CN212640339U - Equipment for preparing p-anisidine - Google Patents
Equipment for preparing p-anisidine Download PDFInfo
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- CN212640339U CN212640339U CN202021114221.9U CN202021114221U CN212640339U CN 212640339 U CN212640339 U CN 212640339U CN 202021114221 U CN202021114221 U CN 202021114221U CN 212640339 U CN212640339 U CN 212640339U
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Abstract
The utility model provides a preparation equipment of para anisidine. The apparatus comprises: the hydrogenation reaction kettle is used for carrying out hydrogenation reaction; and the catalyst pulping kettle is connected with the inlet of the hydrogenation reaction kettle through a pipeline and is used for replenishing the catalyst in the hydrogenation reaction process. The p-anisidine prepared by the equipment of the utility model has high purity, high yield and higher content, and can meet the requirement of the disperse dye intermediate 2-amino-4-acetamino anisole on the raw material. Further, the utility model discloses a preparation equipment of para anisidine, the energy resource consumption of this equipment is low, and is with low costs to can realize serialization production, the productivity improves greatly.
Description
Technical Field
The utility model relates to a preparation method of para anisidine and equipment for preparing the para anisidine, which belong to the field of fine chemical engineering and chemical equipment.
Background
P-anisidine of formula C7H9NO, molecular weight 123.15, is an important dye and pharmaceutical intermediate. In the dye industry, the method is a main raw material for synthesizing a disperse dye intermediate 2-amino-4-acetamino anisole. In the field of medicine, it can be used as raw material for synthesizing medicines of atabrine, indomethacin and others. Currently, the global demand for para-anisidine is up to several tens of thousands of tons.
Among conventional industrial synthetic methods, the conventional method for producing p-anisidine is to reduce p-nitroanisole by sodium sulfide or Fe powder to prepare p-anisidine. However, the process has the defects of high consumption, high cost, poor quality and the like, and particularly has large discharge amount of waste water and waste residue, thereby causing serious environmental pollution. If the waste water and the waste residue are treated, the cost is greatly increased, and secondary pollution is possibly caused by improper treatment.
At present, the catalytic hydrogenation reduction method slowly replaces the reduction of sodium sulfide, generally, methanol and paranitroanisole solution are reduced under certain hydrogen pressure, then the catalyst is separated, and then the methanol is recovered, and finally the paraanisidine is obtained. The method has stable quality, the byproduct is water, and the method is environment-friendly, but the solvent recovery is troublesome, the method has the defects of high energy consumption, large solvent loss and the like, and the methanol can also cause environmental pollution.
Patent publication CN1861570A discloses two methods for preparing p-anisidine by a catalytic hydrogenation method. The method takes methanol as a solvent, takes a p-nitroanisole mixture as a raw material, takes Raney-Ni or Pd-C as a catalyst, introduces hydrogen to carry out catalytic hydrogenation reduction reaction, and finishes the catalytic hydrogenation reaction when no more hydrogen is consumed; after the catalyst is recovered from the reaction mixture, the oil phase is separated by liquid-liquid separation and recrystallized to obtain the required p-anisidine. The method is a clean production process, has low corrosion to equipment, and can reduce pollution. However, this method ends the catalytic hydrogenation reduction reaction on the basis of "no more hydrogen consumption", so that the control of the end point of the reaction is not very accurate, and thus it is difficult to prepare p-anisidine with high yield and high selectivity, and the purity of the target product is only 98%.
Patent publication CN105272863A discloses a method for preparing P-anisidine, which comprises the step of hydrogenating P-anisidine liquid phase by batch hydrogenation in the presence of a ternary amorphous alloy catalyst of Ni-Mo-B or Ni-Co-P. It is claimed that p-anisidine can be obtained in a purity of up to 99% or more. However, the preparation method is too complex, the content of the mixed solution needs to be detected every hour, the equipment consumption is high, the cost is too high, the energy consumption is high, the solvent loss is large, and more manpower and material resources are wasted.
Therefore, research on a preparation method of p-anisidine and equipment for preparing the p-anisidine, which have the advantages of relative simplicity, low equipment consumption, low cost, high purity of the p-anisidine and small solvent loss, is a technical problem to be solved urgently.
SUMMERY OF THE UTILITY MODEL
Utility modelProblems to be solved
In view of the technical problem that exists among the prior art, for example, preparation method is too complicated, needs the content of detecting the mixed liquid every hour, and equipment consumption is very big, and is with high costs, and energy resource consumption is high, and the solvent loss is big, extravagant more manpower and materials, and the yield is low, and to anisidine's purity low grade, the utility model provides an equipment for preparing anisidine, the energy resource consumption of this equipment is low, and is with low costs to can realize serialization production, the productivity improves greatly.
