CN103628087A - Continuous butanedioic acid electrolytic solution crystallization method - Google Patents
Continuous butanedioic acid electrolytic solution crystallization method Download PDFInfo
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- CN103628087A CN103628087A CN201310657657.0A CN201310657657A CN103628087A CN 103628087 A CN103628087 A CN 103628087A CN 201310657657 A CN201310657657 A CN 201310657657A CN 103628087 A CN103628087 A CN 103628087A
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Abstract
The invention discloses a continuous butanedioic acid electrolytic solution crystallization method which comprises the following steps: conveying an electrolytic solution to a cold-hot exchanger, cyclically crystallizing the electrolytic solution automatically flowing into the cold-hot exchanger, gradually releasing crystal substances with temperature reduction, filtering the crystal substances in a vibration filter device, processing one path of mother liquid in a centrifuging drying packaging device through a discharging hole to obtain butanedioic acid, re-circulating the other path of mother liquid to materials of a material dissolving kettle for dissolving, and continuously electrolyzing the mother liquid in an electrolytic tank so as to achieve continuous electrolytic solution crystallization and produce more butanedioic acid. According to the method, high-temperature replacement of the electrolytic solution is fully utilized, the crystallized mother liquid can perform cold-hot exchange by self energy due to low temperature, the continuous butanedioic acid crystallization and the circulating production can be realized, the investment cost is reduced, and the effective volume of an electrolytic reaction is increased.
Description
Technical field
The present invention relates to a kind of crystallization method of succinic acid electrolytic solution, be specifically related to a kind of crystallization method that carries out continuously succinic acid electrolytic solution.
Background technology
Succinic acid is the basic material of various complex organic compounds, is widely used in the industries such as medicine, food, agricultural chemicals, dyestuff and biodegradable material, has wide future develop.Producing at present the producer of succinic acid, is mainly the electrochemical hydrogenation method that is raw material by take along divinyl dicarboxylic anhydride, and its crystallization is the method that the crystallisation by cooling with reactor one still one still filters, and produces succinic acid product.But along with the continuous increase of succinic acid production capacity demand, this traditional crystallization method is produced succinic acid, has the shortcomings such as facility investment is high, throughput is low, maintenance, operational difficulty.
Summary of the invention
The object of the present invention is to provide that a kind of throughput is high, save energy carry out continuously the crystallization method of succinic acid electrolytic solution, the method can realize continous way crystallization succinic acid, can form cyclic production again, save cost of investment, improve electrolytic reaction useful volume.
The present invention carries out the crystallization method of succinic acid electrolytic solution continuously, comprises the steps:
A gets raw material and reacts in material still, and reacted material is delivered in electrolyzer and is carried out electrolysis by the first recycle pump, obtains concentration and be 18% succinic acid electrolytic solution;
B is delivered to the succinic acid electrolytic solution of a step in 5 μ m candle filters 85-97 ℃ of temperature by the second recycle pump, decolours, after the removal of impurity, obtains the succinic acid electrolytic solution after removal of impurities;
C walks b in the succinic acid electrolytic solution input cool-heat-exchanger after removal of impurities, and when temperature drops to 8-12 ℃, succinic acid crystallization generates, and obtains solid-liquid miscellany;
D will carry out solid-liquid separation in the solid-liquid miscellany input solid-liquid concussion separator of c step, and obtaining succinic acid xln and concentration is the electrolytic solution clear liquid of 6.9 %;
E enters dryer by the succinic acid xln of d step again and dries after whizzer, must be dried succinic acid product;
F pumps into cool-heat-exchanger by d one-step electrolysis liquid clear liquid again by the 3rd recycle pump, heating zone by the tubulation in cool-heat-exchanger is heated to 35-45 ℃, mother liquor outlet through cool-heat-exchanger pumps in material still again, with the material in material still, again loop next round and produce, must be dried succinic acid product.
Described filtering core filtering device comprises filter body, and the upper end of filter body is provided with outlet, and lower end is provided with import, and the inside of filter body is provided with filter core, and filter core is provided with feed-pipe, and feed-pipe is connected with import through pipeline; Tensimeter is located on the shell of filter body.
Described cool-heat-exchanger comprises interchanger body, and interchanger body two ends are respectively equipped with electrolyte outlet and electrolytic solution import, interchanger body be provided with the outlet of mother liquor import and mother liquor, the inside of interchanger body is provided with some tubulations.
