CN102731289B - Thickening process of coarse adipic acid - Google Patents
Thickening process of coarse adipic acid Download PDFInfo
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- CN102731289B CN102731289B CN201210247210.1A CN201210247210A CN102731289B CN 102731289 B CN102731289 B CN 102731289B CN 201210247210 A CN201210247210 A CN 201210247210A CN 102731289 B CN102731289 B CN 102731289B
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Abstract
The invention provides a thickening process of coarse adipic acid. In the thickening process, a static bundling-type thickener is used. The thickener consists of a thickener shell side and a thickener tube side; a candlewick-type filter element is used; and a filter tube of the thickener tube side is provided with a plurality of filter elements. The time sequence automatic control procedure is adopted in the whole operation process, comprises the steps of feeding, online cleaning of filter cloth, re-feeding, pre-filtering, filtering, draining feed liquid, exhausting air and removing filter cakes, wherein the whole filtering process lasts for 12-20 minutes, preferably 14 minutes. The thickening process of coarse adipic acid solves the problems of high fault rate, poor production continuity and limited capacity of the conventional thickener. By the thickening process, the operation period is short, the fault rate of equipment is low, the continuous operation period of a thickening system is as long as one year, and the production capacity of equipment is greatly improved, so that the thickening process has high industrial application value.
Description
Technical field
The present invention relates to a kind of thickening technology of thick hexanodioic acid, especially a kind of thickening process of the thick hexanodioic acid that uses static cluster type thickener.
Background technology
Hexanodioic acid has another name called hexane dicarboxylic acid, adipic acid (Adipic acid; Hexanedioic acid, is called for short AA) be most important aliphatic dibasic acid, can carry out condensation reaction with multi-functional compound, as industrial, utilize the condensation reaction of the same diamines of adipic acid to produce nylon salt, further polycondensation obtains Nylon 66.In addition, hexanodioic acid also can be produced adipic acid ester with alcohols reaction, as products such as softening agent, synthetic lubricant and polyester polyols.Adipic acid, as the souring agent of various food and drink, is still the raw material of medicine, yeast purification, sterilant, tamanori, synthetic leather, synthol and spices simultaneously.Along with the development of China's oil chemical industry, national economy will improve constantly the demand of hexanodioic acid.
Hexanodioic acid is to make catalyzer with copper and vanadium, with nitric acid oxidation hexalin reaction generation.Then through crystallization, enrichment, centrifugally obtain thick hexanodioic acid.Thick hexanodioic acid through dissolving, activated carbon decolorizing is again through crystallization, enrichment, obtain smart adipic acid product after centrifugal, dry.
Thick hexanodioic acid thickening technology belongs to thick hexanodioic acid workshop section, first the thick hexanodioic acid salpeter solution coming from oxidation operation in thick hexanodioic acid workshop section enters crystallizer, crystallizer is divided into multiple crystallisation chamber, the operating temperature and pressure of each crystallisation chamber becomes stepped reduction, press the crystallization curve design of material, under vacuum, adiabatic evaporation cooling crystallizes out hexanodioic acid from salpeter solution.Then, containing the slurry of crystallization of adipic acid, enter enrichment strainer and whizzer, after centrifuge dehydration, obtain thick hexanodioic acid.
Thick hexanodioic acid thickener is one of key equipment of Production Processes of Adipic Acid.If the hexanodioic acid magma from thick crystallization of adipic acid device is directly delivered to whizzer, can cause whizzer operational load to strengthen, reduce separating effect, the power of whizzer can be larger simultaneously, and number of units can be more.So adopt suitable thickener very crucial, in old-fashioned thickener, be provided with rotational circle dish type filter frame, filter screen is stainless steel metal wire mesh grid, each filter frame is divided into again 12 independently compartments.During operation, filter frame is with certain rotating speed rotation, and when filter frame rotates to certain angle, filtrate is extracted pipeline out and is attached thereto, now filtrate is drawn out of, and filter cake is attached on filter screen, when filter frame rotates to another angle, clear liquid is pressed into pipeline and is attached thereto, and now filter cake is swept away and sinks to thickener bottom.Visible, thus old-fashioned thickener is to realize thickening power by the rotation of filter frame, but this rotating machinery failure rate is high, and its time of moving continuously only had about two months, and this makes continuous production poor, and device capbility is limited.Simultaneously old-fashioned filter is clapped after application for some time and also can be followed " escaping crystalline substance " phenomenon, and the content increase of " escaping crystalline substance " in filtrate has not only reduced the economy of device, also makes in the systematic stock solution hexanodioic acid content higher, and through constantly accumulation, the risk of system jams rises.
