5-acid ammonium solution adopts the press filter type tripping device to carry out the solid-liquid separation, the solid-liquid separation obtains the purified mother liquor and enters next step, and the adsorption-edulcoration agent that solid-phase material obtains after the water vapor desorption and regeneration is handled enters previous step, and agent recycles as adsorption-edulcoration;
(4) in and acidifying: the refinement mother liquor that previous step is obtained adds 98% industrial sulphuric acid 12.8kg, pH value in the regulation system is 4, carries out the acidifying neutralizing treatment, material is cooled to about 20 ℃ simultaneously, obtain 2, the crystalline solid of two pairs of toluidine terephthalic acids of 5-;
(5) solid-liquid separates: the material that previous step is obtained adopts press filter type solid-liquid tripping device to carry out the solid-liquid separation, separation obtains 2 through solid-liquid, the solid materials of two pairs of toluidine terephthalic acids of 5-enters next step, and liquid phase material separates the material that removes after desalting through crystallisation by cooling, solid-liquid and directly recycles as the water and the raw material of the first step;
(6) washing: previous step is obtained 2, and the solid of two pairs of toluidine terephthalic acids of 5-is washed operation, gets purified 2, and two pairs of toluidine terephthalic acid solid of 5-, the water cycle of process washing are applied mechanically and used or recycle after treatment;
(7) drying: previous step is obtained 2, and the solid of two pairs of toluidine terephthalic acids of 5-obtains 2 118 ℃ of dryings, two pairs of toluidine terephthalic acids of 5-(DTTA) solid high purity product.
Remove the various embodiments described above, embodiment of the present invention also have a lot, and the technical scheme that all employings are equal to or equivalence is replaced is all within protection scope of the present invention.
Claims (9)
1. one kind 2, the separation and refining method of 5-diaryl-amine base terephthalic acid DXTA is with 2, and the crude product of 5-diaryl-amine base terephthalic acid is that raw material adopts the recrystallization separation and purification to obtain high-purity 2,5-diaryl-amine base terephthalic acid DXTA is characterized in that described method steps is as follows:
(1) rising temperature for dissolving: with raw material 2, carry out rising temperature for dissolving in the crude product of 5-diaryl-amine base terephthalic acid, mineral alkali and the water adding rising temperature for dissolving equipment, make 2,5-diaryl-amine base terephthalic acid is dissolved in the inorganic alkali solution, neutralization reaction takes place in the rising temperature for dissolving process, generate 2, the aqueous solution of 5-diaryl-amine base terephthalate;
(2) adsorption-edulcoration: in adsorption-edulcoration equipment, with previous step obtain 2, add the operation of adsorption-edulcoration agent carrying out adsorption-edulcoration in the 5-diaryl-amine base terephthalic acid salts solution;
(3) solid-liquid separates: with previous step obtain 2, the material that adds the adsorption-edulcoration agent in the 5-diaryl-amine base terephthalic acid salts solution carries out solid-liquid to be separated, the solid-liquid separation obtains the purified mother liquor and enters next step, and the adsorption-edulcoration agent that solid-phase material obtains after manipulation of regeneration enters previous step and recycles;
(4) in and acidifying: the refinement mother liquor that previous step is obtained adds mineral acid and carries out the acidifying neutralizing treatment, and neutralizing treatment finishes back control pH value 2～6, obtains 2, the crystalline solid of 5-diaryl-amine base terephthalic acid;
(5) solid-liquid separates: separation obtains 2 to the material that previous step is obtained through solid-liquid, the solid materials of 5-diaryl-amine base terephthalic acid enters next step, and the material that liquid phase material is removed behind the inorganic salt through crystallisation by cooling, solid-liquid separation directly recycles as the water and the raw material of the first step;
(6) washing: previous step is obtained 2, and the solid of 5-diaryl-amine base terephthalic acid is washed operation, gets purified 2, and 5-diaryl-amine base terephthalic acid solid, the water cycle of process washing are applied mechanically and used or recycle after treatment;
(7) drying: previous step is obtained 2, and the solid of 5-diaryl-amine base terephthalic acid obtains 2 80 ℃～120 ℃ dryings, 5-diaryl-amine base terephthalic acid DXTA solid high purity product.
