CN203187603U

CN203187603U - System for recycling butynediol low-pressure hydrogenation catalyst

Info

Publication number: CN203187603U
Application number: CN201320066687XU
Authority: CN
Inventors: 卢文新; 肖敦峰; 金沙杨; 赵国杰; 李雁; 肖晓愚; 徐建民; 夏吴
Original assignee: China Wuhuan Engineering Co Ltd
Current assignee: China Wuhuan Engineering Co Ltd
Priority date: 2013-02-05
Filing date: 2013-02-05
Publication date: 2013-09-11
Anticipated expiration: 2023-02-05

Abstract

The utility model relates to a system for recycling a butynediol low-pressure hydrogenation catalyst, and solves the problems that existing equipment for recycling the butynediol low-pressure hydrogenation catalyst is numerous, filtration efficiency is low, catalyst recycling efficiency is low, process period is long, energy consumption is high and running cost is high. The technical scheme is that the system comprises a serous fluid trough, a serous fluid pump and a hydrogenation reactor, wherein the serous fluid trough, the serous fluid pump and the hydrogenation reactor are sequentially connected through pipelines, and a gas-liquid separation tank, a condenser and a refining filter are also sequentially connected. A butynediol solution is subjected to hydrogenation reaction, flash evaporation, concentration and refining to obtain a 1,4-butanediol solution and recover a catalyst. The system provided by the utility model is simple in system, low in investment and running cost, capable of reducing the number of equipment needed for recycling the catalyst and efficiently recycling the butynediol low-pressure hydrogenation catalyst, and high in environment protection and economic values.

Description

Butynediol low-voltage hydrogenation catalyst recovery is utilized system

Technical field

The utility model relates to the synthetic preparation field of a kind of 1,4 butyleneglycol, and a kind of butynediol low-voltage hydrogenation catalyst recovery is utilized system specifically.

Background technology

1,4-butyleneglycol is a kind of important basic Organic Chemicals and fine chemical material, and is of many uses, and at present, 1, the 4 butyleneglycol production technique in the whole world mainly comprises alkynes aldehyde method, butadiene process, butane/cis-butenedioic anhydride method, propylene oxide/vinylcarbinol method.From the employed technology of worldwide production merchant, alkynes aldehyde method technology production capacity share accounts for bigger advantage.

The main raw material that alkynes aldehyde method (Reppe method) is produced 1,4-butyleneglycol has calcium carbide, methyl alcohol and hydrogen.Wherein, calcium carbide is mainly used to prepare acetylene, and methyl alcohol is used for preparing formaldehyde.Acetylene and formaldehyde prepare butynediol by ethynylation.Butynediol can prepare 1,4-butyleneglycol by low-voltage hydrogenation and high-pressure hydrogenation reaction process.

Because butynediol low-voltage hydrogenation process is carried out in gas, liquid, solid three phase slurry bed bioreactor, after reaction was finished, hydrogen, catalyzer and 1,4-butyleneglycol product solution needed to separate.In the traditional technology route, enter subsider from low pressure 1,4 butanediol solution of low-voltage hydrogenation reactor and the mixed serum of catalyzer, isolate the slurries that contain granules of catalyst.Granules of catalyst is deposited to the subsider bottom, with pump it is sent back to slurry tank then, squeezes into the low-voltage hydrogenation reactor more again by pump.1,4 butyleneglycol product overflows to the product groove by the weir on subsider top.Because subsider adopts the principle of gravity settling separation, only has separating effect for the granules of catalyst more than the 30 μ m, then be difficult to realize separating for short grained catalyzer, therefore by subsider top overflow 1, therefore still the catalyzer that contains more small particle size in the 4 butyleneglycol products must just can enter subsequent processing after removing granules of catalyst through further separating through heavy filtrations of a plurality of equipment such as electromagnetic filter, disk filter, fine filter I and fine filter II successively after the pump pressurization.

There is the problem that filter plant is numerous, filtration efficiency is low, catalyst recovery yield is low, process cycle is long, energy consumption is high, running cost is high in present technical process.

Summary of the invention

The purpose of this utility model is in order to solve the problems of the technologies described above, and provides that a kind of technology is simple, the cycle is short, energy consumption is low, catalyst recovery yield is high, facility investment and the low butynediol low-voltage hydrogenation catalyst recovery of running cost utilize system.

The utility model system comprises slurry tank, slush pump and the hydrogenator that connects successively through pipeline, also is connected with knockout drum, thickener and fine filter in turn.

Described thickener comprises slurries outlet and taphole, and described slurries outlet is connected with slurry tank through pipeline, and described taphole is connected with fine filter.

The processing method that adopts may further comprise the steps:

(1). the mixed serum of butyne diol solutions and catalyst slurry is sent in the hydrogenator through slush pump in the slurry tank, in hydrogenator, butynediol under catalyst action with H ₂Reaction generates 1,4 butyleneglycol, obtains containing 1,4 butanediol solution of catalyzer and hydrogen;

(2). 1, the 4 butyleneglycol product solution that contains catalyzer and hydrogen through hydrogenator generates at first enters knockout drum and flashes off the H that is dissolved in the liquid phase ₂, obtain containing 1,4 butanediol solution of catalyzer;

(3). 1,4 butanediol solution that contains catalyzer that obtains after the flash distillation enters thickener again and concentrates, through isolating catalyst slurry and 1,4 butanediol solution that contains the above granules of catalyst of 10 μ m behind the thickener;

(4). described 1,4 butanediol solution through isolated catalyst content≤15ppm behind the thickener is sent into subsequent processing after fine filter filters.

The catalyst slurry that described step (3) obtains is back to slurry tank to be mixed with butyne diol solutions and obtains mixed serum, enters the low-voltage hydrogenation reactor again through the slush pump pressurization again.

