CN102311331A - Process for crystallizing chloroacetic acid - Google Patents
Process for crystallizing chloroacetic acid Download PDFInfo
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- CN102311331A CN102311331A CN201110282308A CN201110282308A CN102311331A CN 102311331 A CN102311331 A CN 102311331A CN 201110282308 A CN201110282308 A CN 201110282308A CN 201110282308 A CN201110282308 A CN 201110282308A CN 102311331 A CN102311331 A CN 102311331A
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Abstract
The invention relates to a process for crystallizing chloroacetic acid, which belongs to the fine chemical research field, more specifically provides a technical scheme of a process for producing chloroacetic acid by using acetic acid. The invention is characterized in that a plurality of crystallizers are connected together by intermediate equipment with stirring, when a crystallization solution in a crystallizer reaches a saturated state, a solid-liquid mixture can be introduced from the other crystallizer in time, which is a technical scheme of the process by introducing a certain amount of crystal as a seed crystal to shorten the time of a cooling process and raise the efficiency. The scheme is a safe, environmental and advanced technical scheme. The technical scheme of the present invention is capable of saving the required time from nucleus generation to a value of crystal concentration by the crystallizer, so that the crystallization efficiency can be enhanced.
Description
Technical field
A kind of Mono Chloro Acetic Acid crystalline of the present invention technology belongs to the fine chemistry industry research field, is specifically related to a kind of technical scheme of utilizing the chloroacetic process method of acetic acid production.
Background technology
Utilize acetic acid chlorination method to produce chloroacetic main technique route and have two kinds: a kind of is acetic acid chlorination reaction product; Its compositing range is: the mixture of Mono Chloro Acetic Acid (87.0%～95.0%), dichloro acetic acid (4.0%～10.0%), acetic acid (0.5%～3.0%); Obtain the Mono Chloro Acetic Acid xln through cooling crystallization method; Acetic acid in the mixture, dichloro acetic acid form mother liquor after then can dissolving the part Mono Chloro Acetic Acid, with after liquid-solid the separation, obtain the Mono Chloro Acetic Acid solid phase prod then.Another kind method is to make the dichloro acetic acid hydrodechlorination be reduced to Mono Chloro Acetic Acid through hydrogenating reduction above-mentioned chlorinated mixture, go out acetic acid through rectifying separation again after, then with obtaining solid phase prod behind the fused Mono Chloro Acetic Acid knot sheet.Call crystallization processes to first method, second kind is called hydrogenation technique.
Utilize crystallization processes to produce Mono Chloro Acetic Acid, crystallization processes (preface) is bigger to quality product and production efficiency influence, and the operational requirement of Crystallization Procedure is comparatively strict, and crystallization time is long, and energy consumption is higher.Crystallisation process is that solution is lowered the temperature gradually; Make a certain component in the solution be converted into the process of separating out behind the crystal, be characterized in that from high to low solution can become state of saturation by undersaturated condition with temperature; Arrive supercooled state again; Separate out nucleus gradually in this process, nucleus is grown up gradually afterwards, constantly produces nucleus simultaneously again.Reach capacity or stage of little supercooled state at solution, the nucleus in the solution is rare, and it is not enough that the wall of mold is crossed dynamics cold or that stir; Very easily make nucleus paste the wall growth; In case this type of situation occurs, crystal can gather thicker and thicker on wall, when the heat transfer of wall can't effectively be carried out; Crystallization promptly can't normally go on, and needs recrystallization.Therefore, when solution is about to reach capacity state, the temperature head of wall and solution necessary little extremely to a certain degree (2～4 ℃ generally speaking); When this temperature difference remained to the crystal that q.s is arranged in the solution, temperature head just can strengthen gradually, and the time spent in this stage is longer; Cause whole crystallisation process to use duration, efficient is not high, if when the volume of mold is big; Its surface-area reduces with the ratio of volume relatively, and efficient is then lower.Therefore, when solution reaches state of saturation, in time introduce crystal and then can shorten the time of temperature-fall period, thereby raise the efficiency.Adding crystalline mode has multiple, but from safety, environmental protection and advanced angle, should select a kind of comparatively feasible way for use.
Summary of the invention
The purpose of a kind of Mono Chloro Acetic Acid crystallization processes of the present invention is: produce the problem that exists in the chloroacetic prior art in order to solve above-mentioned employing crystallization processes; The technology that the intermediate equipment that provides one of a kind of usefulness to have stirring links together many molds; When the crystal solution in the mold reaches state of saturation; Can be in time introduce solid-liquid mixtures from other mold, promptly introduce a certain amount of crystal as crystal seed shorten the time of temperature-fall period, the technical scheme of the technology of raising the efficiency.