Summary of the invention
The problem that invention will solve is to overcome that old-fashioned dynamically to turn the equipment failure rate that bat formula thickener spills cruelly high, and the problem such as the continuous production of thickening system is poor, and device capbility is limited provides a kind of thickening process of thick hexanodioic acid.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
A thickening process for thick hexanodioic acid, is used static cluster type thickener in this technique, this thickener consists of thickener shell side and thickener tube side, adopts candle wick formula filtering element, is provided with several filter cores on the strainer tube of thickener tube side.
Whole operating process adopts sequential automatic control program, and operating process comprises that charging, filter cloth on-line cleaning, charging again, filtration, feed liquid are emptying, exhaust and filter cake discharge process.
Concrete steps are as follows:
(1) charging: when start a new filtration cycle, the self check that first brings into operation of thickener sequential procedure.Complete on inspection possess after operational conditions, and thickener feed valve is opened and started charging filling process.After being full of in thickener, closing feed valve and stop charging.
(2) filter cloth on-line cleaning: after charging filling step completes, start to carry out the operation of filter cloth on-line cleaning.Open compressed-air line valve, start to clean.
(3) charging again: through cleaning operation, in thickener, liquid level can decline, and therefore needs to carry out feed operation again.Open feed valve and start charging, after between sequential control arrival necessarily, stop.
(4) filter: after pre-filtering completes, start filter operation.Open thickener feed valve and filtrate outlet valve, after between sequential control arrival necessarily, stop filter operation.
(5) feed liquid is emptying: after having filtered, open thickener discharging valve, make in a part of solution backflow overfall batch can.
(6) exhaust: and then open thickener vent valve vent gas.
(7) filter cake is discharged: open compressed-air line valve and thickener below bleeder valve, utilize the filter cake on pressurized air blowback filter cloth, it is come off, enter into the intermediate pulp tank of thickener below.
One filtration cycle about 12-20 minute, preferably 14 minutes, according to actual condition capable of regulating filtration time, filtration time was relevant with the size of crystal grain in slurry, crystal grain is larger, pre-filtering and filtration procedure are effective, filtration time can shorten.
Before described filtration step, also comprise pre-filtering program, be specially:
Before filtering, need to carry out pre-filtering, open thickener feed valve and loop back slurry tank pipeline valve, start pre-filtering operation, by stopping after sequential control arrival certain hour.
The pre-filtering process that this measure refluxes by Matter Transfer is adhered to one deck hexanodioic acid solid on filtering element, thereby makes follow-up filtration procedure can reach desirable filter effect, has reduced the phenomenon with " escaping crystalline substance " in filtrate mother liquor acid.
Advantage and positively effect that the present invention has are:
The thickening process of a kind of thick hexanodioic acid of the present invention, adopts static cluster type structure, and it is short that thickener has filtration cycle, stable operation, good filtration effect, the feature that service life of equipment is long.The application of the static cluster type thickener of thick hexanodioic acid, significantly reduces equipment failure rate, and the continuous cycle of operation of thickening system is extended to more than 1 year by old-fashioned thickener for about two months, has increased substantially equipment capacity.By design optimization, adipic acid plant wastewater flow rate is significantly declined simultaneously, greatly reduce the load of follow-up sour concentration systems, device capbility also increases.
The present invention applies to static cluster type thickener in the production of hexanodioic acid first, the advantage of this technology has been to overcome the old-fashioned shortcoming that bat formula thickener equipment failure rate is high, the cycle of operation is short that dynamically turns, thickening system continuously-running, has increased substantially equipment capacity and device capbility.
Accompanying drawing explanation
Fig. 1 is the thickening process schematic flow sheet of a kind of thick hexanodioic acid of the present invention.
