CN105130786A - Method for preparing high purity chloroacetic acid by gap method - Google Patents
Method for preparing high purity chloroacetic acid by gap method Download PDFInfo
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- CN105130786A CN105130786A CN201510452809.2A CN201510452809A CN105130786A CN 105130786 A CN105130786 A CN 105130786A CN 201510452809 A CN201510452809 A CN 201510452809A CN 105130786 A CN105130786 A CN 105130786A
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- acetic acid
- mono chloro
- chloroacetic
- chloro acetic
- crystal grain
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/347—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups
- C07C51/363—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups by introduction of halogen; by substitution of halogen atoms by other halogen atoms
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- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for preparing high purity chloroacetic acid by a gap method. The method comprises that glacial acetic acid and chlorine undergo a reaction to produce a reaction product containing chloroacetic acid, dichloroacetic acid and hydrochloric acid, the reaction product is cooled to form chloroacetic acid crystal particles, the chloroacetic acid crystal particles are heated to a temperature of 35-38 DEG C by supersaturated steam so that the dichloroacetic acid by-product adsorbed by the surfaces of the chloroacetic acid crystal particles is melt, and a solid-liquid separation process is carried out by a centrifuge so that high purity chloroacetic acid is obtained. The method has a reasonable technical design, a small equipment investment, low energy consumption, easily controllable processes and a high yield, adopts an optimized method to remove dichloroacetic acid impurities on the chloroacetic acid surface, can prepare high-quality chloroacetic acid with purity of 99.50-99.99%, has a high application value, solves the problems of prior art and has good technical effects.
Description
Technical field
The present invention relates to a kind of preparation method of chemical reagent, it is controlled to be specifically related to a kind of technique, adopts the chloroacetic method of gap method manufacture high purity.Belong to chemical industrial field
Technical background
Chlorine and acetic acidreaction produce chloroacetic industrial technology step, chlorine and acetic acidreaction generate Mono Chloro Acetic Acid and hydrogen chloride gas, but can by-product dichloroacetic acid be produced in reaction process, wherein Mono Chloro Acetic Acid becomes solution shape with dichloro acetic acid, mix, during separation, dichloro acetic acid is very easily adsorbed on the surface of Mono Chloro Acetic Acid crystal, causes normal Mono Chloro Acetic Acid purity of producing can only about 95 ~ 97%, do not reach high purity requirement, limit it and apply.
Summary of the invention
Goal of the invention: the object of the invention is the deficiency existed to solve prior art, there is provided a kind of technological design reasonable, steady quality, energy consumption is low, fully can remove the by-product dichloroacetic acid in Mono Chloro Acetic Acid, prepare the high purity that purity is 99.50 ~ 99.99%, the chloroacetic preparation method of high-quality.
Technical scheme: in order to realize above object, the technical scheme that the present invention takes is:
A kind of chloroacetic method of gap method manufacture high purity, it comprises the following steps:
(1) get reaction vessel, add glacial acetic acid, then pass into chlorine, reaction prepares containing Mono Chloro Acetic Acid, the reaction product of dichloro acetic acid and hydrochloric acid;
(2) get the reaction product of step (1), place cooling, obtained Mono Chloro Acetic Acid crystal grain;
(3) the Mono Chloro Acetic Acid crystal grain that step (2) is obtained is got, use supersaturated vapor heating Mono Chloro Acetic Acid crystal grain to 35 ~ 38 DEG C, make the dichloro acetic acid by product fusing being adsorbed on Mono Chloro Acetic Acid crystal grain surface, then solid-liquid separation is carried out with whizzer, by-product dichloroacetic acid enters into parting liquid in the lump with liquid, and prepares highly purified Mono Chloro Acetic Acid;
(4) get step (3) and be separated the parting liquid obtained, continue to place cooling, make the Mono Chloro Acetic Acid crystallization again of partial melting, then continue to use supersaturated vapor heating Mono Chloro Acetic Acid crystal grain to 35 ~ 38 DEG C, make the dichloro acetic acid by product fusing being adsorbed on Mono Chloro Acetic Acid crystal grain surface, and then carry out solid-liquid separation with whizzer, reduce the quantity of by product, prepare the crystallizing chloroacetic acid that purity is high.
