CN102826991B - Process and device for continuous acidification of acidification section in production of sebacic acid - Google Patents
Process and device for continuous acidification of acidification section in production of sebacic acid Download PDFInfo
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- CN102826991B CN102826991B CN201210258878.6A CN201210258878A CN102826991B CN 102826991 B CN102826991 B CN 102826991B CN 201210258878 A CN201210258878 A CN 201210258878A CN 102826991 B CN102826991 B CN 102826991B
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Abstract
The invention relates to the technical field of production of sebacic acid and discloses a process and a device for continuous acidification of an acidification section in production of sebacic acid. The process comprises the following steps of: heating a decoloring solution obtained in advance of the acidification section in a storage tank, pumping feed liquid into an acidifier for the acidification by a pipeline pump through a rotor flow meter, heating the feed liquid in a heating tank, cooling and crystallizing the feed liquid in an acidification crystallizing tank, and carrying out layering in a thickener through gravity settling; and after the layering in the thickener through the gravity settling is carried out, filtering clear mother liquid at the upper layer through a filter, discharging filtrate to a wastewater pool, and separating thick sebacic acid liquid (which flows to a drying procedure independently) at the a lower layer, wherein the continuous and layer-by-layer self-flowing of the feed liquid among the procedures is realized by virtue of the height difference of the feed liquid after the feed liquid is subjected to the acidification through the acidifier and the settlement through the thickener. The process and the device can be used for realizing the continuous production, improving the production efficiency, reducing the production cost, improving the product yield and quality, making the most of secondary water, and saving water resources.
Description
Technical field
The present invention relates to the production field of Chemicals sebacic acid, be specially continuously acidizing technique and the processing unit thereof of acidizing process in sebacic acid production.
Background technology
Sebacic acid is a kind of important fine-chemical intermediate, at present in industry mainly taking Viscotrol C as waste, also belong to one of agriculture and forest chemical industry product, high in technological content, added value is high, and it is widely used for production engineering plastics (as nylon 1010, NYLON610, nylon 8 10, nylon 9, nylon 9 10 etc.), cold resistant plasticizer, solvent, tenderizer, additive, dimethyl sebacate, ethyl sebacate, dioctyl sebacate, Uniflex DBS, Wickenol 117 and polyester derivatives etc.In addition be also used as the raw material of the aspects such as high temperature resistant luboil, epoxy curing agent, sebacic anhydride, synthetic lubricating ester and synthetic flavour, medicine.Along with the fast development of industrial plastic and softening agent, increasing to the demand of sebacic acid both at home and abroad, market outlook are boundless.
Taking Viscotrol C as waste sebacic acid, general technical process is Viscotrol C hydrolysis → cracking → neutralization → decolouring → acidifying → water dumping → refining → packaging, wherein acidizing process is the important procedure that is related to quality product and output, operation is reacted the sebacic acid list sodium salt obtaining and under the effect of sulfuric acid, is reacted generation sebacic acid above, and crystallization, therefore acidification technique directly affects the Quality and yield of sebacic acid product.The intermittent type acidification technique that at present domestic acidizing process in sebacic acid is produced generally adopts, the workshop section such as acid adding reacting by heating, crystallization thickening in acidification technique all carries out in same retort, from being fed to discharging, all taking tank as production of units, cannot realize the continuous production of continuous-flow type, seriously restrict output, equipment configuration automatization level is low, technique falls behind, and causes that production efficiency is low, the unstable product quality of output.In addition intermittently in acidifying when slow cooling, it is too much that penstock is opened, the easy ramming material of coil pipe, cooling-down effect is reduced, and temperature fall time increases, for shortening temperature fall time, must be a large amount of for recirculated water, cause water resources, energy dissipation serious, the more high problems of production cost.The technique falling behind at present has seriously restricted the development of enterprise and industry.
Summary of the invention
The technological deficiency existing for above-mentioned technical background, the object of the present invention is to provide a kind of sebacic acid produce in the equipment of continuously acidizing in the processing method of continuously acidizing and process application in acidifying workshop section, cannot meet the requirement of scale operation to meet intermittent type acidification technique.
