CN102580347B - Continuous crystallization method of tetraacetylethylenediamine - Google Patents
Continuous crystallization method of tetraacetylethylenediamine Download PDFInfo
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- CN102580347B CN102580347B CN201210052768.4A CN201210052768A CN102580347B CN 102580347 B CN102580347 B CN 102580347B CN 201210052768 A CN201210052768 A CN 201210052768A CN 102580347 B CN102580347 B CN 102580347B
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Abstract
The invention discloses a continuous crystallization method of tetraacetylethylenediamine. The method is characterized by comprising the following steps that: (a) after the synthesis reaction of tetraacetylethylenediamine is finished, reaction material enters a crystallization pre-cooling kettle, and the temperature of the material is kept at 100-140 DEGE C; (b) the material in the crystallization pre-cooling kettle is conveyed by a crystallization feed pump, mixed with the outer circulation material of a continuous crystallizer and then conveyed by an outer circulation pump 2 of a crystallizer, and enters a continuous crystallizer 1 through a heat exchanger 3; (c) the material in the crystallizer passes through an outer circulation material outlet 2.8 and the outer circulation pump 2 and the heat exchanger 3 to enter the crystallizer from the an outer circulation material inlet 2.9 to finish the outer circulation process; and (d) the material discharged from the crystallization system is conveyed into a centrifugal separation device by a crystallization discharge pump 4 from a crystal mush outlet 2.11, and the obtained solid is washed and dried to obtain the crystal of tetraacetylethylenediamine. Through the method disclosed by the invention, the high-purity pure white tetraacetylethylenediamine product can be directly obtained, continuous crystallization is realized, and the production efficiency and product quality are obviously improved.
Description
Technical field
The present invention relates to a kind of method for crystallising of tetraacetyl ethylene diamine, is more specifically a kind of technique of tetraacetyl ethylene diamine continuous crystallisation, can directly obtain high-purity and coloury tetraacetyl ethylene diamine product.
Background technology
Tetraacetyl ethylene diamine preparation under catalyst exists by diacetyl ethylenediamine and aceticanhydride, in reaction system except containing catalyst, have diacetyl ethylenediamine, triacetyl ethylenediamine and tetraacetyl ethylene diamine, also have a small amount of foreign pigment, make system show brown or brown, after in US Patent No. 4240980, once employing adds the method for active carbon or atlapulgite to decolour, crystallization obtains qualified product; European patent EP 0484634 adopts the method for recrystallization need to refine the crude product of tetraacetyl ethylene diamine, and crude product tetraacetyl ethylene diamine is refined.These operations have all increased equipment investment and the operating cost of producing.
Existing chemical products, when cold crystallization, generally adopt the mode of single still intermittently operated, and the heat transfer efficiency of equipment is low, takies quantity many, and investment is large, and production efficiency is low, and product cut size is controlled difficulty.Common outer circulation continuous crystalizer, although in heat transfer efficiency and production capacity, there is obvious improvement, inner at crystallizer, do not have the parts setting of special strengthening mass transfer, just by outer circulation material import and export position, improve crystallization process.Use existing crystallization kettle, crystallization is slow, and the time is long, and production efficiency is low, and product particle is inhomogeneous, not of uniform size, and color is also bad in addition, has a strong impact on the quality of product.
Summary of the invention
The object of the invention is to overcome the shortcomings and deficiencies that exist in prior art, a kind of continuous crystallisation process of tetraacetyl ethylene diamine is provided, can directly obtain the tetraacetyl ethylene diamine product that high-purity color and luster is pure white, realize continuous crystallisation, significantly improve production efficiency and product quality.