Preferably, the chloroacetic method of above-described gap method manufacture high purity, Mono Chloro Acetic Acid crystal grain obtained in step (3), uses supersaturated vapor in 5 ~ 30 seconds, and heating Mono Chloro Acetic Acid crystal grain is to 35 DEG C.The present invention filters out best processing step by great many of experiments, adopt supersaturated vapor in 5 ~ 30 seconds rapid heating Mono Chloro Acetic Acid crystal grain to 35 DEG C, the dichloro acetic acid amount impurity being adsorbed on crystallizing chloroacetic acid surface can be effectively made fully to dissolve and principal product can not be made to dissolve in a large number, adopt high speed centrifugation method, effectively remove dichloro acetic acid by product, thus obtain highly purified Mono Chloro Acetic Acid, achieve extraordinary technique effect.
Preferably, the chloroacetic method of above-described gap method manufacture high purity, in step (1), the mole dosage ratio of glacial acetic acid and chlorine is 1; 1 ~! : 2, temperature of reaction is 30 ~ 60 degree, and the reaction times is 30 ~ 60 minutes.
Preferably, the chloroacetic method of above-described gap method manufacture high purity, is characterized in that, carries out crystallisation by cooling under step (2) and step (4) are placed on-5 ~ 5 degree.The present invention filters out the temperature of best crystallisation by cooling by great many of experiments, can make Mono Chloro Acetic Acid sufficient crystallising, and the dichloro acetic acid amount of carrying secretly is minimum, can improve purification efficiency, improves Mono Chloro Acetic Acid purity.
Preferably, the chloroacetic method of above-described gap method manufacture high purity, in step (3), whizzer carries out the centrifugal speed of solid-liquid separation is 10000 ~ 15000 revs/min.
Preferably, the chloroacetic method of above-described gap method manufacture high purity, the chloroacetic purity that step (3) and step (4) prepare is 99.50 ~ 99.99%.
Compared to the prior art, the present invention has the following advantages:
The present invention screens the chloroacetic method of gap method manufacture high purity obtained by great many of experiments, whole technological design is reasonable, and facility investment is little, and energy consumption is low, and production process is easy to control, and productive rate is high.
Be crystal grain after reacting the Mono Chloro Acetic Acid cooling prepared, dichloro acetic acid is liquid, but dichloro acetic acid by product is firmly adsorbed on Mono Chloro Acetic Acid grain surface in crystallisation process, existing isolation technique is difficult to by dichloro acetic acid separation of by-products out, the present invention removes the method for impurity dichloro acetic acid by great many of experiments screening, adopt first crystallisation by cooling, then hot steam is adopted within 30 second short period of time, to heat rapidly Mono Chloro Acetic Acid crystal grain to 35 ~ 38 DEG C, then ultracentrifugal method is adopted rapidly, remove the dichloro acetic acid of Mono Chloro Acetic Acid grain surface, the high-quality Mono Chloro Acetic Acid of high purity 99.50 ~ 99.99% can be prepared, using value is high, thus the technical deficiency of prior art can be solved, achieve extraordinary technique effect.
Specific implementation method
Below in conjunction with specific embodiment, illustrate the present invention further, these embodiments should be understood only be not used in for illustration of the present invention and limit the scope of the invention, after having read the present invention, the amendment of those skilled in the art to the various equivalent form of value of the present invention has all fallen within the application's claims limited range.