A kind of Mono Chloro Acetic Acid crystalline of the present invention technology; It is characterized in that be adopt a kind of utilize one have a stirring can prevent the Mono Chloro Acetic Acid crystal deposition in the liquid-solid mixture; The intermediate equipment of fast cooling links together 2～12 molds therein again; When solution in mold or solid-liquid mixtures cool near state of saturation; Crystal solution or solid-liquid mixtures can in time be put the technology in other or several the molds into through intermediate equipment, and the volume of mold is 1: 30～1: 4 with the ratio of the volume of intermediate equipment, and its described intermediate equipment is meant to have and stirs and chuck; Can play threading a pipe of preventing that deposition of solids from can lower the temperature or heat again more, on threading a pipe, be provided with the mouth of pipe more again and be complementary to satisfy to be connected with 2～12 molds.
Above-mentioned a kind of Mono Chloro Acetic Acid crystalline technology is characterized in that and can mold is placed on a plane or be placed on different plane according to flow arrangement, and according to the volume of mold size, difference of altitude h is 0～8 meter scope.
Above-mentioned a kind of Mono Chloro Acetic Acid crystalline technology is characterized in that described mold platform number is 6～8, and the volume size of mold is identical or different all can.
The advantage of a kind of Mono Chloro Acetic Acid crystalline of the present invention technology is: solved existing crystallization processes and produced and have long, the inefficient problem of crystallization time in the chloroacetic technology; The technology that the intermediate equipment that provides one of a kind of usefulness to have stirring is bound up many molds; When the solution in the mold reaches state of saturation; Can be in time introduce the solid-liquid thing, introduce promptly that a certain amount of crystal shortens the temperature-fall period time, the technical scheme of the technology of raising the efficiency from other mold.This scheme is the technical scheme of a kind of safety, environmental protection and advanced person's technology.Adopt technical scheme of the present invention can exempt mold and reach certain to crystal concentration and be worth the needed time, thereby improve crystalline rate from producing nucleus.
Description of drawings
Fig. 1 be equipment layout at conplane process flow diagram, a1, a2 are mold.C is an intermediate equipment.
Fig. 2 arranges synoptic diagram for equipment layout has the process flow diagram of certain height difference and plane facade, and a1, a2, b1 to b6 are mold among the figure, and c is an intermediate equipment.
Embodiment
Embodiment 1
Reference example:
At 10m
3Input content is that the chlorated liquid material amount of 93.6% (wt%) is 6.8m in the mold
3, the density of material is 1.36t/m
3, 74 ℃ that get into from material by the suitable temperature difference in the crystallisation process progressively are cooled to 25 ℃ of blowings, required time is 39 hours, during replenish mother liquor according to solid-liquid in the material than size.
Adopt a DN500, length 2020mm, volume V are 0.38m
3The jacketed intermediate equipment, be placed on same plane with 4, volume is 10m
3The technology that mold links together (like the technology of synoptic diagram 1).The chlorated liquid material amount that in a mold, drops into 93.8% (wt%) is 6.8m
3Identical from 74～59 ℃ of temperature-fall periods with the former, when temperature of charge is 59 ℃, introduce 30 ℃ of liquid-solid mixture 1.5m from other another mold
3But, introduce back material temperature fast cooling to 52 ℃, afterwards by suitable temperature difference cooling, during replenish mother liquor according to solid-liquid in the material than size, 26 hours whole temperature-fall period times spent, when economizing on 13 hours.
Adopt above-mentioned technology, the chlorination liquid measure that is 93.8% (wt%) at a certain mold input content is 6.8m
3, the density of chlorated liquid is 1.36t/m
3, material is identical with the former from 73～59 ℃ of temperature-fall periods in the crystallisation process, when temperature of charge is 59 ℃, introduces 33 ℃ of liquid-solid mixture 2.5m from other mold
3But, introduce back material temperature fast cooling to 50 ℃, afterwards by suitable temperature difference cooling, during replenish mother liquor according to solid-liquid in the material than size, 22 hours whole temperature-fall period times spent, when economizing on 17 hours.
Embodiment 2
Reference example: the employing volume is 12M
3Mold, 93.4% the chlorated liquid material amount of dropping into content and be is 8.3m
3, the density of material is about 1.36t/m
3, 73 ℃ that get into from material by the suitable temperature difference in the crystallisation process progressively are cooled to 25 ℃ of blowings, during to replenish the mother liquor required time according to solid-liquid in the material than size be 43 hours.
