CN101607922B - Acrylamide crystal preparation method - Google Patents
Acrylamide crystal preparation method Download PDFInfo
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- CN101607922B CN101607922B CN200910101271A CN200910101271A CN101607922B CN 101607922 B CN101607922 B CN 101607922B CN 200910101271 A CN200910101271 A CN 200910101271A CN 200910101271 A CN200910101271 A CN 200910101271A CN 101607922 B CN101607922 B CN 101607922B
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- acrylic amide
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Abstract
The invention relates to an acrylamide crystal preparation method, comprising the following steps: (1) sending low concentration of acrylamide stock solution into a preheater, then keeping the temperature of the solution at 75-85 DEG C; sending the preheated acrylamide stock solution to an evaporator of which temperature is controlled at 75-85 DEG C, then sending the solution to a separator to separate steam and concentrated solution, sending steam to a compressor from the steam outlet of the separator to store energy and form secondary steam, then sending the steam back to the evaporator through the steam inlet of the evaporator, exchanging heat in the evaporator, sending the condensed water generated by the heat exchange through the preheater to preheat the acrylamide stock solution which is sent in the preheater and form distilled water; processing crystallization step on the concentrated solution of which the weigh percent of acrylamide is controlled above 55% in the separator; refluxing the concentrated solution which does not meet the demand to the stock solution; (2) crystallizing, centrifuging and drying the concentrated solution of which the weigh percent of acrylamide is above 55% to obtain acrylamide crystal. Compared with the prior art, the invention has the advantages of low energy consumption and cost.
Description
Technical field
The present invention relates to a kind of preparation method of acrylamide crystal.
Background technology
Acrylic amide (Acryl amide) is a kind of broad-spectrum important Organic Chemicals, is not following hundred kinds of unit synthetic products with it, wherein is mainly used in to produce SEPIGEL 305 (Polyacrylamide).SEPIGEL 305 is widely used in every field such as oil production, paper industry, ore dressing, coal washing, metallurgy, water treatment, sugaring, building materials, fabric treating and chemical industry as flocculation agent, thickening material, toughener etc.Because the market potential of SEPIGEL 305 in above each field shows especially day by day; The particularly progressively rise of environmental protection industry; Will bigger demand be arranged to SEPIGEL 305; Must the more acrylamide monomer of demand, so the acrylic amide industry has wide developing prospect, the development in this field also will fully develop talents.Yet China's acrylic amide depends on import to a great extent at present, and output in domestic far can not satisfy the needs of every profession and trade, particularly can not satisfy the demand of high purity polypropylene acid amides, so the product broad market prospect.
In 19 end of the centurys, synthesized acrylic amide first from acrylate chloride and ammonia.1954, American Cyanamid Co. adopted vinyl cyanide sulphuric acid hydrolysis technology to carry out industrial production.1972, Mitsui east pressed chemical company at first to set up the full scale plant of skeleton copper (seeing metal catalyst) catalyzing propone nitrile hydration system acrylic amide, and after this various countries have developed dissimilar catalyzer in succession, adopt this technology to carry out industrial production.The eighties, Japanese Ri Dong chemical industrial company has realized with the industrial production of biological catalyst by vinyl cyanide system acrylic amide.
The technology that microbial method is produced acrylic amide as the third generation has highly selective, high reactivity and high-efficiency characteristics.Reacting completely of vinyl cyanide and water, impurity such as no coupling product, inorganic salt and remaining copper ion.