A continuous crystallisation process for tetraacetyl ethylene diamine, is characterized in that, comprises the following steps:
(a) after tetraacetyl ethylene diamine synthetic reaction finishes, reaction mass enters crystallization precooling still, and keeping temperature of charge is 100 ~ 140 ℃;
(b) material in crystallization precooling still is carried by crystallization feed pump, with continuous crystalizer outer circulation mixing of materials, then by crystallizer outer circulation pump 2, is carried, and through heat exchanger 3, enters continuous crystalizer 1;
Described continuous crystalizer 1 comprises upper cover 2.1, outer cylinder body 2.2, lower cone 2.3, low head 2.10; Inner near being provided with an inner cone 2.4 with the connecting portion of upper cover 2.1 at outer cylinder body 2.2, inner cone 2.4 lower edges are connected with inner barrel 2.5; Inner cone 2.4 and inner barrel 2.5 inside are provided with guide shell 2.7; In guide shell 2.7, establish pushing-type agitator 2.6; Below outer cylinder body 2.2 and inner cone 2.4 connecting portions, be provided with outer circulation material outlet 2.8, outer circulation material inlet 2.9 is established in low head 2.10 centres, and outer circulation material inlet 2.9 is provided with sleeve 2.12, and sleeve 2.12 stretches into guide shell 2.7 inside; Low head 2.10 is established magma outlet 2.11 in addition;
(c) the interior material of crystallizer, by outer circulation material outlet 2.8 through outer circulation pump 2, heat exchanger 3, enters crystallizer from outer circulation material inlet 2.9, completes outer circulation process;
(d) crystal system discharging delivers into centrifugal separating device from magma outlet 2.11 via crystallization discharging pump 4, and gained solid obtains tetraacetyl ethylene diamine crystal after washing, being dried.
Further, in step (b), the crystallization temperature of material is controlled by heat exchanger, in the situation that guarantee that the exchange capability of heat of heat exchanger is enough, controlling material temperature after heat exchanger heat exchange is 0 ℃ ~ 50 ℃, is preferably 10 ℃ ~ 20 ℃.
In step (c), in crystallizer, material is 0 ℃ ~ 10 ℃ through the temperature difference before and after heat exchanger, is preferably 2 ℃ ~ 5 ℃.The temperature difference of heat exchanger inlet feed and outlet material can be controlled by controlling the ratio of inlet amount and circulating pump discharging flow.
By controlling feed rate, guarantee the crystallization time of staying of material, and make discharging speed consistent with feed rate, thus the continous-stable of assurance crystallization process.The time of staying of crystallization process is 0.5h ~ 30h, preferably 5h ~ 20h.
In the methods of the invention, the crystallization apparatus of use is mainly comprised of continuous crystalizer, outer circulation pump, heat exchanger, crystallization discharging pump.Continuous crystalizer is by arranging a series of members such as upper pushing-type agitator in internal guide cylinder and guide shell, strengthen mixing and the directed flow of the outer circulation material and the interior material of crystallizer that contain newly to enter material.The rotating speed that is entered the outer circulation inventory of crystallizer and above pushed away stirring by adjusting reaches to be controlled material in outer circulation material and crystallizer and mixes with proper ratio, along guide shell, moves upward.Material moves downward after crossing guide shell upper edge, and after arriving inner barrel lower edge, part enters gap between outer cylinder body and inner barrel and moves upward and arrive outer circulation material outlet, enters in outer circulation material; Leftover materials continue downwards, and part is left crystallizer from magma outlet, and some enters and in guide shell, enters next circulation.The setting of the process inner barrel that material is descending, can make to enter crystal in the material in itself and outer cylinder body space because Action of Gravity Field partly settles down, thereby it is slightly high to make to arrive in the material of outer circulation material outlet stillness of night ratio.The setting of continuous crystalizer internals of the present invention, makes magma except having outer loop, and crystallizer inside has also formed interior circulation, has strengthened the mass transport process in crystallizer.
By controlling of the automatic hierarchy of control, can realize the steady state operation of crystallization process, make process control and all improve significantly at production efficiency and product quality and particle diameter.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of continuous crystallisation device.
Fig. 2 is the structural representation of continuous crystalizer.
Fig. 3 is the top view of continuous crystalizer shown in Fig. 2.
In figure, 1-continuous crystalizer, 2-outer circulation pump, 3-heat exchanger, 4-crystallization discharging pump;
2.1-upper cover, 2.2-outer cylinder body, 2.3-lower cone, 2.4-inner cone, 2.5-inner barrel, 2.6-upper pushing-type stirring, 2.7-guide shell, 2.8-outer circulation material outlet, 2.9-outer circulation material inlet, 2.10-low head, the outlet of 2.11-magma, 2.12-sleeve, 2.13-gusset I, 2.14-gusset II.
Below in conjunction with accompanying drawing, the present invention is described in further detail.
