CN201746485U - Apparatus of preparing m-phenol diamine by continuous hydrolysis of metaphenylene diamine - Google Patents

Apparatus of preparing m-phenol diamine by continuous hydrolysis of metaphenylene diamine Download PDF

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Publication number
CN201746485U
CN201746485U CN2009202956067U CN200920295606U CN201746485U CN 201746485 U CN201746485 U CN 201746485U CN 2009202956067 U CN2009202956067 U CN 2009202956067U CN 200920295606 U CN200920295606 U CN 200920295606U CN 201746485 U CN201746485 U CN 201746485U
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China
Prior art keywords
hydrolysis
mphenylenediamine
tower reactor
resorcinol
line mixer
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Expired - Lifetime
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CN2009202956067U
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Chinese (zh)
Inventor
何旭斌
王新武
陶建国
孟明
朱敬鑫
张桂香
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SHANGHAI HONGYUAN XINCHUANG MATERIAL TECHNOLOGY CO., LTD.
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ZHEJIANG HONGSHENG CHEMICAL RESEARCH Ltd
ZHEJIANG LONGSHENG CHEMICALS CO Ltd
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Abstract

Disclosed is an apparatus of preparing m-phenol diamine by continuous hydrolysis of metaphenylene diamine, which comprises a pipeline mixer for preparing metaphenylene diamine hydrolysis materials, a heat exchanger for heating mixing raw materials, and a tower reactor for performing hydrolysis reaction, an outlet of the pipeline mixer is communicated with a raw material inlet of the heat exchanger, a raw material outlet of the heat exchanger is communicated with a hydrolysis raw material inlet of the tower reactor, baffle boards are arranged in the tower reactor from top to bottom, and a heating coil is arranged on the outer wall of the tower reactor. The utility model has advantages of high efficiency, short production period, high product yield, stable product quality, and simple process control, and effectively reduces the equipment investment.