The production of acrylic amide generally is after generating acrylamide solution by acrylonitrile hydration, to prepare acrylamide crystal through the method that concentrates, cools again.Traditional crystal production technology is: with getting into upgrading tower top after 0.3MPa (table) steam heating.In upgrading tower, air counter current contact on column plate of going into tower from the tower lower curtate that feed liquid and roots blower are sent here is conducted heat, and air is taken away moisture evaporated in the feed liquid from cat head.Circulation when the concentration of acrylic amide reaches 50%～70%, through recycle pump, separates laggard drying machine with whizzer to crystallizer after concentrating again.Like application number is open " a kind of preparation method of acrylamide crystal " (publication number is CN101143831A) of Chinese invention patent application of 200710122048.X, and and for example application number is open " a kind of working method of acrylamide crystal " (publication number is CN101391967A) of Chinese invention patent application of 200810224258.4.The production of existing acrylamide crystal must will be accomplished preliminary concentrating at upgrading tower, the problem that therefore exists earlier: at first, upgrading tower uses steam to need to replenish endlessly, and power consumption is high, and cost is big; Secondly, upgrading tower is bulky, takies very big space; Once more, water resources can not rational and effective recycle, and waste is serious; At last, flow process is complicated, and the production cycle is longer.Also there is the patent documentation that adopts scraper evaporator to accomplish preliminary spissated preparation acrylamide crystal open; See that application number is 200610043896.7 Chinese invention patent application open " producing the method for acrylamide crystal " (publication number is CN1844086A); This application exists equally; The shortcoming of power consumption waste water needs to improve and develop new technical scheme.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of power consumption low to the above-mentioned state of the art, the preparation method of acrylamide crystal that cost is little.
The present invention solves the problems of the technologies described above the technical scheme that is adopted: a kind of preparation method of acrylamide crystal is characterized in that comprising the steps:
1. the acrylic amide stoste of lower concentration remains 75～85 ℃ through preheater through temperature behind the preheater; Acrylic amide stoste after the preheating is passed in the vaporizer, and then is passed in the separator, and evaporator temperature is controlled at 75 ℃～85 ℃; After acrylic amide stoste gets into separator; Isolate steam and liquid concentrator, steam comes out to form secondary steam through the compressor accumulation of energy from the vapour outlet of separator, gets back to the steam inlet of vaporizer; In vaporizer, carry out heat exchange; Water of condensation after the heat exchange carries out preheating through described preheater to the acrylic amide stoste that gets into preheater, forms zero(ppm) water after the preheating; The weight percent of acrylic amide is controlled at the liquid concentrator more than 55% in the separator, gets into crystallisation step; Not meeting the requirements of liquid concentrator is back in the stoste;
2. the weight percent of acrylic amide through crystallization, centrifugal, dry, promptly gets acrylamide crystal at the liquid concentrator more than 55%.
Acrylic amide weight percent in the acrylic amide stoste of step described in 1. can be 25%.
The acrylic amide stoste of step in is 1. passed through preheater through behind the surge tank earlier again.Be convenient to control the former flow velocity of acrylic amide, be beneficial to preheating and follow-up heat exchange.
The vaporizer of step in 1. adopts and rises film or the falling liquid film mode is evaporated.
As preferably, the secondary steam temperature of step in 1. is controlled at 83～93 ℃.
Further, step does not meet the requirements of the stoste import that liquid concentrator is back to vaporizer in 1. and evaporates separation again.
As preferably, during the 1. described compressor operating of step, vacuum tightness is 40～60Kpa.
The crystallization of step in 2., centrifugal, dry, adopt following mode for preferred:
Get into crystallizer after chilled brine is cooled to 4 ℃～6 ℃; Form the acrylic amide magma; Then the acrylic amide magma is transferred in the magma still; The solid-liquid weight ratio reaches 9: 1 above magmas and changes whizzer over to from the magma still, takes off a layer wet feed after centrifugal and falls into worm conveyor and deliver to drying bed and carry out drying.
Weight in wet base per-cent is no more than 5% in the described wet feed, is beneficial to oven dry.
Compared with prior art, the invention has the advantages that: the steam that separator comes out forms secondary steam to the vaporizer heat supply through the compressor accumulation of energy; Be used for the heat exchange of acrylic amide stoste, the steam of the usefulness that circulates so directly separates from acrylic amide stoste and converts, and does not need extra additional steam; As long as compressor is improved kinetic energy, power consumption reduces greatly, and condensed zero(ppm) water can also be applied to other aspects; Water resources is rationally recycled, and the overall manufacturing cost reduces greatly; Whole evaporation separation system volume is less relatively, is beneficial to spatial arrangement, and technical process is simple, and the cycle of producing acrylamide crystal reduces relatively.