Means for solving the problems
The utility model provides a preparation para anisidine's equipment, it includes:
the hydrogenation reaction kettle is used for carrying out hydrogenation reaction; and
and the catalyst pulping kettle is connected with the inlet of the hydrogenation reaction kettle through a pipeline and is used for replenishing the catalyst in the hydrogenation reaction process.
According to the utility model discloses an equipment, wherein, equipment still includes: and the storage tank is connected with the inlet of the hydrogenation reaction kettle through a pipeline.
According to equipment, wherein, the storage tank includes at least one kind in paranitroanisole storage tank, hydrogen storage tank and the nitrogen gas storage tank.
According to the utility model discloses an equipment, wherein, equipment still includes:
a continuous settling tank comprising at least an inlet, a first outlet, and a second outlet; wherein the inlet of the continuous settling tank is connected with the outlet of the hydrogenation reaction kettle through a pipeline; the first outlet is positioned at the bottom of the continuous settling tank, and the first outlet is connected with the inlet of the hydrogenation reaction kettle through a pipeline.
According to the utility model discloses an equipment, wherein, equipment still includes:
and the filtering device is connected with the outlet of the hydrogenation reaction kettle or the second outlet of the continuous settling tank and is used for separating to obtain a p-anisidine final product.
According to the utility model discloses an equipment, wherein be provided with the sample connection on the entry of continuous settling tank with the pipeline between hydrogenation cauldron's the export.
The equipment of, wherein be provided with first measuring pump between the p-nitroanisole storage tank with the hydrogenation cauldron.
According to the utility model discloses an equipment, wherein be provided with the second measuring pump on the pipeline between catalyst making beating cauldron and the hydrogenation cauldron.
According to the utility model discloses an equipment, wherein, be provided with the third metering pump on the pipeline between the first export of continuous settling tank and hydrogenation cauldron's entry.
The equipment of the utility model, wherein, a balance valve is arranged on the pipeline between the second outlet of the continuous settling tank and the inlet of the hydrogenation reaction kettle; and/or
Overflow valves are arranged on pipelines of the inlet of the continuous settling tank and the outlet of the hydrogenation reaction kettle; and/or
And an emptying pipeline connected with a second outlet of the continuous settling tank is also arranged on the continuous settling tank, and an emptying valve is arranged in the emptying pipeline to control the opening and closing of the emptying pipeline.
Effect of the utility model
The p-anisidine prepared by the equipment of the utility model has high purity, high yield and higher content, and can meet the requirement of the disperse dye intermediate 2-amino-4-acetamino anisole on the raw material.
Further, the utility model discloses a preparation equipment of para anisidine, the energy resource consumption of this equipment is low, and is with low costs to can realize serialization production, the productivity improves greatly.
Drawings
Fig. 1 shows an apparatus for preparing p-anisidine according to an embodiment of the present invention.
Description of the reference numerals
A is a p-nitroanisole storage tank; b is a hydrogen storage tank; c is a nitrogen storage tank;
d is a catalyst pulping kettle; e is a hydrogenation reaction kettle; f is a continuous settling tank;
g is a filtering device; h is a p-anisidine end product storage tank;
p-1 is a first metering pump; p-2 is a second metering pump;
p-3 is a third metering pump.
Detailed Description
Hereinafter, the present invention will be described in detail. The technical features described below are explained based on typical embodiments and specific examples of the present invention, but the present invention is not limited to these embodiments and specific examples. It should be noted that:
in the present specification, the numerical range represented by "numerical value a to numerical value B" means a range including the end point numerical value A, B.
In the present specification, "plural" in "plural", and the like means a numerical value of 2 or more unless otherwise specified.
In this specification, the terms "substantially", "substantially" or "substantially" mean an error of less than 5%, or less than 3% or less than 1% as compared to the relevant perfect or theoretical standard.
In the present specification, the meaning of "may" includes both the meaning of performing a certain process and the meaning of not performing a certain process.
In this specification, "optional" or "optionally" means that the subsequently described event or circumstance may or may not occur, and that the description includes instances where the event occurs and instances where it does not.
In the present specification, reference to "some particular/preferred embodiments," "other particular/preferred embodiments," "embodiments," and the like, means that a particular element (e.g., feature, structure, property, and/or characteristic) described in connection with the embodiment is included in at least one embodiment described herein, and may or may not be present in other embodiments. In addition, it is to be understood that the described elements may be combined in any suitable manner in the various embodiments.
First aspect
The utility model discloses a first aspect provides a preparation method of p-anisidine, and it includes following step:
step 1) providing a p-nitroanisole raw material, and carrying out hot melting treatment on the p-nitroanisole raw material to obtain p-nitroanisole in a molten state;
step 2) under the condition that a catalyst exists, taking a first part of p-nitroanisole in a molten state to carry out hydrogenation reaction to obtain a p-anisidine primary product;
and 3) continuously adding a second part of p-nitroanisole in a molten state into the p-anisidine primary product, supplementing a catalyst, continuously carrying out hydrogenation reaction, and separating and obtaining a p-anisidine final product.