Fig. 2 is the structure diagram of thickener in the thickening of a kind of thick hexanodioic acid of the present invention.
In figure:
1, thick hexanodioic acid slurry tank 2, thick acid-thickened device fresh feed pump 3, thick hexanodioic acid thickener
4, thick hexanodioic acid whizzer 5, thick hexanodioic acid dissolving vessel 6, intermediate pulp tank
7, thickener shell side 8, thickener tube side 9, filter core
Embodiment
Below in conjunction with specific embodiment, the invention will be further described, but do not limit protection scope of the present invention.
A thickening process for thick hexanodioic acid, is used static cluster type thickener in this technique, this thickener consists of thickener shell side 7 and thickener tube side 8, adopts candle wick formula filtering element, is provided with several filter cores 9 on the strainer tube of thickener tube side.Whole operating process adopts sequential automatic control program.
The beginning of a filtration cycle, first Controlling System moves self-check program, checks whether the liquid level in thick hexanodioic acid slurry tank 1 and thick hexanodioic acid thickener 3 is normal liquid level, if liquid level is normal, enters filter.
Filtration procedure is as follows:
(1) charging: open the feed valve that thick acid-thickened device fresh feed pump 2 exports thick hexanodioic acid slurry is driven in thick hexanodioic acid thickener 3, in 180 seconds of opening time, on this pipeline, variable valve control flow is 240m
3/ h;
(2) filter cloth on-line cleaning: filter cloth on-line cleaning has four groups of pressurized air valves, during cleaning, opens respectively four groups of valves and carries out cleaning operation each 5 seconds;
(3) charging again: open the feed valve that thick acid-thickened device fresh feed pump 2 exports hexanodioic acid slurry is driven in thick hexanodioic acid thickener 3, in 15 seconds of opening time, on this pipeline, variable valve control flow is 240m
3/ h;
(4) pre-filtering: open the feed valve that thick acid-thickened device fresh feed pump 2 exports, on this pipeline, variable valve control flow is 180m
3/ h, opens thick hexanodioic acid thickener 3 simultaneously and loops back valve on thick hexanodioic acid slurry tank 1 pipeline, and pre-filtering starts, 20 seconds of filtration time;
(5) filter: open the feed valve that thick acid-thickened device fresh feed pump 2 exports, on this pipeline, variable valve control flow is 180m
3/ h, the filtrate outlet valve of simultaneously opening thick hexanodioic acid thickener 3 carries out filter operation, 180 seconds of filtration time;
(6) feed liquid is emptying: after having filtered, open the discharging valve of thick hexanodioic acid thickener 3, a part of solution is refluxed back in thick hexanodioic acid slurry tank 1, close discharging valve while reaching 2000mm by the liquidometer control liquid level on thick hexanodioic acid thickener 3.
(7) exhaust: open the vent valve vent gas on thick hexanodioic acid thickener 3.
(8) filter cake is discharged: open the bleeder valve of compressed-air line valve and thick hexanodioic acid thickener 3 belows, utilize the filter cake on pressurized air blowback filter cloth, it is come off, enter into the intermediate pulp tank 6 of thickener below, 40 seconds of opening time.
After thickening, it is centrifugal that hexanodioic acid magma is delivered to thick hexanodioic acid whizzer 4, enters afterwards thick hexanodioic acid dissolving vessel 5, and thickening mother liquor acid turns back to nitric acid enrichment process.
The thickening process of this kind of thick hexanodioic acid is short filtration cycle, stable operation, and good filtration effect, service life of equipment is long.The application of the static cluster type thickener of thick hexanodioic acid, significantly reduces equipment failure rate, and the continuous cycle of operation of thickening system is extended to more than 1 year by old-fashioned thickener for about two months, has increased substantially equipment capacity.By design optimization, adipic acid plant wastewater flow rate is significantly declined simultaneously, greatly reduce the load of follow-up sour concentration systems, device capbility also increases.
Above preferred embodiment of the present invention is had been described in detail, but described content is only preferred embodiment of the present invention, can not be considered to for limiting practical range of the present invention.All equalization variations of doing according to the present patent application scope and improvement etc., within all should still belonging to patent covering scope of the present invention.