In aforesaid method, by filtering core filtering device by electrolytic solution decolour, the removal of impurity, improve the quality of crystallisate; By the setting of cool-heat-exchanger, in realization response process, the segmentation of temperature of charge is controlled in cold heat exchanger, progressively generates xln, makes xln uniform particles, surface-area is little, foreign matter content is low; By separator, crystal and liquid are separated, clear body after separation enters cool-heat-exchanger by recycle pump again, after cool-heat-exchanger heats, input again in material still, on the one hand by thermal energy transfer to the electrolytic solution raw material in material still, realize save energy, on the other hand, then carry out circulation crystallization, produce more succinic acid product.
The present invention has following characteristics and advantage:
1, crystallization yield is high, realizes circulation crystallization;
2, good product quality, crystal grain is even;
3, energy consumption is low, saves production cost;
4, labour intensity is low, and level of automation is high.
Accompanying drawing explanation
Fig. 1 is the schema that carries out continuously the crystallization method of succinic acid electrolytic solution of the present invention;
Fig. 2 is the filtering core filtering device structural representation in the present invention;
Cool-heat-exchanger structural representation in Fig. 3 the present invention.
Embodiment
The crystallization method that the present invention is carried out to succinic acid electrolytic solution continuously below in conjunction with accompanying drawing is described further;
From Fig. 1, Fig. 2, Fig. 3, the present invention carries out the crystallization method of succinic acid electrolytic solution continuously, comprises the steps:
A gets raw material and reacts in material still 1, and reacted material is delivered to 3 li, electrolyzer by the first recycle pump 2 and carries out electrolysis, obtains concentration and be 18% succinic acid electrolytic solution;
B is delivered to 5 μ m candle filter 5 li by the succinic acid electrolytic solution of a step 85-97 ℃ of temperature by the second recycle pump 4, decolours, after the removal of impurity, obtains the succinic acid electrolytic solution after removal of impurities;
The succinic acid electrolytic solution that c walks b after removal of impurities is inputted 6 li of cool-heat-exchangers, and when temperature progressively drops to 8-12 ℃, succinic acid crystallization generates, and obtains solid-liquid miscellany;
D walks 7 li of solid-liquid miscellany input solid-liquid concussion separators by c and carries out solid-liquid separation, and obtaining succinic acid xln and concentration is the electrolytic solution clear liquid of 6.9 %;
E enters dryer 10 by the succinic acid xln of d step again and dries after whizzer 9, must be dried succinic acid product;
F pumps into cool-heat-exchanger 6 by d one-step electrolysis liquid clear liquid again by the 3rd recycle pump 8, in the heating zone of the tubulation 66 by 6 li of cool-heat-exchangers, be heated to 35-45 ℃, mother liquor outlet 65 through cool-heat-exchanger 6 pumps into 1 li of material still again, material with 1 li of material still loops next round production again, must be dried succinic acid product.
Described filtering core filtering device 5 comprises filter body 51, and the upper end of filter body 51 is provided with outlet 52, and lower end is provided with import 53, and the inside of filter body 51 is provided with filter core 54, and filter core 54 is provided with feed-pipe 55, and feed-pipe 55 is connected with import 53 through pipeline; Tensimeter 56 is located on the shell 57 of filter body 51.
Described cool-heat-exchanger 6 comprises interchanger body 61, interchanger body 61 two ends are respectively equipped with electrolyte outlet 62 and electrolytic solution import 63, interchanger body 61 be provided with mother liquor import 64 and mother liquor outlet 65, the inside of interchanger body 61 is provided with some tubulations 66.
Embodiment 1:
A gets raw material and reacts in material still 1, and reacted material is delivered to 3 li, electrolyzer by the first recycle pump 2 and carries out electrolysis, obtains concentration and be 18% succinic acid electrolytic solution;
B walks succinic acid electrolytic solution by the second recycle pump 4 by a and is delivered to 5 li of 5 μ m candle filters 85 ℃ of temperature, decolours, after the removal of impurity, obtains the succinic acid electrolytic solution after removal of impurities;
The succinic acid electrolytic solution that c walks b after removal of impurities is inputted cool-heat-exchangers 6 from electrolytic solution import 63, and when temperature progressively drops to 8 ℃, succinic acid crystallization generates, and obtains solid-liquid miscellany;
D walks solid-liquid miscellany by c and carry out solid-liquid separation from electrolyte outlet 62 input solid-liquid concussion separator 7, and obtaining succinic acid xln and concentration is the electrolytic solution clear liquid of 6.9 %;
E enters dryer 10 by the succinic acid xln of d step again and dries after whizzer 9, must be dried succinic acid product;
F pumps into cool-heat-exchanger 6 from mother liquor outlet 64 by d one-step electrolysis liquid clear liquid again by the 3rd recycle pump 8, in the heating zone of the tubulation 66 by 6 li of cool-heat-exchangers, be heated to 35 ℃, mother liquor outlet 65 through cool-heat-exchanger 6 enters 1 li of material still again, material with 1 li of material still loops next round production again, obtains succinic acid product.