The catalyst content of controlling in 1,4 butanediol solution that contains catalyzer in the described step (2) after the flash distillation is 3-7wt%.

Controlling the catalyst content in the catalyst slurry described in the described step (3) is 9-12 wt %.

Control enters before the hydrogenator that the mass ratio of catalyzer and butynediol is 0.10-0.15 in the mixed serum, when going into operation, can be earlier with butyne diol solutions with send into back hydrogen reactor again after fresh catalyst slurry mixes in slurry tank, when system normally moves, then will directly be mixed with butyne diol solutions by the catalyst slurry that thickener draws back, in the operational process, detect in real time the content ratio of catalyzer and butynediol, to satisfy the requirement of follow-up hydrogenation reaction, when detect catalyzer contain quantity not sufficient the time, can replenish appropriate amount of catalysts in the slurry tank and get final product with the loss amount that remedies in the catalyst recovery process.

Described catalyzer is nickel-base catalyst commonly used in the butynediol hydrogenation reaction, can enumerate A-7063 type catalyzer that the Johnson mapphey company as Britain that do not limit produces etc., and described catalyst slurry comprises evenly outstanding catalyzer and the water that mixes.Described butyne diol solutions is from existing ethynylation unit.In the utility model, at hydrogenator reacted 1, contain hydrogen and catalyzer in 4 butanediol solutions, utilize knockout drum that the hydrogen flash distillation is come out earlier, and then by thickener to containing 1 of catalyzer, 4 butanediol solutions concentrate, the process of this concentration process gravity settling separation in the past, following advantage is arranged: (2) good separating effect, the catalyst slurry that can disposablely will contain the above granules of catalyst of 10 μ m is separated, by once concentration just can guarantee to obtain 1, catalyst content in 4 butanediol solutions is down to≤the 15ppm(mass percent), thereby follow-up need are once made with extra care the demand that just can satisfy subsequent processing of filtering in a fine filter, thereby the required various filter plants of follow-up multiple times of filtration have been significantly reduced, greatly reduce the investment of equipment and the energy consumption of bringing thus, shortened process cycle.(2) because enrichment step is low voltage operated, therefore the catalyst slurry that obtains can need not the pump pressurization, utilizes the pressure of self can be back to slurry tank, thereby has reduced the energy consumption of pump.(3) since most of catalyzer in thickener, be separated, thereby improved the rate of recovery of catalyzer greatly, reduce the loss of catalyzer, be conducive to further reduce running cost.

The utility model system is simple, and investment and running cost are low, have significantly reduced the required number of devices of catalyst recovery, have realized the high efficiente callback recycle of butynediol low-voltage hydrogenation catalyzer, have very high environmental protection and economic worth.

Description of drawings

Fig. 1 is the utility model system schematic and mechanical flow digram.

Wherein, 1-slurry tank, 2-slush pump, 3-low-voltage hydrogenation reactor, 4-flash drum, 5-thickener, the outlet of 5.1-slurries, 5.2-taphole, 6-fine filter.

Embodiment

System embodiment:

With reference to Fig. 1, slurry tank 1 is connected by pipeline successively through slush pump 2 and low-voltage hydrogenation reactor 3, knockout drum 4, thickener 5 and fine filter 6, wherein, described thickener comprises slurries outlet 5.1 and taphole 5.2, described slurries outlet 5.1 is connected with slurry tank 1 through pipeline, and described taphole 5.2 is connected with fine filter 6.

The process implementing example:

With reference to Fig. 1,

(1). the mixed serum (mass ratio of catalyzer and butynediol is 0.10-0.15 in the mixed serum) of butyne diol solutions and catalyst slurry is sent in the low-voltage hydrogenation reactor through slush pump 2 in the slurry tank 1, in low-voltage hydrogenation reactor 3 butynediol under catalyst action with H ₂Reaction generates 1,4 butyleneglycol, obtains containing 1,4 butanediol solution of catalyzer and hydrogen;

(2). 1, the 4 butyleneglycol product solution that contains catalyzer and hydrogen through hydrogenator 3 generates at first enters knockout drum 4 and flashes off the H that is dissolved in the liquid phase ₂, (catalyst content is 3-7wt%) to obtain containing 1,4 butanediol solution of catalyzer;

(3). what obtain after the flash distillation contains 1 of catalyzer, 4 butanediol solutions enter thickener 5 again and concentrate, through isolating catalyst slurry (catalyst content is 9-12 wt %) and 1,4 butanediol solution that contains the above granules of catalyst of 10 μ m behind the thickener;

(4). described 1,4 butanediol solution through the isolated catalyst content≤15ppm in thickener 5 backs is discharged to send into by taphole 5.2 and is sent into subsequent processing after fine filter 6 filters; Described step (3) obtains catalyst slurry and obtains mixed serum being back to slurry tank 1 in to mix with butyne diol solutions through slurries outlet 5.1 under the low pressure effect, and pressurizeing through slush pump 2 enters the low-voltage hydrogenation reactor again again.

Be example to produce 50000 ton of 1,4 butyleneglycol project per year, the application of the utility model system can be saved facility investment 2,600 ten thousand every year, 60,000 kwh/ that cut down the consumption of energy, and the above catalyzer of 10um obtains reclaiming substantially.

Claims

1. a butynediol low-voltage hydrogenation catalyst recovery is utilized system, comprises the slurry tank, slush pump and the hydrogenator that connect successively through pipeline, it is characterized in that, also is connected with knockout drum, thickener and fine filter in turn.

2. butynediol low-voltage hydrogenation catalyst recovery as claimed in claim 1 is utilized system, it is characterized in that, described thickener comprises slurries outlet and taphole, and described slurries outlet is connected with slurry tank through pipeline, and described taphole is connected with fine filter.