CN111111888A - Production device of m/p-phthaloyl chloride of air milling raw material - Google Patents

Production device of m/p-phthaloyl chloride of air milling raw material Download PDF

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Publication number
CN111111888A
CN111111888A CN201911384318.3A CN201911384318A CN111111888A CN 111111888 A CN111111888 A CN 111111888A CN 201911384318 A CN201911384318 A CN 201911384318A CN 111111888 A CN111111888 A CN 111111888A
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China
Prior art keywords
pipeline
reaction
communicated
condenser
cyclone separator
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CN201911384318.3A
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Chinese (zh)
Inventor
刘嵩
张泰铭
张良
孙丰炜
张聪聪
孙丰春
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Shandong Kaisheng New Materials Co Ltd
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Shandong Kaisheng New Materials Co Ltd
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Priority to CN201911384318.3A priority Critical patent/CN111111888A/en
Publication of CN111111888A publication Critical patent/CN111111888A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C19/00Other disintegrating devices or methods
    • B02C19/06Jet mills
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C23/00Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C23/00Auxiliary methods or auxiliary devices or accessories specially adapted for crushing or disintegrating not provided for in preceding groups or not specially adapted to apparatus covered by a single preceding group
    • B02C23/18Adding fluid, other than for crushing or disintegrating by fluid energy
    • B02C23/20Adding fluid, other than for crushing or disintegrating by fluid energy after crushing or disintegrating

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  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention relates to a production device of m/p-phthaloyl chloride of an air grinding raw material, belonging to the technical field of chemical synthesis production equipment. The invention solves the problem of the prior m-paraphthaloyl chloride. The invention comprises an airflow mill for airflow grinding solid m/terephthalic acid, wherein an airflow inlet pipeline is arranged on one side of the airflow mill, and an m/terephthalic acid passing feed pipeline is arranged at the top of the airflow mill; the primary cyclone separator is used for separating gas and m/p-phthalic acid powder, the primary cyclone separator is communicated with the output end of the airflow grinding machine through a pipeline, and the discharge end of the primary cyclone separator is connected with the superfine powder intermediate tank through a pipeline.