The utility model discloses the technical scheme who adopts, the reaction equation is as follows:
the utility model discloses a preparation method of p-anisidine uses the p-nitroanisole of molten state as the solvent, earlier reacts the p-nitroanisole hydrogenation of molten state to the amino anisole primary product, uses p-anisidine primary product self as the solvent again, and catalyst and molten state p-nitroanisole are added to continuous ration, obtain p-anisidine final product. Furthermore, the final product of the amino anisole and the catalyst can be obtained by collection and separation of a settling kettle and a filtering device, and the whole system keeps the balance of feeding and discharging. Specifically, the method comprises the following steps:
the p-nitroanisole in a molten state is obtained by hot melting, the temperature of the hot melting is 50-100 ℃, preferably 60-80 ℃, for example: the temperature of the hot melting can be 55 ℃, 62 ℃, 65 ℃, 68 ℃, 70 ℃, 72 ℃, 75 ℃, 78 ℃, 85 ℃, 90 ℃, 95 ℃ and the like. In addition, the paranitroanisole in a molten state can be stored in a storage tank, and the storage tank is convenient to use.
The catalyst used in the reaction system is not particularly limited in the present invention, and may be a catalyst commonly used in the art. Specifically, the catalyst in step 2) and/or step 3) includes a raney nickel metal catalyst, a skeletal nickel metal catalyst, a noble metal catalyst (for example: au, etc.) in a predetermined amount. Among them, one or both of a raney nickel metal catalyst and a skeletal nickel metal catalyst are preferably used.
In the hydrogenation reaction, it is necessary to purge the gas in the hydrogenation reaction vessel before use, and the gas in the hydrogenation reaction vessel may be purged by using an inert gas, for example, nitrogen gas. After the gas in the hydrogenation reaction kettle is completely removed by using nitrogen, hydrogen is used for replacing the nitrogen, so that the hydrogenation reaction is effectively carried out.
The amount of hydrogen is not particularly limited, and is generally determined according to the reaction equation. In general, hydrogen may be used in excess for the purpose of orderly progress of the reaction. The amount of hydrogen used may be determined depending on the pressure of the system, and generally, the pressure of the system may be maintained at 0.1 to 5.0MPa, and the pressure may be lowered when the chemical reaction is carried out in the system, and the hydrogen may be continuously introduced until the reaction is completed when the pressure of the system is not changed in order to keep the pressure unchanged.
In some specific embodiments, in step 2), the catalyst is added in an amount of 0.5 to 20%, preferably 1 to 15%, based on the total mass of the first portion of p-nitroanisole in molten state. When the adding amount of the catalyst is 0.5-20%, the first part of the p-nitroanisole in a molten state can be completely reacted to obtain a p-anisidine primary product, wherein the specific gravity of the p-nitroanisole at room temperature is 1.233. Specifically, the catalyst may be added in an amount of 0.8%, 2%, 4%, 6%, 8%, 10%, 12%, 14%, 16%, 18%, etc.
Further, in the step 2), in order to more efficiently perform the hydrogenation reaction, the temperature of the hydrogenation reaction is 50 to 100 ℃, preferably 60 to 80 ℃, and the pressure of the hydrogenation reaction is 0.1 to 5.0MPa, preferably 0.5 to 4MPa, more preferably 1 to 3MPa, and still more preferably 1 to 2 MPa. Specifically, the temperature of the hydrogenation reaction may be 55 ℃, 62 ℃, 65 ℃, 68 ℃, 70 ℃, 72 ℃, 75 ℃, 78 ℃, 85 ℃, 90 ℃, 95 ℃ or the like. The pressure of the hydrogenation reaction may be 0.5MPa, 1MPa, 1.5MPa, 2MPa, 2.5MPa, 3MPa, 3.5MPa, 4MPa, 4.5MPa, etc.
In the step 3), when the p-anisidine end product is prepared, as the p-anisidine end product is output, a part of the catalyst inevitably leaves the system along with the p-anisidine end product, so that a part of the catalyst needs to be added to keep the balance of the catalyst in the system. The catalyst can be a completely new and unused catalyst or a catalyst recovered from a reaction system. In some specific embodiments, the amount of the catalyst added is 1 to 30 per thousand based on the total mass of the second part of the p-nitroanisole in the molten state, wherein the specific gravity of the p-nitroanisole at room temperature is 1.233. Specifically, the addition amount of the catalyst can be 2%, 4%, 6%, 8%, 10%, 12%, 14%, 16%, 18%, 20%, 22%, 24%, 26%, 28% and the like.