Description

The mphenylenediamine continuous hydrolysis prepares the device of Resorcinol
Technical field
The utility model belongs to the preparation facilities of Resorcinol.
Background technology
Resorcinol (Resorcinol) is commonly called as resorcinol, have another name called 1,3-dihydroxy-benzene etc., it is a kind of important Organic Chemicals, be widely used in fields such as agricultural chemicals, dyestuff, coating, medicine, plastics, rubber, electronic chemical product, wherein be mainly used in the soaker used of preparation tyre cord, use for synthetic rubber tacky resin, wood gluing plate hight performance tackiness agent, synthetic benzophenone UV light absorber, Metha Amino Phenon etc.
It is the sulfonated alkali fusion method of raw material that the route of the synthetic Resorcinol of industrialization at present mainly contains with benzene, be the oxidation style and the mphenylenediamine hydrolysis method of raw material with the m-Diisopropylbenzene.Domestic main employing is the sulfonated alkali fusion method of raw material with benzene, owing to technology and equipment reason, has the technology barrier that is difficult to overcome aspect production cost and the environment protection treating improving.The mphenylenediamine hydrolysis process presents good prospects for application because of raw material sources facility, technical process weak point, good environmental protection, and corresponding, the High Temperature High Pressure of hydrolysis reaction and acidic medium operating mode have proposed higher requirement to the reactor material erosion resistance.
Reactor intermittent hydrolysis flow process is adopted in mphenylenediamine hydrolysis at present more, because there is certain coefficient in reactor, the input and output material of intermittent hydrolysis flow process, material heating and cooling non-cutting times is long etc., production efficiency of equipment is low, make the reaction volume that the batch reactor requirements of process is bigger, single complete equipment production capacity is very low.The heating and cooling of intermittent process material periodically hocket, and energy can't rationally be utilized, and energy consumption is bigger.The equipment that Resorcinol is produced in the mphenylenediamine hydrolysis generally adopts nonferrous materials manufacturings such as zirconium, tantalum, and the relevant device cost is higher, causes the whole investment of device excessive, considers from the technology macroeconomic, and heavy industrialization is lacked competitiveness.
In addition tank reactor since temperature of reaction and pressure height, reaction medium to the particular requirement of stirring rake solidity to corrosion and sealing property, the investment increase of agitator is more.Rhythmic reaction is not with under the condition of stirring at reactor, relies on the heating of outer wall coil pipe will cause material in reactor to have bigger thermograde, and the control of hydrolysis reaction processing condition (mainly being temperature) is all had adverse influence.
For improving Resorcinol yield and production efficiency of equipment, CN200710019561B has proposed a kind of method of preparing resorcinol by continuous hydrolyzing metaphenylene diamine, this patent adopts the placed in-line hydrolysis process of many stills, adopt three hydrolysis kettles, a rewinding still among the embodiment, the highly pressured hydrolysis still is made by Monel metal or tantalum material or zirconium material.Reaction mass mphenylenediamine sulfate liquor is intermittently batching, adding continuously in batches, reaction product is taken out continuously, has avoided batch reactor loading and unloading material supervisor, has improved the utilization coefficient of equipment, compare production capacity with interrupter method and improve 1~2 times, reduced facility investment relatively.But obviously, there is serious backmixing in material in the still formula hydrolysis reactor: during the tank reactor operate continuously, and the material diffusion of moving from top to bottom, the interior mixing of materials of raw material that the concentration of adding is higher and pot, the natural convection that the severe difference of one side different components causes all can produce backmixing; On the other hand, because liquid-flow form difference in the reactor, if do not dispose stirring rake, mixing of materials and inhomogeneous in the still, partial material residence time in reactor is longer.Although adopt a plurality of reactor serial operations, the degree that has suppressed backmixing relatively, but the transformation efficiency of per unit reactor volume reactant is this minimum in flow reactor shortcoming still can't be avoided, therefore, be inevitable in order to obtain the bigger reactor of high conversion employing or to increase reactor progression.In addition, owing to there is the material back-mixing, partial material residence time in reactor is very long, causes the increase of side reaction product amount easily.