Continuity acidification technique in sebacic acid acidifying of the present invention workshop section, develops into continous way acidifying by intermittent type acidifying, and its acid adding, intensification, decrease temperature crystalline, the each link of thickening have realized the continuously acidizing technique of feed liquid gravity flow.Its Technical Design is as accompanying drawing 3.
First continuously acidizing technique of the present invention be together in series acidifier, warming tank, acidizing crystal tank, thickener, carries out after acidifying from acidifier, and feed liquid utilizes liquid level difference to realize gravity flow, flows automatically to thickener operation always.
The destainer obtaining before described acidifying workshop section in hold-up vessel by steam heating to 85 DEG C-100 DEG C, through spinner-type flowmeter, feed liquid is driven into acidifier with in-line pump, utilize sulfuric acid high position tank to add sulfuric acid in acidifier simultaneously, the pH value of feed liquid is controlled to 1-3, feed liquid utilizes high potential difference to flow automatically to the first warming tank from acidifier, feed liquid is heated to more than 100 DEG C with well heater at the first warming tank, feed liquid is mixed, boiling, feed liquid flows automatically to the second warming tank, continue heating, further make feed liquid fully seethe with excitement, feed liquid flows to acidizing crystal tank certainly from the second warming tank, feed liquid is cooled to 85 DEG C-100 DEG C naturally through the first step to third stage acidizing crystal tank, make souring tank mixing control at 25-35 rev/min simultaneously, feed liquid is lowered the temperature with intermediate water when through seven grades of acidizing crystal tanks of the fourth stage to the, drop to 65 DEG C-70 DEG C, lowering the temperature with intermediate water equally to the tenth two-stage acidulation crystallizer through the 8th grade, drop to 45 DEG C-50 DEG C, finally by the 13 grade during to the 16 grade of acidizing crystal tank with an a small amount of water for cooling to 30 DEG C～40 DEG C, the feed liquid that contains sebacic acid crystal, continue to flow automatically to thickener, sebacic acid sedimentation under the effect of gravity, the clear mother liquor stream on upper strata is to strainer, through filtering, a small amount of sebacic acid is stopped, after filtration, the clear mother liquor containing sebacic acid does not flow to wastewater disposal basin, the sebacic acid dope of lower floor flows automatically to water dumping operation and separates.
The equipment of continuously acidizing technique in a kind of sebacic acid production, comprise: storage tank, in-line pump, acidifier, warming tank, acidizing crystal tank, is characterized in that described storage tank discharge port is provided with in-line pump, in-line pump discharge port is connected with acidifier feeding mouth by pipeline, and the locus of acidifier, warming tank, four kinds of equipment of acidizing crystal tank and thickener is connected, is fixed by pipeline from top to bottom.
On the sebacic acid list sodium salt input channel of acidifier, under meter and accurate filter are all installed on the pipeline of sulfuric acid input, acidifier is connected with a sulfuric acid high position tank by sulfuric acid input channel.
Described warming tank is that two-stage warming tank is connected up and down, acidizing crystal tank is that 16 grades of acidizing crystal tanks are connected up and down, in acidizing crystal tank, agitator is installed, before first three grade of acidizing crystal pot bottom, the position of coil pipe is chuck, last step acidizing crystal device discharge port is connected with thickener opening for feed pipeline, and agitator is installed in thickener.
The beneficial effect of the technical scheme of sebacic acid continuously acidizing Processes and apparatus of the present invention is:
In technical solutions according to the invention, the souring tank of generally applying in intermittent type acidifying is changed into acidifier, warming tank.And on the pipeline of the sebacic acid list sodium salt input of acidifier, on the pipeline of sulfuric acid input, under meter is installed respectively, and so that control material liquid pH, be separately installed with accurate filter, filter impurity, to ensure feed liquid quality.Solve material spray problem, ensured workman's safety operation.In addition, the supply of sulfuric acid, has increased sulfuric acid high position tank, utilizes high potential difference to supply acid, avoids using sulfated pump often to occur acidifying fault, has stablized the continuity of acidifying.