In order to better realize the addition of the catalyst to the system, the added catalyst can be added in the form of a catalyst-water mixture, and preferably, the mass concentration of the catalyst in the catalyst-water mixture is 1-10%. Specifically, the mass concentration of the catalyst may be 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, or the like.
It should be noted that, for the second part of the p-nitroanisole in molten state and the additional catalyst-water mixture, the p-nitroanisole in molten state and the additional catalyst-water mixture can be continuously added into the reaction system at a certain flow rate, so that the system balance can be better maintained. Specifically, in the present invention, when the volume of the hydrogenation reaction kettle is 0.5-10L, the flow rate of the second molten p-nitroanisole may be 0.5-10L/h, for example, the flow rate of the second molten p-nitroanisole is 1L/h, 2L/h, 3L/h, 4L/h, 5L/h, 6L/h, 7L/h, 8L/h, 9L/h, etc.; the flow rate of the catalyst-water mixture may be 0.05 to 2L/h, for example, the flow rate of the catalyst-water mixture is 0.1L/h, 0.3L/h, 0.5L/h, 0.8L/h, 1L/h, 1.2L/h, 1.5L/h, 1.8L/h, etc.
The utility model discloses still introduce dwell time's notion, specifically, to hydrogenation's dwell time, it is according to hydrogenation cauldron's volume and carry to the flow determination of adding reation kettle's total material. In particular, the residence time of the hydrogenation reaction may mean the use of a certain volume (V, dm)3) The hydrogenation reaction kettle is used for reaction, the total material conveyed to the hydrogenation reaction kettle is added into a reaction system at a certain flow rate (Q, L/h), the residence time (T, h) is V/Q, and the formula (I) is expressed as follows. Namely:
T＝V/Q (I)
wherein T is the residence time of the hydrogenation reaction, h;
v is the volume of the hydrogenation reaction kettle dm3；
Q is the flow of the total material conveyed to the hydrogenation reaction kettle, and L/h.
Wherein, in the utility model discloses in, the total material of carrying to the hydrogenation cauldron includes the flow of the p-nitroanisole of second part molten state, the flow of catalyst-water mixture and optionally the retrieval and utilization flow three's that some products return to the hydrogenation cauldron after separating at the back sum.
For the units in the formula, various conversions can be made according to specific situations. For example: the volume of the hydrogenation reaction kettle is 10 cubic meters, the total material conveyed to the hydrogenation reaction kettle is conveyed in at a flow rate of 5 cubic meters per hour, and the retention time is 2 hours.
Further, in the step 3), in order to make the hydrogenation reaction more effectively proceed, the residence time of the hydrogenation reaction is 1-5 hours, the temperature of the hydrogenation reaction is 50-100 ℃, and the pressure of the hydrogenation reaction is 0.1-5.0 MPa. Specifically, the residence time of the hydrogenation reaction may be 1.5 hours, 2 hours, 2.5 hours, 3 hours, 3.5 hours, 4 hours, 4.5 hours, or the like; the hydrogenation reaction temperature can be 55 ℃, 62 ℃, 65 ℃, 68 ℃, 70 ℃, 72 ℃, 75 ℃, 78 ℃, 85 ℃, 90 ℃, 95 ℃ and the like; the pressure of the hydrogenation reaction may be 0.5MPa, 1MPa, 1.5MPa, 2MPa, 2.5MPa, 3MPa, 3.5MPa, 4MPa, 4.5MPa, etc.
The separation method in step 3), which is not particularly limited in the present invention, may be any separation method commonly used in the art. In particular, in some particular embodiments, in order to allow the reaction to proceed continuously without affecting the quality of the reaction product, the separation may include settling and/or filtration to give the para-anisidine end product.
Most of the catalyst in the reaction product can be removed by settling, and the quality of the part of the catalyst is hardly changed, and although some reaction products are doped, because other impurity substances are not introduced, the part of the catalyst doped with some reaction products can be directly reused in the reaction system. For the catalyst doped with some reaction products reused in the reaction system, it can be reused in the reaction system at a certain flow rate, generally speaking, the reuse flow rate can be 20-60%, preferably 25-50% of the flow rate of the p-nitroanisole feed in the second molten state, for example: may be 22%, 30%, 32%, 35%, 38%, 40%, 42%, 45%, 52%, 55%, 58%, etc.