The preparation of mphenylenediamine hydrolysis material also is the important step of this device.Because the mphenylenediamine storage process very easily decomposes, and influences the yield and the quality product of follow-up hydrolysis.The technology of now having reported all adopts the mechanical agitation type mixing tank intermittently to prepare the technology of mphenylenediamine sulfate solution, adopts stirring tank to divide two step configuration dilute sulphuric acid and mphenylenediamine sulfate solutions as CN200710019561B.There is the mixing region ununiformity in the mechanical agitation type mixing tank, and is even in order to make two kinds or multiple liquid material thorough mixing in the shortest time, must strengthen mixture strength, and mixture strength increases and certainly will cause outside input energy consumption too high.Intermittently batching is used for ensureing subsequent handling, need dispose the dosing unit and the storage vessel of two cover dosing units or a cover comparatively large vol simultaneously, and this all can cause the hydrolysis material storage time long, and raw material decomposes to be increased, and has reduced reaction yield and quality product.
Summary of the invention
Produce in order to overcome existing mphenylenediamine hydrolysis that the plant efficiency of Resorcinol is lower, the production cycle is long, product yield is low, unstable product quality, technology controlling and process complexity, the higher deficiency of facility investment, the mphenylenediamine continuous hydrolysis that the utility model provides that a kind of plant efficiency is higher, with short production cycle, product yield is higher, constant product quality, technology controlling and process are easy, reduce facility investment effectively prepares the device of Resorcinol.
The technical scheme that its technical problem that solves the utility model adopts is:
A kind of mphenylenediamine continuous hydrolysis prepares the device of Resorcinol, comprise the line mixer in order to preparation mphenylenediamine hydrolysis material, interchanger and tower reactor in order to be hydrolyzed and to react in order to mixing raw material is heated, the outlet of described line mixer is communicated with the material inlet of described interchanger, the material outlet of described interchanger is communicated with the hydrolysis material import of described tower reactor, arrange traverse baffle in the described tower reactor from top to bottom, the outer wall of described tower reactor has heating coil.
Further, described device also comprises the metering topping-up pump, and described metering topping-up pump is installed on the pipeline that the import of described line mixer is connected.
Described device also comprises topping-up pump, and under meter and variable valve is installed on the pipeline that the import of described line mixer is connected.
Mphenylenediamine sulfate solution process for preparation adopts the metering topping-up pump to carry or common topping-up pump+flow metering+valve control.
Further again, described interchanger is a tube and shell heat exchanger, and heating medium adopts thermal oil.Certainly, also can select the interchanger of other types, as long as mixing raw material is heated to the temperature of setting.
The length of described traverse baffle is littler than the inner chamber width of described tower reactor, and adjacent traverse baffle up and down is installed in the both sides of tower reactor respectively.
Described line mixer inside is provided with mixed cell, mixed cell is flight, petal plate, waved plate or grizzly bar, have choked flow, mixing functions, liquid is flowed produce when passing through mixed cell shunting, intersection mixing and reverse eddy flow etc., two strands of liquid disperse to be mixed with each other the material thorough mixing when flowing in mixer tube with certain flow velocity simultaneously separately.
Described line mixer is the compact cascade type mixing tank, and described compact cascade type mixing tank comprises one-level mixing tank and secondary mixing tank, and the outlet of described one-level mixing tank connects the inlet of described secondary mixing tank.
Technical conceive of the present utility model is: the technology of producing resorcinol by continuously hydrolyzing m-phenylenediamine, the preparation process, hydrolyzing process and the postprocessing working procedures that comprise hydrolysis material mphenylenediamine vitriol, the preparation process that it is characterized in that hydrolysis material adopts the continuous blended mode of two-stage pipeline, and the hydrolysis material prepares and promptly enters hydrolysis reaction; Hydrolyzing process adopts the mode of tower reactor continuous hydrolysis to carry out, and reduces the material back mixing, improves product yield and plant efficiency.May further comprise the steps: 1. desired raw material sulfuric acid, water, mphenylenediamine are pumped up respectively, after measuring by under meter (or volume pump), directly enter the line mixer batching, prepare the aqueous solution of dilute sulphuric acid, mphenylenediamine vitriol continuously by line mixer, form the aqueous solution of uniform mphenylenediamine vitriol; 2. the hydrolysis material for preparing is by interchanger, joins hydrolytic reaction pot with behind thermal oil indirect heating to 230~250 ℃; 3. hydrolysis reactor adopts the tower reactor of a band traverse baffle, reactor outer wall belt coil pipe, with heat-conducting oil heating keeping temperature of reaction, hydrolysate continuous extraction of discharge port at the bottom of the tower.4. the hydrolysis material obtains the Resorcinol product through operations such as follow-up cooling, extraction, rectifying.
The utility model adopts online line mixer can finish effective mixing moment, solves the decomposition spoilage problems of still formula batching material storage process.Adopt line-blending, in whole mixing process, the composition of very fast definite mixture, and it is remained on any numerical value of adjusting in advance, like this, not only increased operational handiness, by the flow of parallel control mixture, the concentration of fluid on whole cross section is continuously and equilibrated not only is easy to accomplish to mix, reduce energy consumption, and can effectively control device.