In described warming tank operation, warming tank adopts the design of heating of two-stage warming tank, makes feed liquid have time enough fully to mix, and stablizes pH value, dissolves sebacic acid completely.
In described acidizing crystal operation, in tank, sebacic acid and sodium sulfate mixed solution are taked the mode of lowering the temperature step by step, have solved cooling rate too fast, and difference variation is huge, affect crystalline particle and the interior quality of sebacic acid; Cross slowly, reduce production efficiency, increase the problem of production cost, ensured the quality of sebacic acid.In addition the coil pipe of first three grade of acidizing crystal tank is removed, utilize chuck to carry out just cooling, solved coil pipe ramming material problem.After last step souring tank, increase thickener, acidizing fluid is separated automatically, improve the utilization ratio of whizzer in follow-up water dumping operation.
In described thickener operation, thickener is provided with agitator, and stirring velocity per minute 5-10 turns, and can stir sebacic acid dope and prevent sebacic acid dope blocking pipe, can not hinder again the sedimentation of sebacic acid.
Continuously acidizing technique of the present invention is got up the devices in series such as acidizing crystal tank, has overcome the intermittently dependence of acidifying to tank quantity and manpower, has saved manpower, and process parameter is better controlled, and can meet the requirement of large scale continuous prod; Material and sulfuric acid measure with spinner-type flowmeter, material from acidifier to warming tank in, can fully mix, fully boiling, stable operation, has ensured quality.In the cooling process of continuously acidizing, make full use of intermediate water series connection cooling, comparing must be a large amount of for recirculated water in gloxylic acid metallization processes, save water resources, the mode of connection of souring tank thoroughly changes, overcome troubling coil pipe ramming material problem in intermittently acidifying, and manually frequent switch stirring and steam valve, penstock, production efficiency greatly improved.The acidifying of continuously acidizing is in acidifier, and acidifying, the acidified crystallizer of the material having seethed with excitement have overcome the shortcoming of corroding acidifying crystallizer, have ensured workman's safety.In the time that middle control detects chemical examination, continuously acidizing is only just passable from a regular sample examination in control point, has overcome the intermittently defect of the necessary every tank chemical examination of acidifying, has saved manpower, has saved expense, has improved efficiency.
Continuously acidizing technical scheme of the present invention can effectively promote the progress of sebacic acid production technology, significantly promote the original throughput of sebacic acid enterprise, reduce production costs, improve industry overall technology level, promote whole industry health, sustainable development, drive the development of upstream and downstream related industries, industrialization prospect is wide.
Brief description of the drawings
Accompanying drawing 1 is technological process apparatus figure: 1 storage tank, 2 acidifiers, 3 two-stage warming tanks, 40 six grades of acidizing crystal tanks.
Accompanying drawing 2 is continuously acidizing equipment drawing: 1 storage tank, 2 acidifiers, 3 two-stage warming tanks, 40 six grades of acidizing crystal tanks, 5 in-line pumps, 6 spinner-type flowmeters, 7 strainers, 8 sulfuric acid high position tanks, 9 thickeners.
Accompanying drawing 3 is acidification reaction technical scheme steps.
Embodiment
The continuously acidizing technique and the processing unit that the invention discloses acidifying workshop section in a kind of sebacic acid production, the art personnel can use for reference content herein, suitably improve processing parameter and realize.Special needs to be pointed out is, all similar replacements and change are apparent to those skilled in the art of the present technique, and they are all deemed to be included in the present invention.Method of the present invention and application are described by preferred embodiment, related personnel obviously can change methods and applications as herein described in content of the present invention, spirit and scope or suitably change and combination not departing from, and realizes and apply the technology of the present invention.