Embodiment 1
1. the chloroacetic method of gap method manufacture high purity, it comprises the following steps:
(1) get reaction vessel, add 1 mole of glacial acetic acid, then pass into 2 moles of chlorine, 35 degree of reactions 40 minutes, prepare containing Mono Chloro Acetic Acid, the reaction product of dichloro acetic acid and hydrochloric acid;
(2) get the reaction product of step (1), cool at being placed on-4 DEG C, obtained Mono Chloro Acetic Acid crystal grain;
(3) the Mono Chloro Acetic Acid crystal grain that step (2) is obtained is got, supersaturated vapor is used in 30 seconds, to heat rapidly Mono Chloro Acetic Acid crystal grain to 35 DEG C, make the dichloro acetic acid by product fusing being adsorbed on Mono Chloro Acetic Acid crystal grain surface, then under 15000 revs/min of high speeds, solid-liquid separation is carried out with whizzer rapidly, by-product dichloroacetic acid enters into parting liquid in the lump with liquid, and prepares highly purified Mono Chloro Acetic Acid; Detected result shows that Mono Chloro Acetic Acid purity is 99.96%.
(4) get step (3) and be separated the parting liquid obtained, cool at continuing to be placed on-4 DEG C, make the Mono Chloro Acetic Acid crystallization again of partial melting, then continue to use supersaturated vapor heating Mono Chloro Acetic Acid crystal grain to 35 DEG C, make the dichloro acetic acid by product fusing being adsorbed on Mono Chloro Acetic Acid crystal grain surface, and then carry out solid-liquid separation with whizzer, reduce the quantity of by product, prepare the crystallizing chloroacetic acid that purity is high.Detected result shows that Mono Chloro Acetic Acid purity is 99.92%.
Embodiment 2
1. the chloroacetic method of gap method manufacture high purity, it comprises the following steps:
(1) get reaction vessel, add 1 mole of glacial acetic acid, then pass into 1 mole of chlorine, 60 degree of reactions 50 minutes, prepare containing Mono Chloro Acetic Acid, the reaction product of dichloro acetic acid and hydrochloric acid;
(2) get the reaction product of step (1), cool at being placed on-5 DEG C, obtained Mono Chloro Acetic Acid crystal grain;
(3) the Mono Chloro Acetic Acid crystal grain that step (2) is obtained is got, supersaturated vapor is used to heat rapidly Mono Chloro Acetic Acid crystal grain at 30 seconds to 38 DEG C, make the dichloro acetic acid by product fusing being adsorbed on Mono Chloro Acetic Acid crystal grain surface, then under 10000 revs/min of high speeds, solid-liquid separation is carried out with whizzer rapidly, by-product dichloroacetic acid enters into parting liquid in the lump with liquid, and prepares highly purified Mono Chloro Acetic Acid; Detected result shows that Mono Chloro Acetic Acid purity is 99.8%.
(4) get step (3) and be separated the parting liquid obtained, cool at continuing to be placed on-5 DEG C, make the Mono Chloro Acetic Acid crystallization again of partial melting, then continue to use supersaturated vapor heating Mono Chloro Acetic Acid crystal grain to 38 DEG C, make the dichloro acetic acid by product fusing being adsorbed on Mono Chloro Acetic Acid crystal grain surface, and then carry out solid-liquid separation with whizzer, reduce the quantity of by product, prepare the crystallizing chloroacetic acid that purity is high.Detected result shows that Mono Chloro Acetic Acid purity is 99.94%.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (6)
1. the chloroacetic method of gap method manufacture high purity, is characterized in that, comprise the following steps:
(1) get reaction vessel, add glacial acetic acid, then pass into chlorine, reaction prepares containing Mono Chloro Acetic Acid, the reaction product of dichloro acetic acid and hydrochloric acid;
(2) get the reaction product of step (1), place cooling, obtained Mono Chloro Acetic Acid crystal grain;
(3) the Mono Chloro Acetic Acid crystal grain that step (2) is obtained is got, use supersaturated vapor heating Mono Chloro Acetic Acid crystal grain to 35 ~ 38 DEG C, make the dichloro acetic acid by product fusing being adsorbed on Mono Chloro Acetic Acid crystal grain surface, then solid-liquid separation is carried out with whizzer, by-product dichloroacetic acid enters into parting liquid in the lump with liquid, and prepares highly purified Mono Chloro Acetic Acid;
(4) get step (3) and be separated the parting liquid obtained, continue to place cooling, make the Mono Chloro Acetic Acid crystallization again of partial melting, then continue to use supersaturated vapor heating Mono Chloro Acetic Acid crystal grain to 35 ~ 38 DEG C, make the dichloro acetic acid by product fusing being adsorbed on Mono Chloro Acetic Acid crystal grain surface, and then carry out solid-liquid separation with whizzer, reduce the quantity of by product, prepare the crystallizing chloroacetic acid that purity is high.