Adopt a DN400, length 1550mm, volume V are 0.1gM
3The jacketed intermediate equipment, being placed on a last plane volume with 2 respectively is 5M
3Mold and 3 to be placed on next plane volume be 12M
3The technology that mold links together, two planar difference of altitude are 2.0m, input content is that 93.9% chlorated liquid material amount is 8.5m in following one deck mold
3, the density of material is about 1.38t/m
3, identical with the former from 75～59 ℃ of temperature-fall periods, when temperature of charge was 59 ℃, mold was introduced 33 ℃ of liquid-solid mixture 2.6m from the upper strata
3But, introduce back material temperature fast cooling to about 51.5 ℃, afterwards by suitable temperature difference cooling, during replenish mother liquor according to solid-liquid in the material than size, 25 hours whole temperature-fall period times spent, when economizing on 18 hours.
Embodiment 3
Adopt and experimentize with embodiment 2 identical equipment and technologies.94.1% the chlorated liquid material amount of dropping into content and be is 7.9m
3, the density of material is about 1.36t/m
3, identical from 75～59 ℃ of temperature-fall periods with the former, when temperature of charge is 59 ℃, introduce 28 ℃ of liquid-solid mixture 3.5m from other mold
3But, introduce back material temperature fast cooling to about 48.5 ℃, afterwards by suitable temperature difference cooling, during replenish mother liquor according to solid-liquid in the material than size, 20 hours whole temperature-fall period times spent, when economizing on 23 hours.
Claims (3)
1. Mono Chloro Acetic Acid crystalline technology; It is characterized in that be adopt a kind of utilize one have a stirring can prevent the Mono Chloro Acetic Acid crystal deposition in the liquid-solid mixture; The intermediate equipment of fast cooling links together 2～12 molds therein again; When solution in mold or solid-liquid mixtures cool near state of saturation; Crystal solution or solid-liquid mixtures can in time be put the technology in other or several the molds into through intermediate equipment, and the volume of mold is 1: 30～1: 4 with the ratio of the volume of intermediate equipment, and its described intermediate equipment is meant to have and stirs and chuck; Can play threading a pipe of preventing that deposition of solids from can lower the temperature or heat again more, on threading a pipe, be provided with the mouth of pipe more again and be complementary to satisfy to be connected with 2～12 molds.
2. according to the said a kind of Mono Chloro Acetic Acid crystalline technology of claim 1, it is characterized in that and can mold is placed on a plane or be placed on different plane according to flow arrangement that according to the volume of mold size, difference of altitude h is 0～8 meter scope.
3. according to the said a kind of Mono Chloro Acetic Acid crystalline technology of claim 1, it is characterized in that described mold platform number is 6～8, the volume size of mold is identical or different all can.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110282308A CN102311331A (en) | 2011-09-21 | 2011-09-21 | Process for crystallizing chloroacetic acid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110282308A CN102311331A (en) | 2011-09-21 | 2011-09-21 | Process for crystallizing chloroacetic acid |
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| CN102311331A true CN102311331A (en) | 2012-01-11 |
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| CN201110282308A Pending CN102311331A (en) | 2011-09-21 | 2011-09-21 | Process for crystallizing chloroacetic acid |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102976921A (en) * | 2012-11-30 | 2013-03-20 | 江苏省格林艾普化工股份有限公司 | Chlorinating liquid draining system for chloroacetic acid production |
| CN104326897A (en) * | 2014-11-21 | 2015-02-04 | 河北科技大学 | Continuous crystallization method of chloroacetic acid |
| CN115215741A (en) * | 2021-04-21 | 2022-10-21 | 湖北泰盛化工有限公司 | Quick crystallization and purification process for chloroacetic acid |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1867535A (en) * | 2003-10-16 | 2006-11-22 | 因维斯塔技术有限公司 | Crystallization of adipic acid from its solution in aqueous nitric acid |
-
2011
- 2011-09-21 CN CN201110282308A patent/CN102311331A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1867535A (en) * | 2003-10-16 | 2006-11-22 | 因维斯塔技术有限公司 | Crystallization of adipic acid from its solution in aqueous nitric acid |
Non-Patent Citations (1)
| Title |
|---|
| 石沃陵: "氯乙酸生产中结晶工艺的改进", 《农药》, no. 03, 1980, pages 17 - 18 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102976921A (en) * | 2012-11-30 | 2013-03-20 | 江苏省格林艾普化工股份有限公司 | Chlorinating liquid draining system for chloroacetic acid production |
| CN104326897A (en) * | 2014-11-21 | 2015-02-04 | 河北科技大学 | Continuous crystallization method of chloroacetic acid |
| CN115215741A (en) * | 2021-04-21 | 2022-10-21 | 湖北泰盛化工有限公司 | Quick crystallization and purification process for chloroacetic acid |
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Application publication date: 20120111 |