Description of drawings
Fig. 1 is the process flow sheet of embodiment step in 1..
Embodiment
Embodiment describes in further detail the present invention below in conjunction with accompanying drawing.
Preparation method of acrylamide crystal in the present embodiment comprises the steps:
1. as shown in Figure 1, the acrylic amide stoste of lower concentration (weight percent is 25%) is passed through surge tank (do not have the figure and show), preheater 4 successively after original fluid container comes out, remain 75 ℃～85 ℃ through preheater 4 back temperature, is the best with 80 ℃; Acrylic amide stoste after the preheating is driven in the vaporizer 1 by pump 5, and the acrylic amide stoste that will obtain heat then is passed in the separator 2 again, and vaporizer 1 temperature is controlled at 75 ℃～85 ℃; Preferred 80 ℃, acrylic amide stoste is isolated steam and liquid concentrator after getting into separator 2; Steam comes out to form secondary steam through compressor 3 accumulation of energys from the vapour outlet of separator 2, and the secondary steam temperature is controlled at 83 ℃～93 ℃, is the best with 88 ℃; During compressor operating, vacuum tightness is 40～60Kpa.Secondary steam is got back to the steam inlet of vaporizer 1, in vaporizer 1, carries out heat exchange, and the water of condensation after the heat exchange carries out preheating through preheater 4 to the acrylic amide stoste that gets into preheater 4, forms zero(ppm) water after the preheating; The weight percent of acrylic amide reaches 60% liquid concentrator in the separator 2, gets into crystallisation step; Do not meet the requirements of the stoste import that liquid concentrator is back to vaporizer 1 and evaporate separation again.Wherein, preheater 4 adopts plate-type heat-exchange, and vaporizer 1 adopts the shell and tube heat exchange, and vaporizer 1 employing rises film or the falling liquid film mode is evaporated.
At first in vaporizer 1, squeeze into a part of bright steam acrylic amide stoste is carried out heat exchange; Wait whole evaporation separation system to reach thermal equilibrium then; Need not continue to mend bright steam this moment and heat, only need compressor 3 to keep the thermal equilibrium of whole evaporation separation system.Whole evaporation separation system all has PLC control to realize, all outputs and incoming semator system operation are accomplished by computingmachine, and level of automation improves greatly.
2. the weight percent of acrylic amide reaches 60% liquid concentrator and gets into crystallizers after-9 ℃ of chilled brines are cooled to 4 ℃～6 ℃ by pump 6; Form the acrylic amide magma, then the acrylic amide magma is transferred in the magma still, the solid-liquid weight ratio reaches 9: 1 above magmas and changes whizzer over to from the magma still; Taking off a layer wet feed after centrifugal falls into worm conveyor and delivers to drying bed and carry out drying; Weight in wet base per-cent is no more than 5% in the wet feed, and wet feed with after warm air fully contacts boiling fluidisation dehydrates, promptly gets acrylamide crystal in drying bed; Deliver to the automatic packing machine packing by tremie pipe at last, wait to produce.
Claims (8)
1. a preparation method of acrylamide crystal is characterized in that comprising the steps:
1. the acrylic amide stoste of lower concentration remains 75 ℃～85 ℃ through preheater through temperature behind the preheater; Acrylic amide stoste after the preheating is passed in the vaporizer, and then is passed in the separator, and evaporator temperature is controlled at 75 ℃～85 ℃; After acrylic amide stoste gets into separator; Isolate steam and liquid concentrator, steam comes out to form secondary steam through the compressor accumulation of energy from the vapour outlet of separator, gets back to the steam inlet of vaporizer; In vaporizer, carry out heat exchange; Water of condensation after the heat exchange carries out preheating through described preheater to the acrylic amide stoste that gets into preheater, forms zero(ppm) water after the preheating; The weight percent of acrylic amide is controlled at the liquid concentrator more than 55% in the separator, gets into crystallisation step; Not meeting the requirements of liquid concentrator is back in the stoste;
2. the weight percent of acrylic amide through crystallization, centrifugal, dry, promptly gets acrylamide crystal at the liquid concentrator more than 55%;
Step does not meet the requirements of the stoste import that liquid concentrator is back to vaporizer in 1. and evaporates separation again.