Description

Production device of m/p-phthaloyl chloride of air milling raw material
Technical Field
The invention relates to a production device of m/p-phthaloyl chloride of an air grinding raw material, belonging to the technical field of chemical synthesis production equipment.
Background
M/P-phthaloyl chloride, also known as terephthaloyl dichloride, TPC or TCL for short, is an important fine chemical product, is mainly used as a polymeric monomer of poly (p-phenylene terephthalamide) (aramid 1414 or PPTA for short) and polysulfonamide, and has certain application in synthesis of permeable membrane materials, high polymer materials and pesticides. Due to the excellent characteristics of aramid 1414, the aramid 1414 has a wide application field and is a new material which is emphasized and developed in China. The quality of the paraphthaloyl chloride serving as one of the important raw materials of the aramid fiber 1414 is directly related to the product performance of the downstream aramid fiber 1414, and along with the rapid development of the aramid fiber industry in China, the demand of the paraphthaloyl chloride is rapidly increased, and meanwhile, higher requirements are provided for the quality of the paraphthaloyl chloride.
The existing production device has long reaction time, and reaction tail gas cannot be discharged out of a system in time, so that the production rate of a reaction process is restricted; meanwhile, the raw materials of the reaction, i.e. the m-terephthalic acid and the terephthalic acid, have larger particles, so that the reaction speed is influenced.
Disclosure of Invention
The invention aims to overcome the defects of the existing m/p-phthaloyl chloride production device, and provides the m/p-phthaloyl chloride production device for the raw material of the air mill.
The invention is realized by adopting the following technical scheme:
a production device of m/p-phthaloyl chloride of an air grinding raw material comprises:
the jet mill is used for carrying out jet milling on solid m/terephthalic acid, a gas flow inlet pipeline is arranged at one side of the jet mill, and an m/terephthalic acid passing feed pipeline is arranged at the top of the jet mill;
the primary cyclone separator is used for separating gas and m/p-phthalic acid powder, the primary cyclone separator is communicated with the output end of the airflow mill through a pipeline, and the discharge end of the primary cyclone separator is connected with an ultrafine powder intermediate tank through a pipeline;
the reaction kettle is used for reacting the m/terephthalic acid and the thionyl chloride, the reaction kettle is communicated with the superfine powder intermediate tank, and a thionyl chloride feeding pipeline and a catalyst feeding pipeline are arranged at the upper part of the reaction kettle;
the gas phase separation mechanism is used for extracting gas phase generated in the reaction kettle and comprises a thionyl chloride recovery mechanism and a gas phase evacuation driving device, and one end of the gas phase evacuation driving device is transferred to the tail gas treatment mechanism through a tail gas absorption pipeline;
the thionyl chloride recovery mechanism is communicated with the reaction kettle through a gas phase lifting pipe, the gas phase lifting pipe is communicated with a condenser, the condenser is communicated to the reaction kettle through a liquid phase return pipe, and the condenser is communicated with a gas phase evacuation driving device through a tail gas pipeline.
Preferably, the condenser comprises a reaction first-stage condenser and a reaction second-stage condenser which are connected in series, the reaction first-stage condenser and the reaction second-stage condenser are both communicated to the reaction kettle through a liquid phase return pipe, and the reaction second-stage condenser is communicated to the gas phase evacuation driving device through a tail gas pipeline.
Preferably, the gas phase evacuation driving device comprises a thionyl chloride tank, the bottom of the thionyl chloride tank is communicated to an ejector through a circulating pipeline, the ejector is communicated with the tail gas pipeline, and the circulating pipeline is connected with a circulating pump.
Preferably, the rear end of the primary cyclone separator is connected with a secondary cyclone separator in series, and the top air outlet end of the secondary cyclone separator is connected to a gas dust removal device through a dust removal pipeline.
The invention has the beneficial effects that:
(1) the production device of the m/p-phthaloyl chloride of the air-milling raw material is provided with the air-flow mill, the m/p-phthalic acid is subjected to air-flow grinding through the air-flow mill, and the grinded m/p-phthalic acid can reach 40-50 micrometers, so that the m/p-phthalic acid can better react with thionyl chloride, the reaction is more sufficient, and the reaction speed is higher;
(2) the production device of the meta/terephthaloyl chloride of the raw material of the air mill is provided with the gas phase evacuation driving device, so that power is provided for the gas phase after reaction, tail gas after reaction is discharged in time, and the production efficiency of the reaction is further improved.
Drawings
FIG. 1 is a block diagram of an embodiment of the present invention;
in the figure: 1. the method comprises the following steps that (1) m/terephthalic acid enters a pipeline through a feeding pipeline (2) and an airflow inlet pipeline (3), an airflow mill (4), a primary cyclone separator (5) and a secondary cyclone separator (5); 6. the system comprises a dust removal pipeline, a 7 ultrafine powder intermediate tank, 8 a reaction kettle, 9 a thionyl chloride feeding pipeline, 10 a gas phase lifting pipe, 11 a reaction primary condenser, 12 a reaction secondary condenser, 13 a liquid phase return pipe, 14 a tail gas pipeline, 15 an ejector, 16 a thionyl chloride tank, 17 a circulating pump, 18 a tail gas absorption pipeline, 19 and a catalyst feeding pipeline.
Detailed Description
The invention will be further explained with reference to the drawings.
As shown in fig. 1, the apparatus for producing m/p-phthaloyl chloride as a raw material for gas milling according to the present invention comprises:
the jet mill 3 is used for carrying out jet milling on solid isophthalic acid, a gas flow inlet pipeline 2 is arranged on one side of the jet mill 3, and the top of the jet mill 3 is provided with an isophthalic acid passing feed pipeline 1;
the primary cyclone separator 4 is used for separating gas and m/p-phthalic acid powder, the primary cyclone separator 4 is communicated with the output end of the jet mill 3 through a pipeline, and the discharge end of the primary cyclone separator 4 is connected with an ultrafine powder intermediate tank 7 through a pipeline;
a reaction kettle 8 for reacting the m/p-phthalic acid and the thionyl chloride, wherein the reaction kettle 8 is communicated with the superfine powder intermediate tank 7, and the upper part of the reaction kettle 8 is provided with a thionyl chloride feeding pipeline 9 and a catalyst feeding pipeline 20;
the gas phase separation mechanism is used for extracting and separating gas phase generated in the reaction kettle 8 and comprises a thionyl chloride recovery mechanism and a gas phase evacuation driving device, and one end of the gas phase evacuation driving device is transferred to the tail gas treatment mechanism through a tail gas absorption pipeline 18;
the thionyl chloride recovery mechanism is communicated with the reaction kettle 8 through a gas phase lifting pipe 10, the gas phase lifting pipe 10 is communicated with a condenser, the condenser is communicated with the reaction kettle 8 through a liquid phase return pipe 13, and the condenser is communicated with a gas phase evacuation driving device through a tail gas pipeline 14.
The condenser include the reaction first order condenser 11 and the reaction second order condenser 12 that concatenate, reaction first order condenser 11 and reaction second order condenser 12 all communicate to reation kettle 8 through liquid phase back flow 13 on, reaction second order condenser 12 communicates to the gaseous phase through tail gas pipeline 14 and evacuates on the drive arrangement.
The gas phase evacuation driving device comprises a thionyl chloride tank 16, the bottom of the thionyl chloride tank 16 is communicated to an ejector 15 through a circulating pipeline, the ejector 15 is communicated with the tail gas pipeline 14, and the circulating pipeline is connected with a circulating pump 17.
The rear end of the primary cyclone separator 4 is connected with a secondary cyclone separator 5 in series, and the top air outlet end of the secondary cyclone separator 5 is connected to a gas dust removing device through a dust removing pipeline 6.
The working process of the invention is as follows:
the m/p-phthalic acid enters an airflow mill 3 through a feeding pipeline 1, the materials collide with each other under the driving of airflow, so that the particle size of the m/p-phthalic acid is reduced, the m/p-phthalic acid is separated by a primary cyclone separator 4 and a secondary cyclone separator 5, a gas phase is connected to a gas dust removal device through a dust removal pipeline 6, and the ultrafine powder enters an ultrafine powder intermediate tank 7 for temporary storage; powder is put into a reaction kettle 8 and enters the reaction kettle 8 through a thionyl chloride feed line 9, gas in the reaction process is led out through a gas phase lifting pipe 10, passes through a reaction primary condenser 11 and a reaction secondary condenser 12, thionyl chloride in the gas is condensed into a liquid phase, and flows back to the reaction kettle 8 through a liquid phase return pipe 13 to continue to react, the gas phase reaches a tail gas line 14, the gas phase is rapidly separated out of the reaction kettle 8 through a gas phase evacuation driving device (composed of an ejector 15, a thionyl chloride tank 16 and a circulating pump 17), the reaction is carried out in the forward direction, and then the gas phase is removed from an absorption pipeline 18 through a tail gas treatment device.
The comparison with the original production directly using the m/p-phthalic acid raw material without air stream grinding is as follows:
TABLE 1 comparison of M/P-phthaloyl chloride
Figure BDA0002343144740000031
As can be seen from the table above, the reaction time of the prior art is 2/3 of the original production process, which takes less time than 10 hours, so the production speed is greatly improved, the impurities of the intermediate/terephthaloyl chloride content of the produced product are correspondingly less, and the content of the intermediate/terephthaloyl chloride in the produced product is also improved.
The invention is mainly applied to the places where the m/p-phthaloyl chloride is produced.
Of course, the foregoing is only a preferred embodiment of the invention and should not be taken as limiting the scope of the embodiments of the invention. The present invention is not limited to the above examples, and equivalent changes and modifications made by those skilled in the art within the spirit and scope of the present invention should be construed as being included in the scope of the present invention.

