CN1123563C - Method for producing acrylamide crystal - Google Patents
Method for producing acrylamide crystal Download PDFInfo
- Publication number
- CN1123563C CN1123563C CN 98126463 CN98126463A CN1123563C CN 1123563 C CN1123563 C CN 1123563C CN 98126463 CN98126463 CN 98126463 CN 98126463 A CN98126463 A CN 98126463A CN 1123563 C CN1123563 C CN 1123563C
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- Prior art keywords
- crystallization kettle
- crystallization
- temperature
- acrylamide
- crystal
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- 239000013078 crystal Substances 0.000 title claims abstract description 26
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- 238000002425 crystallisation Methods 0.000 claims abstract description 49
- 230000008025 crystallization Effects 0.000 claims abstract description 42
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 12
- 239000012452 mother liquor Substances 0.000 claims description 10
- 239000012530 fluid Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 4
- 238000011010 flushing procedure Methods 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 8
- 230000018044 dehydration Effects 0.000 abstract description 5
- 238000006297 dehydration reaction Methods 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 5
- 229920000642 polymer Polymers 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 3
- 239000007864 aqueous solution Substances 0.000 abstract 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000005119 centrifugation Methods 0.000 abstract 1
- 239000002826 coolant Substances 0.000 abstract 1
- 239000012527 feed solution Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 230000008021 deposition Effects 0.000 description 4
- 239000002609 medium Substances 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 239000012736 aqueous medium Substances 0.000 description 1
- -1 carboxylic acids acid amides Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention discloses a preparation method of acrylamide crystals. The main technology of the preparation method is characterized in that concentrated acrylamide aqueous solution is filtered to remove insoluble substances and cooled after entering a cooler, then the concentrated acrylamide aqueous solution successively enters multi-stage cascade connected crystallization kettles to be cooled and crystallized step by step, the temperature gradient between adjacent crystallization kettles and the temperature difference between coolants in crystallization kettles of all levels and feed solution accordingly are controlled, magma is dewatered by centrifugation and dried in fluidized bed drier, and finished products are obtained. The present invention has the characteristics of simple technological process, convenient operation, less investment, low cost, high crystallization ratio, high dehydration rate, no crystal scale formation, no polymer production, high product purity, good quality, etc.
Description
The present invention relates to a kind of by crystallization operation from solution, separate, the technology of purification of carboxylic acids acid amides, especially a kind of manufacture method of acrylamide crystal.
Acrylamide is a kind of important chemical material, and normally reaction generates in aqueous medium for it, and through concentrating, crystallization and drying process and make its crystal product.Because acrylamide in crystallisation process, is formed brilliant dirt and is influenced cooling efficiency at cooling surface easily, even the occluding device pipeline; In drying process, very easily generate polymkeric substance being higher than under 40 ℃ the temperature, therefore in the crystal manufacturing processed, how preventing the crystal fouling and stoping polymerization is a great problem.Chinese patent CN1004658A discloses a kind of " preparation method of acrylamide crystal ", its major technique feature is respectively from the double wall formula that has the electropolishing cooling tube or shell and-tube heat exchanger is inside and outside flows through with acrylamide solution and refrigerant, acrylamide crystal is crystallized out in the electropolishing cooling tube and can not stick on the tube wall, avoided crystalline deposition, fouling and the phenomenon of occluding device.The electropolishing cooling tube is a gordian technique in this processing method, but along with long-term friction, the corrosive nature of material and medium, its surface can be coarse gradually, and effect will obviously descend.And it gives apparatus processing, installs and bring difficulty, and cost also increases relatively.Moreover its percent crystallization in massecuite has only 20～40%, still belongs to level on the low side.And for the crystalline drying, traditional warm air convection drying technology is adopted in all rare both at home and abroad research usually, poor effect, and its quality product is difficult to improve because of containing more polymkeric substance.
Purpose of the present invention just is to overcome above-mentioned weak point of the prior art, provide a kind of technology simple, operation is convenient, apparatus processing is easy, less investment, and production cost and energy consumption are low, percent crystallization in massecuite and dehydration rate are all higher, do not form brilliant dirt and follow-up drying effect is good, do not produce polymkeric substance, the acrylamide crystal manufacture method of quality product excellence.