Embodiment:
In sebacic acid production, a processing unit for continuously acidizing, comprising: 1 storage tank, 2 acidifiers, 3 two-stage warming tanks, 40 six grades of acidizing crystal tanks, 5 in-line pumps, 6 spinner-type flowmeters, 7 strainers, 8 sulfuric acid high position tanks, 9 thickeners.Wherein said storage tank 1 discharge port is provided with in-line pump 5, in-line pump 5 discharge ports are connected with acidifier 2 feeding mouths by pipeline, spinner-type flowmeter 6 is installed on this segment pipe, and acidifier 2, warming tank 3, acidizing crystal tank 4 are connected and fixed by pipeline from top to bottom with the locus of 9 four kinds of equipment of thickener.
Wherein on the sebacic acid list sodium salt input channel of acidifier 2, under meter 6 and accurate filter 7 are installed respectively on the pipeline of sulfuric acid input, acidifier 2 is connected with sulfuric acid high position tank 8 by sulfuric acid input channel.
Wherein warming tank 3 is connected up and down for two-stage warming tank, acidizing crystal tank is that 16 grades of acidizing crystal tanks 4 are connected up and down, in acidizing crystal tank 4, agitator is installed, before first three grade of acidizing crystal pot bottom, the position of coil pipe is chuck, last step acidizing crystal tank discharge port is connected with thickener 9 opening for feed pipelines, in thickener 9, agitator is installed.
Embodiment 1
Produce continuously acidizing technique according to sebacic acid of the present invention, comprise the following steps:
Destainer in hold-up vessel by steam heating to 92 DEG C, be driven into acidifier through spinner-type flowmeter with in-line pump, in acidifier, add sulfuric acid by 15% than row simultaneously, the pH value of feed liquid is controlled to 2, feed liquid utilizes high potential difference to flow automatically to the first warming tank from acidifier, feed liquid is heated to more than 100 DEG C with well heater at the first warming tank, feed liquid is mixed, boiling, feed liquid flows automatically to the second warming tank, continue heating, further make feed liquid fully seethe with excitement, feed liquid flows to acidizing crystal tank certainly from the second warming tank, feed liquid is cooled to 85 DEG C naturally through the first step to third stage acidizing crystal tank, make souring tank mixing control turn at per minute 27 simultaneously, after feed liquid, when through seven grades of acidizing crystal tanks of the fourth stage to the, lower the temperature with intermediate water, drop to 65 DEG C, lowering the temperature with intermediate water equally to the tenth two-stage acidulation crystallizer through the 8th grade, drop to 45 DEG C, finally by the 13 grade during to the 16 grade of acidizing crystal tank with an a small amount of water for cooling to 30 DEG C, the feed liquid that contains sebacic acid crystal, continue to flow automatically to thickener, thickener agitator stirring velocity per minute 5 turns, sebacic acid sedimentation under the effect of gravity, the clear mother liquor stream on upper strata is to strainer, through filtering, a small amount of sebacic acid is stopped, after filtration, the clear mother liquor containing sebacic acid does not flow to wastewater disposal basin, the sebacic acid dope of lower floor flows automatically to water dumping operation and separates.
Embodiment 2
Produce continuously acidizing technique according to sebacic acid of the present invention, comprise the following steps:
Destainer in hold-up vessel by steam heating to 96 DEG C, be driven into acidifier through spinner-type flowmeter with in-line pump, in acidifier, add sulfuric acid by 18% than row simultaneously, the pH value of feed liquid is controlled to 1.5, feed liquid utilizes high potential difference to flow automatically to the first warming tank from acidifier, feed liquid is heated to more than 100 DEG C with well heater at the first warming tank, feed liquid is mixed, boiling, feed liquid flows automatically to the second warming tank, continue heating, further make feed liquid fully seethe with excitement, feed liquid flows to acidizing crystal tank certainly from the second warming tank, feed liquid is cooled to 95 DEG C naturally through the first step to third stage acidizing crystal tank, make souring tank mixing control turn at per minute 30 simultaneously, after feed liquid, when through seven grades of acidizing crystal tanks of the fourth stage to the, lower the temperature with intermediate water, drop to 70 DEG C, lowering the temperature with intermediate water equally to the tenth two-stage acidulation crystallizer through the 8th grade, drop to 50 DEG C, finally by the 13 grade during to the 16 grade of acidizing crystal tank with an a small amount of water for cooling to 40 DEG C, the feed liquid that contains sebacic acid crystal, continue to flow automatically to thickener, thickener agitator stirring velocity per minute 5 turns, sebacic acid sedimentation under the effect of gravity, the clear mother liquor stream on upper strata is to strainer, through filtering, a small amount of sebacic acid is stopped, after filtration, the clear mother liquor containing sebacic acid does not flow to wastewater disposal basin, the sebacic acid dope of lower floor flows automatically to water dumping operation and separates.