Embodiment 2:
A gets raw material and reacts in material still 1, and reacted material is delivered to 3 li, electrolyzer by the first recycle pump 2 and carries out electrolysis, obtains concentration and be 18% succinic acid electrolytic solution;
B is delivered to 5 μ m candle filter 5 li by the succinic acid electrolytic solution of a step 90 ℃ of temperature by the second recycle pump 4, decolours, after the removal of impurity, obtains the succinic acid electrolytic solution after removal of impurities;
The succinic acid electrolytic solution that c walks b after removal of impurities is inputted cool-heat-exchangers 6 from electrolytic solution import 63, and when temperature progressively drops to 10 ℃, succinic acid crystallization generates, and obtains solid-liquid miscellany;
D walks solid-liquid miscellany by c and carry out solid-liquid separation from electrolyte outlet 62 input solid-liquid concussion separator 7, and obtaining succinic acid xln and concentration is the electrolytic solution clear liquid of 6.9 %;
E enters dryer 10 by the succinic acid xln of d step again and dries after whizzer 9, must be dried succinic acid product;
F pumps into cool-heat-exchanger 6 from mother liquor outlet 64 by d one-step electrolysis liquid clear liquid again by the 3rd recycle pump 8, in the heating zone of the tubulation 66 by 6 li of cool-heat-exchangers, be heated to 40 ℃, mother liquor outlet 65 through cool-heat-exchanger 6 enters 1 li of material still again, material with 1 li of material still loops next round production again, obtains succinic acid product.
Embodiment 3:
A gets raw material and reacts in material still 1, and reacted material is delivered to 3 li, electrolyzer by the first recycle pump 2 and carries out electrolysis, obtains concentration and be 18% succinic acid electrolytic solution;
B is delivered to 5 μ m candle filter 5 li by the succinic acid electrolytic solution of a step 97 ℃ of temperature by the second recycle pump 4, decolours, after the removal of impurity, obtains the succinic acid electrolytic solution after removal of impurities;
The succinic acid electrolytic solution that c walks b after removal of impurities is inputted cool-heat-exchangers 6 from electrolytic solution import 63, and when temperature progressively drops to 12 ℃, succinic acid crystallization generates, and obtains solid-liquid miscellany;
D walks solid-liquid miscellany by c and carry out solid-liquid separation from electrolyte outlet 62 input solid-liquid concussion separator 7, and obtaining succinic acid xln and concentration is the electrolytic solution clear liquid of 6.9 %;
E enters dryer 10 by the succinic acid xln of d step again and dries after whizzer 9, must be dried succinic acid product;
F pumps into cool-heat-exchanger 6 from mother liquor outlet 64 by d one-step electrolysis liquid clear liquid again by the 3rd recycle pump 8, in the heating zone of the tubulation 66 by 6 li of cool-heat-exchangers, be heated to 45 ℃, mother liquor outlet 65 through cool-heat-exchanger 6 enters 1 li of material still again, material with 1 li of material still loops next round production again, obtains succinic acid product.
In the present invention, will strictly control the temperature of displacement in the process of the temperature after utilizing the electrolytic solution displacement Crystallization Separation of 85-97 ℃ at 8-12 ℃, temperature is controlled at 1 ℃/1-3min, meanwhile, keeps interchanger 6 liquid level flow velocitys constant; 8 ℃ of following crystallizer succinic acid crystallisate output capacities of crystallization control temperature are high; During centrifugation, adopt after the deionization water at low temperature washing crystal of reverse osmosis membrane processing, obtain the succinic acid crystal that purity is greater than 99.5 %.