The tower hydrolysis reactor that the utility model adopts is by being provided with traverse baffle, material along column plate radially flow velocity improve relatively, strengthen the homogeneity of Flow of Goods and Materials, reduce the material back-mixing; Uniformity of temperature profile in the tower, hydrolysising reacting temperature rely on the preheating temperature of preheater material to control, and more help accurate, the stable control of temperature of reaction.Above-mentioned measure all helps reducing side reaction and takes place, and improves reaction yield and quality product.
The beneficial effects of the utility model mainly show: plant efficiency is higher, with short production cycle, product yield is higher, constant product quality, technology controlling and process are easy, reduced facility investment effectively.
Description of drawings
Fig. 1 is the schematic diagram that the mphenylenediamine continuous hydrolysis prepares the device of Resorcinol.
Fig. 2 is the structural representation of line mixer, wherein, and 1 import of a-material, 2 imports of b-material, the outlet of c-mixture.
Fig. 3 is the structural representation of tower hydrolysis reactor, wherein, and a-hydrolysis material import b-hydrolysis material outlet c-drain d-relief valve connection e-heating coil.
Embodiment
Below in conjunction with accompanying drawing the utility model is further described.
With reference to Fig. 1~Fig. 3, a kind of mphenylenediamine continuous hydrolysis prepares the device of Resorcinol, comprise the line mixer 1 in order to preparation mphenylenediamine hydrolysis material, interchanger 2 and tower reactor 3 in order to be hydrolyzed and to react in order to mixing raw material is heated, the outlet of described line mixer 1 is communicated with the material inlet of described interchanger 2, the material outlet of described interchanger 2 is communicated with the hydrolysis material import of described tower reactor 3, arrange traverse baffle 4 from top to bottom in the described tower reactor 3, the outer wall of described tower reactor 3 has heating coil.
Described device also comprises metering topping-up pump 5, with the described metering topping-up pump 5 of installation on the pipeline that the import of described line mixer is connected.
Described device also comprises topping-up pump 5, and under meter and variable valve is installed on the pipeline that the import of described line mixer is connected.
The mphenylenediamine sulfate solution process for preparation of present embodiment adopts the metering topping-up pump to carry or common topping-up pump+flow metering+valve control.
Described interchanger 2 is a tube and shell heat exchanger, and heating medium adopts thermal oil or steam.Certainly, also can select the interchanger of other types.
The length of described traverse baffle 4 is littler than the inner chamber width of described tower reactor, and adjacent traverse baffle up and down is installed in the both sides of tower reactor respectively.
Comprise mixed cell 5 in the described line mixer, mixed cell 5 is flight, petal, waved plate or grizzly bar, have choked flow, mixing effect, liquid is flowed produce when passing through mixed cell shunting, intersection mixing and reverse eddy flow etc., two strands of liquid disperse to be mixed with each other the material thorough mixing when flowing in mixer tube with certain flow velocity simultaneously separately.
Described line mixer 1 is the compact cascade type mixing tank, and described compact cascade type mixing tank comprises one-level mixing tank and secondary mixing tank, and the outlet of described one-level mixing tank connects the inlet of described secondary mixing tank.
With reference to accompanying drawing 1, the one-level mixing tank has two imports, and one is the import of water, and it two is 98% vitriolic import, and the secondary mixing tank also has two imports, and one is communicated with the one-level mixer outlet, and it two is the import of mphenylenediamine; On the pipeline of the import of water, 98% sulfuric acid and three kinds of raw materials of mphenylenediamine, can simultaneously the positive battery metering pump be set directly, common topping-up pump+flow metering+valve control perhaps is set simultaneously; Certainly, also can select on the pipeline of import of a certain or two kinds of raw materials the positive battery metering pump to be set, common topping-up pump+flow metering+valve control is set on the pipeline of the import of raw material in addition.
The working process of present embodiment is: 1. desired raw material sulfuric acid, water, mphenylenediamine are pumped up respectively, after measuring by under meter (or volume pump), directly enter the line mixer batching, prepare the aqueous solution of uniform mphenylenediamine vitriol by line mixer continuously; 2. the mixing raw material for preparing is by interchanger, joins hydrolytic reaction pot with behind thermal oil indirect heating to 230~250 ℃; 3. hydrolysis reactor adopts the tower reactor of a band traverse baffle, reactor outer wall belt coil pipe, with heat-conducting oil heating keeping temperature of reaction, hydrolysate continuous extraction of discharge port at the bottom of the tower.4. the hydrolysis material obtains the Resorcinol product through operations such as follow-up cooling, extraction, rectifying.