Embodiment 3
Produce continuously acidizing technique according to sebacic acid of the present invention, comprise the following steps:
Destainer in hold-up vessel by steam heating to 97 DEG C, be driven into acidifier through spinner-type flowmeter with in-line pump, in acidifier, add sulfuric acid by 20% than row simultaneously, the pH value of feed liquid is controlled to 1.5, feed liquid utilizes high potential difference to flow automatically to the first warming tank from acidifier, feed liquid is heated to more than 100 DEG C with well heater at the first warming tank, feed liquid is mixed, boiling, feed liquid flows automatically to the second warming tank, continue heating, further make feed liquid fully seethe with excitement, feed liquid flows to acidizing crystal tank certainly from the second warming tank, feed liquid is cooled to 95 DEG C naturally through the first step to third stage acidizing crystal tank, make souring tank mixing control turn at per minute 25 simultaneously, after feed liquid, when through seven grades of acidizing crystal tanks of the fourth stage to the, lower the temperature with intermediate water, drop to 75 DEG C, lowering the temperature with intermediate water equally to the tenth two-stage acidulation crystallizer through the 8th grade, drop to 55 DEG C, finally by the 13 grade during to the 16 grade of acidizing crystal tank with an a small amount of water for cooling to 40 DEG C, the feed liquid that contains sebacic acid crystal, continue to flow automatically to thickener, thickener agitator stirring velocity per minute 7 turns, sebacic acid sedimentation under the effect of gravity, the clear mother liquor stream on upper strata is to strainer, through filtering, a small amount of sebacic acid is stopped, after filtration, the clear mother liquor containing sebacic acid does not flow to wastewater disposal basin, the sebacic acid dope of lower floor flows automatically to water dumping operation and separates.
After project operation product index and national standard index contrast:
Excellent product performance and stable, meets or exceeds GB 2092-92 standard-requireds completely, after the operation of continuously acidizing operation item, the company that ensured produces the trouble-free operation of the sebacic acid production line of 10000 tons per year, sebacic acid yield improves 3%, 80 yuan of production cost reductions per ton, and year is reduced expenses 800,000 yuan; Expand end-use, improved production marketing price and share of market, for Sustainable Development of Enterprises has been established solid basis.
Claims (7)
1. the technique of acidifying workshop section continuously acidizing in a sebacic acid production, it is characterized in that the destainer obtaining before acidifying workshop section heats in storage tank, after heating, through spinner-type flowmeter, feed liquid is driven into acidifier with in-line pump and carries out acidifying, after acidifying, feed liquid gravity flow enters warming tank heating, after heating, gravity flow enters acidizing crystal tank decrease temperature crystalline, what described decrease temperature crystalline operation adopted is the mode that crystallizer is lowered the temperature step by step, wherein the first step to third stage acidizing crystal tank is nature cooling, make souring tank mixing control turn at per minute 20-40 simultaneously, the fourth stage to the ten two-stage acidulation crystallizers are lowered the temperature with intermediate water, 13 grades to the 16 grade water for cooling for acidizing crystal tank, to the 16 grade, be cooled to 30 DEG C～40 DEG C, after crystallization, gravity flow enters the layering of thickener gravity settling, after the layering of thickener gravity settling, the clear mother liquor stream in upper strata is filtered to strainer, filtrate is discharged to wastewater disposal basin, lower floor's sebacic acid dope flows automatically to water dumping operation and separates, wherein feed liquid is acidified to the operation of thickener sedimentation layering from acidifier, feed liquid high potential difference is realized the gravity flow of continuous successively inter process.