The objective of the invention is that following technical proposal finishes by implementing: will be through concentrating and weight percent concentration is 40～70%, temperature is to send into the water cooler cooling 40～70 ℃ acrylamide solution is removed insoluble impurity in strainer after, control its material liquid outlet temperature in 20～50 ℃ of scopes, successively enter in the crystallization kettle of plural serial stage crystallisation by cooling step by step, thermograde between each adjacent crystallization kettle is 5～15 ℃, crystallization kettle heat-eliminating mediums at different levels are controlled at 5～20 ℃ with the temperature difference of corresponding feed liquid, and last step crystallization kettle controlled temperature is 3～6 ℃.The magma that comes out from final stage crystallization kettle enters the fluid bed dryer through behind the centrifuge dewatering, uses 50～70 ℃ warm air to carry out drying, and controls temperature of charge at 30～40 ℃, and crystal gets product after the drying.About 1/2～1/4 are pumped to dilution magma and flushing still inwall in the crystallization kettles at different levels in the mother liquor of being discharged by whizzer.For obtaining better technique effect, also can further adopt following measures: above-mentioned multistage crystallization still is the best with three grades; Preferably 10 ℃ of thermogrades between described each adjacent crystallization kettle, the heat-eliminating medium and the corresponding feed liquid temperature difference are preferably 10 ℃ in each crystallization kettle; In the described drying process, the warm air that feeds fluid bed dryer is 65 ℃ is advisable, and the temperature of charge that is dried preferably is controlled at 35 ℃.
Embodiment 1: with weight percent concentration be 60%, temperature be 60 ℃ the acrylamide concentrated solution with 1500 kilograms/time flow deliver to and remove impurity in the strainer, enter the water cooler cooling again, the cooler outlet feed temperature is controlled to be 40 ℃.This feed liquid successively enters in three grades of placed in-line crystallisation by cooling stills crystallisation by cooling step by step.First is controlled at 15 ℃ to the third stage crystallization kettle heat-eliminating medium and the temperature difference of corresponding feed liquid, its feed liquid controlled temperature is respectively 28 ℃, 16 ℃, 4 ℃, the magma that the last step crystallization kettle comes out centrifuge dehydration in whizzer, centrifugal back water ratio is that about 6% wet crystal is put into fluid bed dryer, wherein feed 65 ℃ warm air, temperature of charge is controlled at and carries out drying about 35 ℃, obtains the finished product crystal at last.Mother liquor after centrifugal enters mother liquor tank, wherein about mother liquor of about 1/3 by the mother liquor pump with 700 kilograms/time flow be back to and dilute in each crystallization kettle and wash, its percent crystallization in massecuite reaches 50%., after 20 days equipment is detected with the aforesaid method continuous operation, not finding has crystal incrustation in the crystallization kettle, and not finding has polymer deposition in the fluid bed dryer.Acrylamide finished product crystal content after testing reaches 98.5%, does not find polymkeric substance.
Embodiment 2: with weight percent concentration be 70%, temperature be 70 ℃ the acrylamide concentrated solution with 1000 kilograms/time flow deliver to and remove impurity in the strainer, enter the water cooler cooling again, the cooler outlet feed temperature is controlled to be 50 ℃.This feed liquid successively enters in the placed in-line crystallisation by cooling still of level Four crystallisation by cooling step by step.Crystallization kettle heat-eliminating mediums at different levels are controlled at 20 ℃ with the temperature difference of corresponding feed liquid, and first is respectively 35 ℃, 25 ℃, 15 ℃ to third stage crystallization kettle feed liquid controlled temperature, and last step crystallization kettle temperature is controlled to be 5 ℃.The magma that the last step crystallization kettle comes out centrifuge dehydration in whizzer, centrifugal back water ratio is that about 6% wet crystal is put into fluid bed dryer, wherein feed 60 ℃ warm air, temperature of charge is controlled at and carries out drying about 30 ℃, obtains the finished product crystal at last.Mother liquor after centrifugal enters mother liquor tank, wherein about mother liquor of about 1/2 by the mother liquor pump with 600 kilograms/time flow be back to and dilute in each crystallization kettle and wash, its percent crystallization in massecuite reaches 60%.After 20 days, carry out Equipment Inspection with the aforesaid method continuous operation, do not find crystalline deposition, fouling in the crystallization kettle, fluid bed dryer is interior without any polymer deposition.Acrylamide finished product crystal content after testing reaches 98.6%, does not have polymkeric substance to generate.