2. described 2 according to claim 1, the separation and refining method of 5-diaryl-amine base terephthalic acid DXTA, it is characterized in that: the mineral alkali described in the first step rising temperature for dissolving is any one in sodium hydroxide, potassium hydroxide or the ammonia.
3. according to claim 1 described 2, the separation and refining method of 5-diaryl-amine base terephthalic acid DXTA, it is characterized in that: the consumption of mineral alkali is with respect in the material quantity 2 in the first step rising temperature for dissolving, the mol ratio of 5-diaryl-amine base terephthalic acid is 2.05～2.2: 1, the consumption of water is with respect in the material quantity 2 in the system, and the mol ratio of 5-diaryl-amine base terephthalic acid is 100～200: 1.
4. described 2 according to claim 1, the separation and refining method of 5-diaryl-amine base terephthalic acid DXTA is characterized in that: service temperature is 40 ℃～120 ℃ in the first step rising temperature for dissolving, and the operation absolute pressure is 0.1MPa～0.6MPa.
5. described 2 according to claim 1, the separation and refining method of 5-diaryl-amine base terephthalic acid DXTA is characterized in that: in the 4th step and described in the acidifying is in sulfuric acid, hydrochloric acid or the acetic acid any one.
6. described 2 according to claim 1, the separation and refining method of 5-diaryl-amine base terephthalic acid DXTA is characterized in that: the service temperature of the second step adsorption-edulcoration is 40 ℃～120 ℃, and working pressure is 0.1MPa～0.6MPa.
7. according to claim 1 described 2, the separation and refining method of 5-diaryl-amine base terephthalic acid DXTA is characterized in that: the described adsorption-edulcoration agent of second step in the adsorption-edulcoration is the mixture of any one or any two kinds or any three kinds of components in molecular sieve or activated carbon or the diatomite.
8. according to claim 1 described 2, the separation and refining method of 5-diaryl-amine base terephthalic acid DXTA is characterized in that: the first step rising temperature for dissolving equipment and the second step adsorption-edulcoration equipment and in the 4th step and acidizing unit be that the still formula stirs any one in chemical reactor, tubular chemical reactor or the static mixer.
9. according to claim 1 described 2, the separation and refining method of 5-diaryl-amine base terephthalic acid DXTA is characterized in that: the 3rd step and described solid-liquid tripping device of the 5th step are any one in decanter type or press filter type or centrifugal or the vane-type solid-liquid tripping device.
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| CN114195665A (en) * | 2021-12-14 | 2022-03-18 | 武汉世吉药业有限公司 | Neutralization and acidification process and equipment for high-purity NCAA |
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| CN1080283A (en) * | 1992-05-12 | 1994-01-05 | 赫彻斯特股份公司 | 2, the preparation method of 5-diphenyl amino-terephthalic acid and dialkyl ester thereof |
| CN1244522A (en) * | 1998-08-07 | 2000-02-16 | 中外合资湘潭大华颜料化学有限公司 | Production process of dihalo anilino p-benzene dicarboxylic acid |
| CN101448780A (en) * | 2006-05-22 | 2009-06-03 | 太阳化学公司 | 2,5-di(methoxyanilino)terephthalic acid polymorphs and quinacridones realized therefrom |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1080283A (en) * | 1992-05-12 | 1994-01-05 | 赫彻斯特股份公司 | 2, the preparation method of 5-diphenyl amino-terephthalic acid and dialkyl ester thereof |
| CN1244522A (en) * | 1998-08-07 | 2000-02-16 | 中外合资湘潭大华颜料化学有限公司 | Production process of dihalo anilino p-benzene dicarboxylic acid |
| CN101448780A (en) * | 2006-05-22 | 2009-06-03 | 太阳化学公司 | 2,5-di(methoxyanilino)terephthalic acid polymorphs and quinacridones realized therefrom |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114195665A (en) * | 2021-12-14 | 2022-03-18 | 武汉世吉药业有限公司 | Neutralization and acidification process and equipment for high-purity NCAA |
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