2. preparation method according to claim 1 is characterized in that the acrylic amide weight percent in the acrylic amide stoste described in step 1. is 25%.
3. preparation method according to claim 1 is characterized in that the acrylic amide stoste during step is 1. passed through preheater through behind the surge tank earlier again.
4. preparation method according to claim 1 is characterized in that vaporizer during step 1. adopts to rise film or the falling liquid film mode is evaporated.
5. preparation method according to claim 1 is characterized in that the secondary steam temperature during step 1. is controlled at 83 ℃～93 ℃.
6. preparation method according to claim 1, when it is characterized in that the 1. described compressor operating of step, vacuum tightness is 40～60Kpa.
7. preparation method according to claim 1 is characterized in that the crystallization, centrifugal, dry during step is 2., adopts following mode:
Get into crystallizer after chilled brine is cooled to 4 ℃～6 ℃; Form the acrylic amide magma; Then the acrylic amide magma is transferred in the magma still; The solid-liquid weight ratio reaches 9: 1 above magmas and changes whizzer over to from the magma still, takes off a layer wet feed after centrifugal and falls into worm conveyor and deliver to drying bed and carry out drying.
8. preparation method according to claim 7 is characterized in that weight in wet base per-cent is no more than 5% in the described wet feed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910101271A CN101607922B (en) | 2009-07-24 | 2009-07-24 | Acrylamide crystal preparation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910101271A CN101607922B (en) | 2009-07-24 | 2009-07-24 | Acrylamide crystal preparation method |
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| CN101607922A CN101607922A (en) | 2009-12-23 |
| CN101607922B true CN101607922B (en) | 2012-09-19 |
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| CN200910101271A Expired - Fee Related CN101607922B (en) | 2009-07-24 | 2009-07-24 | Acrylamide crystal preparation method |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101920122A (en) * | 2010-08-20 | 2010-12-22 | 王德兴 | Backheating evaporation technology and technology system thereof |
| CN102212016A (en) * | 2010-08-20 | 2011-10-12 | 江苏南天农科化工有限公司 | Preparation method of acrylamide crystal with ultra low water content |
| CN102407029A (en) * | 2011-10-17 | 2012-04-11 | 宜兴市格兰特干燥浓缩设备有限公司 | Evaporated crystallization device |
| CN102659196A (en) * | 2012-05-28 | 2012-09-12 | 天津壹帆水务有限公司 | Energy-saving evaporation process and system thereof |
| CN103274960B (en) * | 2013-06-03 | 2014-10-08 | 宁波先安化工有限公司 | Acrylamide crystal continuous concentration device and preparation method thereof |
| CN116877475B (en) * | 2023-09-06 | 2023-11-14 | 浙江镕达永能压缩机有限公司 | Continuous operation method of centrifugal vapor compressor for sugar boiling, evaporating and crystallizing process |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1844086A (en) * | 2006-04-29 | 2006-10-11 | 山东宝莫生物化工股份有限公司 | Process for producing acrylamide crystal |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1844086A (en) * | 2006-04-29 | 2006-10-11 | 山东宝莫生物化工股份有限公司 | Process for producing acrylamide crystal |
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Effective date of registration: 20160323 Address after: 315204 Beihai Road, chemical industry park, Zhenhai District, Ningbo, Zhejiang Patentee after: Zhejiang Hangzhouwan Acrylic Fibres Co.,Ltd. Patentee after: JIANGSU SUNEVAR ENERGY TECHNOLOGY CO.,LTD. Address before: 315204 Beihai Road, chemical industry park, Zhenhai District, Ningbo, Zhejiang Patentee before: Zhejiang Hangzhouwan Acrylic Fibres Co.,Ltd. Patentee before: SHENZHEN SUNEVAP TECHNOLOGY Co.,Ltd. |
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Granted publication date: 20120919 |