Embodiment 3: crystallization, centrifugally operated press embodiment 1 operational path and controlled variable constant, in drying process, the heated drying air temperature is increased to 70 ℃, temperature of charge is controlled at 38 ℃.After moving 20 days as stated above, carrying out Equipment Inspection. without any poly-precious thing, acrylamide crystal finished product content after testing reaches 98.6% in the boiled bed drying machine, does not have polymkeric substance to generate.
The present invention compared with the prior art, it is simple to have technology, operation is convenient, the equipment handling ease, small investment, Production cost and energy consumption are low, and percent crystallization in massecuite and dehydration rate are all high, do not form brilliant dirt and follow-up drying effect is good, do not produce Give birth to the characteristics such as polymer, be applicable to crystallization, the drying of the concentrate that various method for concentration obtain, and its final product Performance optimal, purity height.
Claims (4)
1, a kind of manufacture method of acrylamide crystal, its main technique is: will be 40～70% through concentrated and weight percent concentration, temperature is 40～70 ℃ acrylamide solution is removed insoluble impurity in strainer after, send into cooling in the water cooler, its material liquid outlet temperature is in 20～50 ℃ of scopes, successively enter in the crystallization kettle of plural serial stage crystallisation by cooling step by step, thermograde between each adjacent crystallization kettle is 5～15 ℃, crystallization kettle heat-eliminating mediums at different levels are controlled between 5～20 ℃ with the temperature difference of corresponding feed liquid, last step crystallization kettle controlled temperature is 3～6 ℃, the magma that comes out from final stage crystallization kettle enters the fluid bed dryer through behind the centrifuge dewatering, carry out drying with 50～70 ℃ warm airs, and the control temperature of charge waits to reach and is scheduled to be the crystal finished product after the ridity in 30～40 ℃ of scopes; Extracting 1/2～1/4 in the mother liquor of being discharged by whizzer delivers to and dilutes magma and flushing still wall in the crystallization kettles at different levels.
2, the manufacture method of acrylamide crystal according to claim 1 is characterized in that preferably three grades of series connection crystallization kettles of described plural serial stage crystallization kettle.
3, the manufacture method of acrylamide crystal according to claim 1 and 2 is characterized in that heat-eliminating medium preferably is 10 ℃ with the corresponding feed liquid temperature difference in thermograde between the described adjacent crystallization kettle and each crystallization kettle.
4, the manufacture method of acrylamide crystal according to claim 1, the warm air that it is characterized in that feeding in the fluid bed dryer is advisable with 65 ℃, and the crystal material optimum control temperature that is dried is 35 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98126463 CN1123563C (en) | 1998-12-24 | 1998-12-24 | Method for producing acrylamide crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 98126463 CN1123563C (en) | 1998-12-24 | 1998-12-24 | Method for producing acrylamide crystal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1227221A CN1227221A (en) | 1999-09-01 |
| CN1123563C true CN1123563C (en) | 2003-10-08 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 98126463 Expired - Fee Related CN1123563C (en) | 1998-12-24 | 1998-12-24 | Method for producing acrylamide crystal |
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| Country | Link |
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| CN (1) | CN1123563C (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100334221C (en) * | 2003-12-31 | 2007-08-29 | 江西昌九农科化工有限公司 | Process for preparing acrylamide aqueous solution through direct method cell enzyme reaction |
| CN100339359C (en) * | 2006-04-29 | 2007-09-26 | 山东宝莫生物化工股份有限公司 | Process for producing acrylamide crystal |
| CN101143831B (en) * | 2007-09-20 | 2010-09-08 | 清华大学 | A kind of preparation method of acrylamide crystal |
| CN102786430A (en) * | 2012-07-20 | 2012-11-21 | 江苏南天农科化工有限公司 | Technology for applying airlift stirring to acrylamide crystallization |
| 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 |
| CN110885743A (en) * | 2019-12-31 | 2020-03-17 | 江苏昌九农科化工有限公司 | Acrylamide production process |
-
1998
- 1998-12-24 CN CN 98126463 patent/CN1123563C/en not_active Expired - Fee Related
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| Publication number | Publication date |
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| CN1227221A (en) | 1999-09-01 |
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