The specific embodiment
Continuous crystallisation device schematic diagram as shown in Figure 1, the structural representation that Fig. 2 is continuous crystalizer, the top view that Fig. 3 is crystallizer.
After tetraacetyl ethylene diamine synthetic reaction finishes, reaction mass enters crystallization precooling still, and the material in crystallization precooling still is carried by crystallization feed pump, with continuous crystalizer outer circulation mixing of materials, then by crystallizer outer circulation pump 2, carried, through heat exchanger 3, enter continuous crystalizer 1.Described continuous crystalizer 1 comprises upper cover 2.1, outer cylinder body 2.2, lower cone 2.3, low head 2.10; Inner near being provided with an inner cone 2.4 with the connecting portion of upper cover 2.1 at outer cylinder body 2.2, inner cone 2.4 lower edges are connected with inner barrel 2.5; Inner cone 2.4 and inner barrel 2.5 inside are provided with guide shell 2.7; In guide shell 2.7, establish pushing-type agitator 2.6; Below outer cylinder body 2.2 and inner cone 2.4 connecting portions, be provided with outer circulation material outlet 2.8, outer circulation material inlet 2.9 is established in low head 2.10 centres, and outer circulation material inlet 2.9 is provided with sleeve 2.12, and sleeve 2.12 stretches into guide shell 2.7 inside; Low head 2.10 is established magma outlet 2.11 in addition;
In crystallizer, material, by outer circulation material outlet 2.8 through outer circulation pump 2, heat exchanger 3, enters crystallizer from outer circulation material inlet 2.9, completes outer circulation process.
Crystal system discharging delivers into centrifugal separating device from magma outlet 2.11 via crystallization discharging pump 4, and gained solid obtains tetraacetyl ethylene diamine crystal after washing, being dried.
Embodiment 1:
After tetraacetyl ethylene diamine synthetic reaction finishes, control 120 ℃ of temperature of charge; Continuous crystalizer volume is 5000L, keeps weight of material 4000kg in continuous crystallisation still; Controlling input and output material speed is 200kg/h, controlled circulation pump discharge 1102kg/h, 2 ℃ of heat exchanger inlet and outlet material temperature difference, 10 ℃ of crystallization temperatures; Centrifugal, washing, the dry crystalline product that obtains; Product adopts HLPC to detect purity, Lab mode detection color and luster.
Embodiment 2
Adjust turnover material speed 400kg/h, controlled circulation pump discharge 22040kg/h, 2 ℃ of heat exchanger inlet and outlet material temperature difference, all the other conditions are with embodiment 1.
Embodiment 3
Control turnover material speed 400kg/h, pump flow 8040kg/h, 5 ℃ of heat exchanger inlet and outlet material temperature difference, 20 ℃ of crystallization temperatures, all the other conditions are with embodiment 1.
Embodiment 4
Control turnover mass flow 800kg/h, pump flow 17680kg/h, 5 ℃ of heat exchanger inlet and outlet material temperature difference, 10 ℃ of crystallization temperatures, all the other conditions are with embodiment 1.
Embodiment 5
Control turnover mass flow 800kg/h, pump flow 16080kg/h, 5 ℃ of heat exchanger inlet and outlet material temperature difference, 20 ℃ of crystallization temperatures, all the other conditions are with embodiment 1.
Embodiment 6(contrast experiment)
React complete temperature of charge and control 120 ℃, directly add 5000L jacketed crystallization kettle, crystallisation by cooling to 20 ℃, insulation 30min; Centrifugal, washing, dry.
Product index is as shown in table 1.
Table 1 product index table
Result surface, adopts the product of the inventive method crystallization to compare purity slightly well with intermittent cooling crystalline product, color and luster obviously better than periodic crystallisation product glossiness, without heterochromatic.