2. continuously acidizing technique according to claim 1, is characterized in that the type of heating of destainer in hold-up vessel is steam heating, and feed liquid is heated to 85 DEG C-100 DEG C.
3. continuously acidizing technique according to claim 1, is characterized in that acidifying acid is sulfuric acid, and after acidifying, the pH of feed liquid is controlled at 1-3.
4. continuously acidizing technique according to claim 1, is characterized in that described warming tank is heated to be the heating of two-stage warming tank, and every grade of warming tank is all heated to feed liquid boiling.
5. continuously acidizing technique according to claim 1, is characterized in that there is stirring in described thickener, and stirring velocity is controlled at 5-10 rev/min.
6. the equipment of continuously acidizing technique in a sebacic acid production, comprise: storage tank, in-line pump, acidifier, warming tank, acidizing crystal tank, it is characterized in that described storage tank discharge port is provided with in-line pump, in-line pump discharge port is connected with acidifier feeding mouth by pipeline, acidifier, warming tank, acidizing crystal tank is connected by pipeline from top to bottom with the locus of four kinds of equipment of thickener, fixing, described warming tank is that two-stage warming tank is connected up and down, acidizing crystal tank is that 16 grades of acidizing crystal tanks are connected up and down, in acidizing crystal tank, agitator is installed, before first three grade of acidizing crystal pot bottom, the position of coil pipe is chuck, last step acidizing crystal device discharge port is connected with thickener opening for feed pipeline, agitator is installed in thickener.
7. the equipment of continuously acidizing technique in a kind of sebacic acid production according to claim 6, it is characterized in that: on the sebacic acid list sodium salt input channel of acidifier, under meter and accurate filter are all installed on the pipeline of sulfuric acid input, acidifier is connected with a sulfuric acid high position tank by sulfuric acid input channel.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210258878.6A CN102826991B (en) | 2012-07-24 | 2012-07-24 | Process and device for continuous acidification of acidification section in production of sebacic acid |
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| CN201210258878.6A CN102826991B (en) | 2012-07-24 | 2012-07-24 | Process and device for continuous acidification of acidification section in production of sebacic acid |
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| CN102826991A CN102826991A (en) | 2012-12-19 |
| CN102826991B true CN102826991B (en) | 2014-09-24 |
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| CN106366042B (en) * | 2016-08-29 | 2019-03-19 | 石家庄杰克化工有限公司 | A kind of 4,6- dihydroxy-pyrimidine continuously acidizing technique |
| CN114917850A (en) * | 2022-06-13 | 2022-08-19 | 宁夏恒力生物新材料有限责任公司 | Device and method for purifying aqueous phase of long-carbon-chain dibasic acid fermentation liquor |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101318892A (en) * | 2008-07-23 | 2008-12-10 | 张敏 | Method for preparing sebacic acid with ricinus oil compounds |
| CN201520730U (en) * | 2009-10-20 | 2010-07-07 | 河南金丹乳酸科技有限公司 | Reaction equipment for continuous acidolysis during production of lactic acid |
| CN102060691A (en) * | 2010-12-13 | 2011-05-18 | 日照鲁信金禾生化有限公司 | Continuous acidolysis process for calcium hydrogen citrate |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101318892A (en) * | 2008-07-23 | 2008-12-10 | 张敏 | Method for preparing sebacic acid with ricinus oil compounds |
| CN201520730U (en) * | 2009-10-20 | 2010-07-07 | 河南金丹乳酸科技有限公司 | Reaction equipment for continuous acidolysis during production of lactic acid |
| CN102060691A (en) * | 2010-12-13 | 2011-05-18 | 日照鲁信金禾生化有限公司 | Continuous acidolysis process for calcium hydrogen citrate |
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