Claims (7)

1. a mphenylenediamine continuous hydrolysis prepares the device of Resorcinol, it is characterized in that: described device comprises in order to the line mixer of preparation mphenylenediamine hydrolysis material, in order to interchanger and the tower reactor in order to be hydrolyzed and to react with the mixing raw material heating, the outlet of described line mixer is communicated with the material inlet of described interchanger, the material outlet of described interchanger is communicated with the hydrolysis material import of described tower reactor, arrange traverse baffle in the described tower reactor from top to bottom, the outer wall of described tower reactor has heating coil.
2. mphenylenediamine continuous hydrolysis as claimed in claim 1 prepares the device of Resorcinol, it is characterized in that: described device also comprises the metering topping-up pump, and described metering topping-up pump is installed on the pipeline that the import of described line mixer is connected.
3. mphenylenediamine continuous hydrolysis as claimed in claim 1 prepares the device of Resorcinol, it is characterized in that: described device also comprises topping-up pump, and under meter and variable valve is installed on the pipeline that the import of described line mixer is connected.
4. prepare the device of Resorcinol as the described mphenylenediamine continuous hydrolysis of one of claim 1-3, it is characterized in that: described interchanger is a tube and shell heat exchanger.
5. the device for preparing Resorcinol as the described mphenylenediamine continuous hydrolysis of one of claim 1-3, it is characterized in that: the length of described traverse baffle is littler than the inner chamber width of described tower reactor, and adjacent traverse baffle up and down is installed in the both sides of tower reactor respectively.
6. prepare the device of Resorcinol as the described mphenylenediamine continuous hydrolysis of one of claim 1-3, it is characterized in that: described line mixer comprises mixed cell, and described mixed cell is flight, petal plate, waved plate or grizzly bar.
7. described mphenylenediamine continuous hydrolysis as claimed in claim 6 prepares the device of Resorcinol, it is characterized in that: described line mixer is the compact cascade type mixing tank, described compact cascade type mixing tank comprises one-level mixing tank and secondary mixing tank, and the outlet of described one-level mixing tank connects the inlet of described secondary mixing tank.
CN2009202956067U 2009-12-31 2009-12-31 Apparatus of preparing m-phenol diamine by continuous hydrolysis of metaphenylene diamine Expired - Lifetime CN201746485U (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106693857A (en) * 2015-07-20 2017-05-24 浙江迪邦化工有限公司 Integrated reactor
CN108043259A (en) * 2017-12-27 2018-05-18 山东高成石油科技有限公司 A kind of in-line blending equipment
CN114307900A (en) * 2021-12-30 2022-04-12 江苏三吉利化工股份有限公司 Multistage combined reaction device for synthesizing benzenediol by phenol hydroxylation

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106693857A (en) * 2015-07-20 2017-05-24 浙江迪邦化工有限公司 Integrated reactor
CN106693857B (en) * 2015-07-20 2018-10-26 浙江迪邦化工有限公司 Integral reactor
CN108043259A (en) * 2017-12-27 2018-05-18 山东高成石油科技有限公司 A kind of in-line blending equipment
CN114307900A (en) * 2021-12-30 2022-04-12 江苏三吉利化工股份有限公司 Multistage combined reaction device for synthesizing benzenediol by phenol hydroxylation

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Effective date of registration: 20170825

Address after: 312369 weft three road, Shangyu Industrial Park, Hangzhou Bay, Zhejiang, Shaoxing

Co-patentee after: SHANGHAI HONGYUAN XINCHUANG MATERIAL TECHNOLOGY CO., LTD.

Patentee after: Zhejiang Hongsheng Chemical Research Limited

Co-patentee after: Zhejiang Longsheng Chemicals Co., Ltd.

Address before: 312369, No. three, No. 15, Shangyu Industrial Park, Hangzhou Bay, Zhejiang, Shangyu

Co-patentee before: Zhejiang Hongsheng Chemical Research Limited

Patentee before: Zhejiang Longsheng Chemicals Co., Ltd.

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CX01 Expiry of patent term

Granted publication date: 20110216