Claims (1)
1. the thickening process of a thick hexanodioic acid, it is characterized in that: in this technique, use static cluster type thickener, this thickener consists of thickener shell side and thickener tube side, adopts candle wick formula filtering element, is provided with several filter cores on the strainer tube of thickener tube side;
Concrete filtration procedure is as follows:
(1) charging: the feed valve of opening thick acid-thickened device fresh feed pump outlet is driven into thick hexanodioic acid slurry in thick hexanodioic acid thickener, and in 180 seconds of opening time, on this pipeline, variable valve control flow is 240m
3/ h;
(2) filter cloth on-line cleaning: filter cloth on-line cleaning has four groups of pressurized air valves, during cleaning, opens respectively four groups of valves and carries out cleaning operation each 5 seconds;
(3) charging again: the feed valve of opening thick acid-thickened device fresh feed pump outlet is driven into hexanodioic acid slurry in thick hexanodioic acid thickener, and in 15 seconds of opening time, on this pipeline, variable valve control flow is 240m
3/ h;
(4) pre-filtering: open the feed valve of thick acid-thickened device fresh feed pump outlet, on this pipeline, variable valve control flow is 180m
3/ h, opens thick hexanodioic acid thickener simultaneously and loops back valve on thick hexanodioic acid slurry tank pipeline, and pre-filtering starts, 20 seconds of filtration time;
(5) filter: open the feed valve of thick acid-thickened device fresh feed pump outlet, on this pipeline, variable valve control flow is 180m
3/ h, the filtrate outlet valve of simultaneously opening thick hexanodioic acid thickener carries out filter operation, 180 seconds of filtration time;
(6) feed liquid is emptying: after having filtered, open the discharging valve of thick hexanodioic acid thickener, a part of solution is refluxed back in thick hexanodioic acid slurry tank, close discharging valve while reaching 2000mm by the liquidometer control liquid level on thick hexanodioic acid thickener;
(7) exhaust: open the vent valve vent gas on thick hexanodioic acid thickener;
(8) filter cake is discharged: open the bleeder valve of compressed-air line valve and thick hexanodioic acid thickener below, utilize the filter cake on pressurized air blowback filter cloth, it is come off, enter into the intermediate pulp tank of thickener below, 40 seconds of opening time.
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| CN201210247210.1A CN102731289B (en) | 2012-07-17 | 2012-07-17 | Thickening process of coarse adipic acid |
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| CN201210247210.1A CN102731289B (en) | 2012-07-17 | 2012-07-17 | Thickening process of coarse adipic acid |
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| CN104130119B (en) * | 2014-07-18 | 2016-03-09 | 中国天辰工程有限公司 | A kind of production method of superfinishing hexanodioic acid |
| CN104961635A (en) * | 2015-07-03 | 2015-10-07 | 新疆独山子天利高新技术股份有限公司 | Method and device of wastewater reuse pretreatment in adipic acid refining process |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2100933U (en) * | 1991-06-24 | 1992-04-08 | 上海川沙努力食品机械厂 | Candle type fitter machine |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2100933U (en) * | 1991-06-24 | 1992-04-08 | 上海川沙努力食品机械厂 | Candle type fitter machine |
Non-Patent Citations (4)
| Title |
|---|
| 李楷等.浅谈烛式过滤器在粗己二酸增稠器上的选型与应用.《河南化工》.2011,第28卷(第4期),49-51. |
| 李楷等.烛式过滤器在己二酸粗增稠器上的选型与应用.《石油与化工设备》.2011,第14卷(第4期),35-38. |
| 浅谈烛式过滤器在粗己二酸增稠器上的选型与应用;李楷等;《河南化工》;2011;第28卷(第4期);49-51,尤其是4.1.2 静态烛式过滤器、4.3.2 自控系统控制、4.4.1 熟悉物性、保证滤芯材质、4.3生产控制不同、表1、4. 3. 1 工作参数设定 * |
| 烛式过滤器在己二酸粗增稠器上的选型与应用;李楷等;《石油与化工设备》;2011;第14卷(第4期);35-38 * |
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