In the process of sedimentation, reaction products flow into the sedimentation system at a certain flow rate, so that sedimentation also has a certain retention time. This residence time is analogous to the meaning of the residence time of the hydrogenation reaction. In particular, the residence time of the sedimentation may mean the use of a sediment having a certain volume (V', dm)3) The reaction product is settled in a settling kettle with a certain flow rate (Q)1', L/h) is fed to a continuous settling tank and the catalyst, doped with some reaction product, is fed at a certain flow rate (Q)2', L/h) is discharged from the continuous settling tank, the residence time (T', h) is V '/(Q'1-Q2') table of the following formula (I)Shown in the figure. Namely:
T’＝V’/(Q1’-Q’2) (I)
wherein T' is the residence time of the sedimentation, h;
v' is the volume of the settling vessel, dm3；
Q1' is the flow rate of the reaction product, L/h;
Q2' is the flow rate, L/h, of the catalyst doped with some reaction products.
In some specific embodiments, the residence time for settling is from 1 to 5 hours, for example: 1.1 hour, 1.5 hours, 2 hours, 2.5 hours, 3 hours, 3.5 hours, 4 hours, 4.5 hours, etc. Furthermore, in order not to influence the reaction system, the sedimentation process needs heat preservation treatment, and the temperature of the heat preservation treatment is 50-100 ℃. For example: 55 deg.C, 62 deg.C, 65 deg.C, 68 deg.C, 70 deg.C, 72 deg.C, 75 deg.C, 78 deg.C, 85 deg.C, 90 deg.C, 95 deg.C, etc.
Specifically, in the present invention, the flow rate of the reaction product flowing into the settling system is generally the sum of the flow rates of the second part of the p-nitroanisole in the molten state and the catalyst-water mixture flowing into the reaction system. In the present invention, when the volume of the continuous settling tank is 0.5 to 10L, the flow rate of the reaction product flowing into the settling system may be 0.55 to 12L. For example, the flow rate of the reaction product into the settling system may be 1L/h, 2L/h, 3L/h, 4L/h, 5L/h, 6L/h, 7L/h, 8L/h, 9L/h, 10L/h, 11L/h, etc. In addition, since settling does not completely separate the catalyst, filtration can also be used after settling so that the catalyst and some solid suspended matter can be effectively separated from the reaction product to obtain the p-anisidine end product. Similarly, the filtration process is also required to be heat-preserved in order not to affect the reaction system, and the temperature of the heat-preservation treatment is 50-100 ℃. For example: 55 deg.C, 62 deg.C, 65 deg.C, 68 deg.C, 70 deg.C, 72 deg.C, 75 deg.C, 78 deg.C, 80 deg.C, 82 deg.C, 85 deg.C, 88 deg.C, 90 deg.C, 95 deg.C, etc. For a small amount of catalyst obtained by filtering and separating, the effective components in the catalyst can be collected and extracted, and the catalyst can be used for preparing new catalysts and the like. Finally, the p-anisidine end product after sedimentation and/or filtration can be continuously conveyed out of the reaction system at a certain flow rate. Finally, the product is dehydrated to obtain a solid p-anisidine end product, the dehydration treatment of the utility model is not particularly limited, and the dehydration treatment can be a dehydration mode commonly used in the field.
The utility model discloses a preparation method of p-anisidine is simple and easy, can save material cost, need not to use other organic solvents, also need not to retrieve the solvent to can save material cost, and can not produce the waste water of the high COD of high salt, green can not cause the pollution to the environment.
The preparation method of the para anisidine of the utility model can obtain the following technical effects:
1. the p-anisidine is not only a product, but also a solvent, so that other organic solvents are not used, and the cost of raw materials is saved;
2. the solvent is not required to be recycled, so that a large amount of manpower and material resources are saved;
3. high-salt and high-COD wastewater cannot be generated;
4. continuous production and greatly improved productivity.
Second aspect of the invention
As shown in fig. 1, a second aspect of the present invention provides an apparatus for preparing p-anisidine, comprising:
the hydrogenation reaction kettle E is used for carrying out hydrogenation reaction; and
and the catalyst pulping kettle D is connected with the inlet of the hydrogenation reaction kettle E through a pipeline and is used for supplementing the catalyst in the hydrogenation reaction process.
The hydrogenation reaction of the utility model is carried out in the hydrogenation reaction kettle E. The catalyst pulping kettle D is internally provided with a catalyst-water mixture, and the catalyst pulping kettle D comprises a stirrer, so that the catalyst can be kept in a uniformly dispersed state under high-speed stirring.
In some specific embodiments, the apparatus of the present invention further comprises: the storage tank is connected with the inlet of the hydrogenation reaction kettle E through a pipeline; preferably, the storage tank comprises at least one of a p-nitroanisole storage tank A, a hydrogen storage tank B and a nitrogen storage tank C.
The p-nitroanisole storage tank A is used for storing the p-nitroanisole in a molten state, and the hydrogen storage tank B is used for storing hydrogen for the hydrogenation reaction kettle E to replace gas and carry out hydrogenation reaction. And the nitrogen storage tank C is used for storing nitrogen for replacing gas in the hydrogenation reaction kettle E.