Claims (3)
1. carry out continuously a crystallization method for succinic acid electrolytic solution, comprise the steps:
A gets raw material and reacts in material still (1), and reacted material is delivered to by the first recycle pump (2) that electrolyzer (3) is inner carries out electrolysis, obtains concentration and be 18% succinic acid electrolytic solution;
It is inner that b is delivered to 5 μ m candle filters (5) by the succinic acid electrolytic solution of a step 85-97 ℃ of temperature by the second recycle pump (4), decolours, after the removal of impurity, obtains the succinic acid electrolytic solution after removal of impurities;
The succinic acid electrolytic solution input cool-heat-exchanger (6) that c walks b after removal of impurities is inner, and when temperature drops to 8-12 ℃, succinic acid crystallization generates, and obtains solid-liquid miscellany;
D walks the inner solid-liquid separation of carrying out of solid-liquid miscellany input solid-liquid concussion separator (7) by c, and obtaining succinic acid xln and concentration is the electrolytic solution clear liquid of 6.9 %;
E walks succinic acid xln by d and after whizzer (9), enters dryer (10) again and dry, and must be dried succinic acid product;
F pumps into cool-heat-exchanger (6) by d one-step electrolysis liquid clear liquid again by the 3rd recycle pump (8), heating zone by the inner tubulation (66) of cool-heat-exchanger (6) is heated to 35-45 ℃, through the mother liquor outlet (65) of cool-heat-exchanger (6), pump into material still (1) more inner, with the inner material of material still (1), again loop next round and produce, must be dried succinic acid product.
2. the crystallization method that carries out continuously succinic acid electrolytic solution according to claim 1, it is characterized in that: described filtering core filtering device (5) comprises filter body (51), the upper end of filter body (51) is provided with outlet (52), lower end is provided with import (53), the inside of filter body (51) is provided with filter core (54), filter core (54) is provided with feed-pipe (55), and feed-pipe (55) is connected with import (53) through pipeline; Tensimeter (56) is located on the shell (57) of filter body (51).
3. the crystallization method that carries out continuously succinic acid electrolytic solution according to claim 1 and 2, it is characterized in that: described cool-heat-exchanger (6) comprises interchanger body (61), interchanger body (61) two ends are respectively equipped with electrolyte outlet (62) and electrolytic solution import (63), interchanger body (61) be provided with mother liquor import (64) and mother liquor outlet (65), the inside of interchanger body (61) is provided with some tubulations (66).
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2135458C1 (en) * | 1997-12-23 | 1999-08-27 | Государственный научный центр Российской Федерации "НИОПИК" | Method of synthesis of succinic acid |
| CN200985348Y (en) * | 2006-12-26 | 2007-12-05 | 浙江工业大学 | Device without diaphragm for electrolytic synthesis succinic acid |
| CN101100758A (en) * | 2007-06-30 | 2008-01-09 | 浙江工业大学 | Technique and device for non-membrane electrolytic synthesis of butanedioic acid |
| CN101736357A (en) * | 2009-12-31 | 2010-06-16 | 浙江工业大学 | Method for continuous electrolytic synthesis of butanedioic acid |
| CN102877087A (en) * | 2012-11-02 | 2013-01-16 | 福建师范大学 | Method of continuously preparing succinic acid through single ion exchange membrane electrolytic cell based on series overflow |
-
2013
- 2013-12-09 CN CN201310657657.0A patent/CN103628087A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2135458C1 (en) * | 1997-12-23 | 1999-08-27 | Государственный научный центр Российской Федерации "НИОПИК" | Method of synthesis of succinic acid |
| CN200985348Y (en) * | 2006-12-26 | 2007-12-05 | 浙江工业大学 | Device without diaphragm for electrolytic synthesis succinic acid |
| CN101100758A (en) * | 2007-06-30 | 2008-01-09 | 浙江工业大学 | Technique and device for non-membrane electrolytic synthesis of butanedioic acid |
| CN101736357A (en) * | 2009-12-31 | 2010-06-16 | 浙江工业大学 | Method for continuous electrolytic synthesis of butanedioic acid |
| CN102877087A (en) * | 2012-11-02 | 2013-01-16 | 福建师范大学 | Method of continuously preparing succinic acid through single ion exchange membrane electrolytic cell based on series overflow |
Non-Patent Citations (2)
| Title |
|---|
| 万新军等: "单室无隔膜电解槽中恒电流电解合成丁二酸的研究", 《厦门大学学报(自然科学版)》, vol. 44, no. 1, 31 January 2005 (2005-01-31), pages 63 - 66 * |
| 沈海平等: "电解合成丁二酸的研究进展", 《化工进展》, vol. 28, no. 1, 31 December 2009 (2009-12-31), pages 86 - 92 * |
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Application publication date: 20140312 |