Claims (5)
1. a continuous crystallisation process for tetraacetyl ethylene diamine, is characterized in that, comprises the following steps:
(a) after tetraacetyl ethylene diamine synthetic reaction finishes, reaction mass enters crystallization precooling still, and keeping temperature of charge is 100 ~ 140 ℃;
(b) material in crystallization precooling still is carried by crystallization feed pump, with continuous crystalizer outer circulation mixing of materials, then by crystallizer outer circulation pump (2), is carried, and through heat exchanger (3), enters continuous crystalizer (1);
Described continuous crystalizer (1) comprises upper cover, outer cylinder body, lower cone, low head; Inner barrel is near being provided with an inner cone with the connecting portion of upper cover outside, and inner cone lower edge is connected with inner barrel; Inner cone and inner barrel inside are provided with guide shell; In guide shell, establish pushing-type agitator; Below outer cylinder body and inner cone connecting portion, be provided with outer circulation material outlet, outer circulation material inlet is established in low head centre, and outer circulation material inlet is provided with sleeve, and sleeve stretches into guide shell inside; Low head is established magma outlet in addition;
(c) the interior material of crystallizer, by outer circulation material outlet through outer circulation pump (2), heat exchanger (3), enters crystallizer from outer circulation material inlet, completes outer circulation process;
(d) crystal system discharging delivers into centrifugal separating device from magma outlet via crystallization discharging pump (4), and gained solid obtains tetraacetyl ethylene diamine crystal after washing, being dried.
2. the method for claim 1, is characterized in that, in step (b), material temperature after heat exchanger heat exchange is 0 ℃ ~ 50 ℃.
3. method as claimed in claim 2, is characterized in that, material temperature after heat exchanger heat exchange is 10 ℃ ~ 20 ℃.
4. the method for claim 1, is characterized in that, in step (c), in crystallizer, material is 0 ℃ ~ 10 ℃ through the temperature difference before and after heat exchanger.
5. method as claimed in claim 4, is characterized in that, in crystallizer, material is 2 ℃ ~ 5 ℃ through the temperature difference before and after heat exchanger.
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| CN103537115B (en) * | 2013-10-21 | 2016-05-25 | 西安近代化学研究所 | A kind of crystallization cooler and method thereof that extends the outer circulation type crystallizer operation cycle |
| CN104071761A (en) * | 2014-05-12 | 2014-10-01 | 江苏大明科技有限公司 | Continuous crystallizing and centrifuging system for producing phosphorous acid |
| CN104028002B (en) * | 2014-07-02 | 2016-04-27 | 岳阳市钾盐科学研究所 | Outer circulation air cooling crystallization process equipment |
| CN105233522B (en) * | 2015-10-29 | 2017-06-27 | 中石化南京工程有限公司 | A kind of freezing and crystallizing device |
| CN108164413B (en) * | 2016-12-07 | 2021-09-28 | 上海凯赛生物技术股份有限公司 | Continuous crystallization equipment, system and method for long-chain dibasic acid |
| CN113476885A (en) * | 2021-07-08 | 2021-10-08 | 斯瑞尔环境科技股份有限公司 | Method for continuously producing iron salt crystals |
| CN113975848B (en) * | 2021-11-01 | 2023-05-02 | 安徽相泉化工有限公司 | Continuous cooling crystallization system with external cooler |
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| CN1396113A (en) * | 2002-07-03 | 2003-02-12 | 夏克立 | Process for continuously preparing big-crystal sodium (or potassium) fluosilicate |
| CN2555903Y (en) * | 2002-06-28 | 2003-06-18 | 云南亚太环境工程设计研究有限公司 | Negative pressure ammonium sulfate concentrate crystallizing tank |
| CN1569304A (en) * | 2004-05-08 | 2005-01-26 | 黄晓军 | Apparatus for deposition and crystallization of continuous flow biochemical products |
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| CN2555903Y (en) * | 2002-06-28 | 2003-06-18 | 云南亚太环境工程设计研究有限公司 | Negative pressure ammonium sulfate concentrate crystallizing tank |
| CN1396113A (en) * | 2002-07-03 | 2003-02-12 | 夏克立 | Process for continuously preparing big-crystal sodium (or potassium) fluosilicate |
| CN1569304A (en) * | 2004-05-08 | 2005-01-26 | 黄晓军 | Apparatus for deposition and crystallization of continuous flow biochemical products |
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Address after: Hangzhou Bay Shangyu economic and Technological Development Zone, Shangyu District, Shaoxing City, Zhejiang Province Patentee after: Zhejiang Jinke Daily Chemical New Materials Co.,Ltd. Address before: 312369 Shangyu Industrial Park, Hangzhou Bay, Shaoxing, Zhejiang Patentee before: ZHEJIANG JINKE HOUSEHOLD CHEMICAL MATERIALS Co.,Ltd. |