In some specific embodiments, the apparatus further comprises: a continuous settling tank F comprising at least an inlet, a first outlet, and a second outlet; wherein the inlet of the continuous settling tank F is connected with the outlet of the hydrogenation reaction kettle E through a pipeline; the first outlet is positioned at the bottom of the continuous settling tank F, and the first outlet is connected with the inlet of the hydrogenation reaction kettle E through a pipeline. Specifically, an overflow valve is further disposed on a pipeline between an inlet of the continuous settling tank F and an outlet of the hydrogenation reactor E, and the overflow valve is used for being opened at a proper time so that a hydrogenation reaction product is conveyed to the continuous settling tank F.
Further, a balance valve can be arranged on a pipeline between a second outlet of the continuous settling tank F and an inlet of the hydrogenation reaction kettle E, in addition, an emptying pipeline connected with the second outlet of the continuous settling tank F is also arranged on the continuous settling tank F, and an emptying valve is arranged in the emptying pipeline to control the opening and closing of the emptying pipeline. The hydrogenation reactor E and the continuous settling tank F can be kept at the same pressure by using a balance valve and a vent valve.
In some specific embodiments, the apparatus may further include a filtering device G connected to the outlet of the hydrogenation reactor E or the second outlet of the continuous settling tank F for separating to obtain a p-anisidine end product.
Further, a sampling port is arranged on a pipeline between the inlet of the continuous settling tank F and the outlet of the hydrogenation reaction kettle E. The purity of the primary product of p-anisidine in the reaction system can be known by sampling at a sampling port.
In addition, in order to control the consumption of raw materials and catalysts, a first metering pump P-1 can be arranged between the P-nitroanisole storage tank A and the hydrogenation reaction kettle E, and/or a second metering pump P-2 can be arranged on a pipeline between the catalyst pulping kettle D and the hydrogenation reaction kettle E, and/or a third metering pump P-3 can be arranged on a pipeline between a first outlet of the continuous settling tank F and an inlet of the hydrogenation reaction kettle E.
The first metering pump P-1 is used for conveying the molten nitroanisole in the P-nitroanisole storage tank A to the hydrogenation reactor E according to a certain flow rate; the second metering pump P-2 is used for conveying the catalyst-water mixture in the catalyst pulping kettle D into the hydrogenation reaction kettle E at a certain flow rate; the third metering pump P-3 is a catalyst recycling metering pump and is used for conveying the catalyst doped with some reaction products to the hydrogenation reaction kettle E according to a certain flow rate.
Further, in order that the finally obtained p-anisidine end product is not contaminated, the p-anisidine end product storage tank H may be used to store the p-anisidine end product.
In a particular embodiment, when the apparatus of the present invention is used, the method for preparing p-anisidine comprises:
(1) heating and melting paranitroanisole, storing the paranitroanisole in a paranitroanisole storage tank A, conveying a first part of paranitroanisole into a hydrogenation reaction kettle E through a first metering pump P-1, replacing gas with nitrogen in a nitrogen storage tank C, and adding a certain amount of catalyst into the hydrogenation reaction kettle E;
(2) replacing the reaction system gas with nitrogen in the nitrogen storage tank C again, and replacing the nitrogen with hydrogen in the hydrogen storage tank B;
(3) pressurizing the reaction system by using hydrogen in a hydrogen storage tank B, stirring at a high speed under a certain temperature and pressure, and carrying out hydrogenation reaction; preferably, the temperature is 50-100 ℃, and the pressure is 0.1-5.0 MPa;
(4) opening a discharging overflow valve after the reaction is qualified, and meanwhile slowly inputting a p-nitroanisole and catalyst-water mixture in a molten state to keep the balance of inlet and outlet, and always keeping a certain temperature and pressure during the reaction; preferably, the residence time of the reaction is 1 to 5 hours, the temperature is 50 to 100 ℃, and the pressure is 0.1 to 5.0 MPa;
(5) and conveying the reaction product and part of the catalyst to a continuous settling tank F, wherein clear liquid at a second outlet on the continuous settling tank F is a P-anisidine final product and a trace amount of the catalyst, further filtering by a filtering device G to obtain high-purity P-anisidine, namely the P-anisidine final product, storing the high-purity P-anisidine final product in a P-anisidine final product storage tank H, and returning the catalyst doped with some reaction products at the bottom of the continuous settling tank F to the hydrogenation reaction kettle E through a third metering pump P-3 at a certain flow rate. Wherein the settling residence time is 1-5 hours, in addition, the settling process needs heat preservation treatment, and the temperature of the heat preservation treatment is 50-100 ℃. Similarly, the filtration process also requires a heat-preservation treatment at a temperature of 50-100 ℃. And finally, dehydrating the product to obtain a solid p-anisidine final product.