Claims (4)

1. A production device of m/p-phthaloyl chloride of an air grinding raw material is characterized by comprising the following components:
the jet mill (3) is used for carrying out jet milling on solid m/terephthalic acid, a gas flow inlet pipeline (2) is arranged at one side of the jet mill (3), and an m/terephthalic acid passing feeding pipeline (1) is arranged at the top of the jet mill (3);
the primary cyclone separator (4) is used for separating gas and m/p-phthalic acid powder, the primary cyclone separator (4) is communicated with the output end of the airflow mill (3) through a pipeline, and the discharge end of the primary cyclone separator (4) is connected with an ultrafine powder intermediate tank (7) through a pipeline;
a reaction kettle (8) for the reaction of the m/terephthalic acid and the thionyl chloride, wherein the reaction kettle (8) is communicated with the superfine powder intermediate tank (7), and the upper part of the reaction kettle (8) is provided with a thionyl chloride feeding pipeline (9) and a catalyst feeding pipeline (19);
the gas phase separation mechanism is used for extracting and separating gas phase generated in the reaction kettle (8), and comprises a thionyl chloride recovery mechanism and a gas phase evacuation driving device, wherein one end of the gas phase evacuation driving device is transferred to the tail gas treatment mechanism through a tail gas absorption pipeline (18);
the thionyl chloride recovery mechanism is communicated with a reaction kettle (8) through a gas phase lifting pipe (10), the gas phase lifting pipe (10) is communicated with a condenser, the condenser is communicated to the reaction kettle (8) through a liquid phase return pipe (13), and the condenser is communicated with a gas phase evacuation driving device through a tail gas pipeline (14).
2. The apparatus for producing m/p-phthaloyl chloride as a raw material for an air mill according to claim 1, characterized in that: the condenser including reaction one-level condenser (11) and reaction secondary condenser (12) that concatenate, reaction one-level condenser (11) and reaction secondary condenser (12) all communicate on reation kettle (8) through liquid phase back flow (13), reaction secondary condenser (12) communicate on the gaseous phase drive arrangement that evacuates through exhaust line (14).
3. The apparatus for producing m/p-phthaloyl chloride as a raw material for an air mill according to claim 2, characterized in that: the gas phase evacuation driving device comprises a thionyl chloride tank (16), the bottom of the thionyl chloride tank (16) is communicated to an ejector (15) through a circulating pipeline, the ejector (15) is communicated with the tail gas pipeline (14), and the circulating pipeline is connected with a circulating pump (17).
4. The apparatus for producing m/p-phthaloyl chloride as a raw material for an air mill according to claim 3, characterized in that: the rear end of the primary cyclone separator (4) is connected with a secondary cyclone separator (5) in series, and the top air outlet end of the secondary cyclone separator (5) is connected to a gas dust removal device through a dust removal pipeline (6).
CN201911384318.3A 2019-12-28 2019-12-28 Production device of m/p-phthaloyl chloride of air milling raw material Withdrawn CN111111888A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112844717A (en) * 2020-12-23 2021-05-28 赣州博立科技有限公司 Full-automatic vertical airflow mill equipment for grinding and grading metal powder by utilizing airflow

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112844717A (en) * 2020-12-23 2021-05-28 赣州博立科技有限公司 Full-automatic vertical airflow mill equipment for grinding and grading metal powder by utilizing airflow

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