2. the chloroacetic method of gap method manufacture high purity according to claim 1, is characterized in that, Mono Chloro Acetic Acid crystal grain obtained in step (3), uses supersaturated vapor in 30 seconds, to heat rapidly Mono Chloro Acetic Acid crystal grain to 35 DEG C.
3. the chloroacetic method of gap method manufacture high purity according to claim 1, is characterized in that, in step (3), whizzer carries out the centrifugal speed of solid-liquid separation is 10000 ~ 15000 revs/min.
4. the chloroacetic method of gap method manufacture high purity according to claim 1, is characterized in that, in step (1), the mole dosage ratio of glacial acetic acid and chlorine is 1; 1 ~! : 2, temperature of reaction is 30 ~ 60 degree, and the reaction times is 30 ~ 60 minutes.
5. the chloroacetic method of gap method manufacture high purity according to any one of Claims 1-4, is characterized in that, carry out crystallisation by cooling under step (2) and step (4) are placed on-5 ~ 5 degree.
6. the chloroacetic method of gap method manufacture high purity according to any one of claim 5, it is characterized in that, the chloroacetic purity that step (3) and step (4) prepare is 99.50 ~ 99.99%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510452809.2A CN105130786A (en) | 2015-07-28 | 2015-07-28 | Method for preparing high purity chloroacetic acid by gap method |
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| CN201510452809.2A CN105130786A (en) | 2015-07-28 | 2015-07-28 | Method for preparing high purity chloroacetic acid by gap method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017135833A1 (en) * | 2016-02-04 | 2017-08-10 | Pcc Mcaa Sp. Z O.O. | Method of producing high-purity monochloroacetic acid |
| US10494325B2 (en) | 2016-02-04 | 2019-12-03 | Pcc Mcaa Sp. Z O. O. | Method of industrially producing monochloroacetic acid |
-
2015
- 2015-07-28 CN CN201510452809.2A patent/CN105130786A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 李福祥等: "氯乙酸生产技术进展及其未来的发展方向", 《氯碱工业》 * |
| 杨义谟: "动态熔融结晶工艺", 《辽宁化工》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017135833A1 (en) * | 2016-02-04 | 2017-08-10 | Pcc Mcaa Sp. Z O.O. | Method of producing high-purity monochloroacetic acid |
| CN108602747A (en) * | 2016-02-04 | 2018-09-28 | Pcc慕卡有限公司 | The method for producing high-purity chloroacetic acid |
| US10494325B2 (en) | 2016-02-04 | 2019-12-03 | Pcc Mcaa Sp. Z O. O. | Method of industrially producing monochloroacetic acid |
| US10538474B2 (en) | 2016-02-04 | 2020-01-21 | Pcc Mcaa Sp. Z O. O. | Method of producing high-purity monochloroacetic acid |
| CN108602747B (en) * | 2016-02-04 | 2021-10-12 | Pcc Mcaa 有限公司 | Method for producing high-purity monochloroacetic acid |
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Application publication date: 20151209 |