In addition, it should be noted that, when the method for producing p-anisidine of the present invention is described in the first aspect, the conditions of the various reaction systems have been described in detail, and therefore, the conditions and the like of the various reaction systems in the second aspect of the present invention are not described in any more detail, and when the steps are the same as those of the first aspect, the reaction conditions and the like are also completely the same.
The utility model discloses an implement equipment of preparation method to anisidine, the energy resource consumption of this equipment is low, and is with low costs to can realize serialization production, the productivity improves greatly.
Examples
Embodiments of the present invention will be described in detail below with reference to examples, but those skilled in the art will understand that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
Example 1
Adding 10L of p-nitroanisole in a molten state into the p-nitroanisole storage tank A, keeping the temperature at 65 +/-5 ℃, keeping the temperature of the whole reaction system well, and continuously adding the p-nitroanisole in the molten state into the nitroanisole storage tank A in the reaction process so as to ensure that the reaction can be normally carried out.
And (3) starting a first metering pump P-1 to pump a first part of the P-nitroanisole in the molten state into a hydrogenation reaction kettle E, wherein the volume of the first part of the P-nitroanisole in the molten state is 3L, and the volume of the hydrogenation reaction kettle is 5L. And after the nitrogen replacement reaction system is qualified, 240g of Raney nickel metal catalyst is added into the hydrogenation reaction kettle E, the nitrogen replacement reaction system is used again, then the reaction system is replaced by hydrogen, the pressure is kept at 1.3MPa, the temperature is 65 +/-5 ℃, and high-speed stirring is started under the temperature and pressure condition to carry out hydrogenation reaction. Until the reaction system does not absorb hydrogen, sampling at a sampling port to detect that the purity of the p-anisidine is 99.23%.
And (2) continuing to start the first metering pump P-1 and the second metering pump P-2, feeding a second part of molten P-nitroanisole in the P-nitroanisole storage tank A to the hydrogenation reactor E at a flow rate of 1.5L/h, supplementing the Raney nickel metal catalyst-water mixture in the catalyst pulping kettle D to the hydrogenation reactor E at a supplement amount of 0.5L/h (the mass concentration of the catalyst is 4%), keeping the temperature and the pressure of the hydrogenation reactor E unchanged, and keeping the retention time of the hydrogenation reaction for 2 h.
And simultaneously opening an overflow valve to convey materials into the continuous settling tank F, conveying the reaction products to the continuous settling tank F at the flow rate of 2L/h, wherein the volume of the continuous settling tank F is 3L, the settling residence time is 2h, and the temperature in the settling process is 65 +/-5 ℃. And (3) after the liquid level of the continuous settling tank F is full to the overflow port, conveying the materials to a filtering device G, wherein the temperature in the filtering process is 65 +/-5 ℃, simultaneously starting a third metering pump P-3 at the bottom of the continuous settling tank F, and returning the materials to the hydrogenation reaction kettle E at the flow rate of 0.5L/h.
The system keeps the balance of inlet and outlet, and the reaction is stopped after the continuous operation is carried out until the total amount of the injected p-nitroanisole is 50L. Because water is generated in the reaction process, and the catalyst also needs water, the purity of the product is 99.30 percent after dehydration treatment, the content is 99.18 percent, and the yield is 98.89 percent.
Example 2
Adding 10L of p-nitroanisole in a molten state into the p-nitroanisole storage tank A, keeping the temperature between 75 +/-5 ℃, keeping the temperature of the whole reaction system well, and continuously adding the p-nitroanisole in the molten state into the nitroanisole storage tank A in the reaction process so as to ensure that the reaction can be normally carried out.
And (3) starting a metering pump P-1 to pump the first part of the P-nitroanisole in the molten state into a hydrogenation reaction kettle E, wherein the volume of the first part of the P-nitroanisole in the molten state is 3L, and the volume of the hydrogenation reaction kettle E is 5L. And after the nitrogen replacement reaction system is qualified, adding 300g of Raney nickel metal catalyst into the hydrogenation reaction kettle E, replacing the reaction system with nitrogen again, replacing the reaction system with hydrogen, keeping the pressure at 1.5MPa and the temperature at 75 +/-5 ℃, and starting high-speed stirring under the temperature and pressure condition to perform hydrogenation reaction. Until the reaction system does not absorb hydrogen, the purity of the p-anisidine is 99.33 percent by sampling and detecting.
And (2) continuing to start the first metering pump P-1 and the second metering pump P-2, feeding a second part of molten P-nitroanisole in the P-nitroanisole storage tank A to the hydrogenation reactor E at a flow rate of 2.0L/h, supplementing the Raney nickel metal catalyst-water mixture in the catalyst pulping kettle D to the hydrogenation reactor E at a supplement amount of 0.8L/h (the mass concentration of the catalyst is 4%), keeping the temperature and the pressure of the hydrogenation reactor E unchanged, and keeping the retention time of the hydrogenation reaction about 1.47 h.
And (3) after the liquid level of the continuous settling tank F is full to an overflow port, conveying the material to a filtering device G, simultaneously starting a third metering pump P-3 at the bottom of the continuous settling tank F, and returning the material to the hydrogenation reaction kettle E at a flow rate of 0.6L/h, wherein the temperature in the filtering process is 75 +/-5 ℃.
The system keeps balance of inlet and outlet, and the reaction is stopped after the system is continuously operated until the total amount of the injected p-nitroanisole is 70L. The product after dehydration had a purity of 99.12%, a content of 99.15% and a yield of 98.71%.
Comparative example 1
Adding 300mL of methanol, 20g of Raney nickel metal catalyst and 250g of p-nitroanisole into a 1000mL hydrogenation reaction kettle, sealing the hydrogenation reaction kettle, replacing nitrogen for 5 times and hydrogen for 5 times, keeping the pressure of a reaction system at 1.5MPa, slowly heating to 60 +/-5 ℃, starting high-speed stirring, carrying out hydrogenation reaction, and keeping the temperature for half an hour after hydrogen is not absorbed. The material is filtered by a Raney nickel metal catalyst, methanol is separated, the purity is 98.90 percent, the content is 98.98 percent and the yield is 98.17 percent after water separation.
It should be noted that, although the technical solutions of the present invention are described by specific examples, those skilled in the art can understand that the present invention should not be limited thereto.
While various embodiments of the present invention have been described above, the above description is intended to be illustrative, not exhaustive, and not limited to the disclosed embodiments. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. The terminology used herein is chosen in order to best explain the principles of the embodiments, the practical application, or improvements made to the technology in the marketplace, or to enable others of ordinary skill in the art to understand the embodiments disclosed herein.
Claims (10)
1. An apparatus for preparing p-anisidine, comprising:
the hydrogenation reaction kettle is used for carrying out hydrogenation reaction; and
and the catalyst pulping kettle is connected with the inlet of the hydrogenation reaction kettle through a pipeline and is used for replenishing the catalyst in the hydrogenation reaction process.
2. The apparatus of claim 1, further comprising: and the storage tank is connected with the inlet of the hydrogenation reaction kettle through a pipeline.
3. The apparatus of claim 2, wherein the tank comprises at least one of a paranitroanisole tank, a hydrogen tank, and a nitrogen tank.
4. The apparatus of claim 3, further comprising:
a continuous settling tank comprising at least an inlet, a first outlet, and a second outlet; wherein the inlet of the continuous settling tank is connected with the outlet of the hydrogenation reaction kettle through a pipeline; the first outlet is positioned at the bottom of the continuous settling tank, and the first outlet is connected with the inlet of the hydrogenation reaction kettle through a pipeline.
5. The apparatus of claim 1 or 4, further comprising:
and the filtering device is connected with the outlet of the hydrogenation reaction kettle or the second outlet of the continuous settling tank and is used for separating to obtain a p-anisidine final product.
6. The apparatus of claim 4, wherein a sampling port is provided on the pipe between the inlet of the continuous settling tank and the outlet of the hydrogenation reactor.
7. The apparatus according to claim 3 or 4, wherein a first metering pump is arranged between the p-nitroanisole storage tank and the hydrogenation reaction kettle.
8. The apparatus according to claim 3, wherein a second metering pump is arranged on the pipeline between the catalyst pulping kettle and the hydrogenation reaction kettle.
9. The apparatus of claim 4, wherein a third metering pump is disposed on the pipeline between the first outlet of the continuous settling tank and the inlet of the hydrogenation reactor.
10. The apparatus according to claim 4, wherein a balance valve is arranged on the pipeline between the second outlet of the continuous settling tank and the inlet of the hydrogenation reaction kettle; and/or
Overflow valves are arranged on pipelines of the inlet of the continuous settling tank and the outlet of the hydrogenation reaction kettle; and/or
And an emptying pipeline connected with a second outlet of the continuous settling tank is also arranged on the continuous settling tank, and an emptying valve is arranged in the emptying pipeline to control the opening and closing of the emptying pipeline.
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| CN111559966A (en) * | 2020-06-16 | 2020-08-21 | 浙江闰土股份有限公司 | Preparation method of p-anisidine and equipment for preparing p-anisidine |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111559966A (en) * | 2020-06-16 | 2020-08-21 | 浙江闰土股份有限公司 | Preparation method of p-anisidine and equipment for preparing p-anisidine |
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