CN1096288A - The chloroacetic production technique of high purity - Google Patents
The chloroacetic production technique of high purity Download PDFInfo
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- CN1096288A CN1096288A CN 94101326 CN94101326A CN1096288A CN 1096288 A CN1096288 A CN 1096288A CN 94101326 CN94101326 CN 94101326 CN 94101326 A CN94101326 A CN 94101326A CN 1096288 A CN1096288 A CN 1096288A
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Abstract
A kind of high purity preparation process for chloroacetic acid belongs to fine chemistry industry technology category, has mainly solved the Glacial acetic acid chlorination process and has produced the low problem of Mono Chloro Acetic Acid product purity.It is characterized in that in Mono Chloro Acetic Acid crystallization and the mother liquor sepn process, the suction filtration gas that enters separator with low-boiling-point substance that from mother liquor, reclaims in right amount or acetic acid humidification, make that dichloroacetic acid content reduces greatly in the product, then rectifying tower is sent in the Mono Chloro Acetic Acid fusing and removed residual low-boiling-point substance or acetic acid etc., distillation then, condensation, knot sheet can obtain the high-purity chloro acetic acid product.Technology of the present invention has not only guaranteed Mono Chloro Acetic Acid purity 〉=99.0%, and outward appearance is pure white, quality is high, and is suitable for scale operation, easily applies, and economic benefit is very considerable.
Description
The invention provides the chloroacetic technology of a kind of production high purity, belong to fine chemistry industry technology category, specifically is exactly to disclose the chloroacetic preparation technology of a kind of high purity.
As everyone knows, in chloroacetic production process, except that generating Monochloro Acetic Acid, also generate the trichoroacetic acid(TCA) of a certain amount of dichloro acetic acid and trace, wherein dichloro acetic acid is very big to the quality influence of Mono Chloro Acetic Acid product.In existing preparation process for chloroacetic acid, after the chlorated liquid crystallization, put into suction filter, the bed of material is evacuated to dried with vacuum pump, because the content of dichloro acetic acid is up to about 35% in the mother liquor, so be higher than 2.0% with the content that remains in the dichloro acetic acid in the product after mother liquor separates in crystallization, in dry season, the content of dichloro acetic acid is just higher, generally all greater than 3.0%, and in rainy season, atmospheric moisture is big, because Mono Chloro Acetic Acid product suction decreases the content of dichloro acetic acid in product, but now in the technology time of suction filtration oversize, the product water content is raise is difficult to drain, simultaneously because the solubleness of Mono Chloro Acetic Acid in water is very big, product loss is also serious, the more important thing is the quality that can not guarantee the Mono Chloro Acetic Acid product, and purity is difficult to improve.
The objective of the invention is to overcome the shortcoming in the existing preparation process for chloroacetic acid, thereby provide a kind of in Mono Chloro Acetic Acid crystallization and mother liquor sepn process, with the low-boiling-point substance or the acetic acid humidification suction filtration gas that reclaim from mother liquor in right amount, distillation behind the rectifying excision low-boiling-point substance, condensation, knot sheet promptly obtain the chloroacetic novel process of high purity then.
High purity preparation process for chloroacetic acid of the present invention, with the Glacial acetic acid chlorinated with chlorine, the chlorated liquid crystallization, after crystal solution is cooled to 20-25 °, crystallization mixture is put into separator separates, it is characterized in that when the Mono Chloro Acetic Acid crystallization separates with mother liquor, enter the gas of strainer with low-boiling-point substance that reclaims in an amount of mother liquor or acetic acid humidification, remove the dichloro acetic acid of carrying secretly in the Mono Chloro Acetic Acid product, make dichloroacetic acid content reduce to≤0.5%(wt), then watery fusion is sent into residual low-boiling-point substance or the acetic acid of rectification under vacuum tower excision, make its content reduce to≤0.3%, then kettle base solution is sent into the finishing column distillation, steams thing and condenses to 70-80 ℃ of high-purity chloro acetic acid product that send flaker can obtain purity 〉=99.0% in flakes.
High-purity chloro acetic acid production technological process of the present invention can be divided into four-stage:
Fs: with Glacial acetic acid chlorination under the condition that SULPHUR POWDER exists, after the chlorated liquid crystallization, solidliquid mixture is put into the anticorrosion separator (strainer) of special band heating jacket, first suction filtration 2-3 hour, makes most mother liquor filterings.
Subordinate phase: use and account for the low-boiling-point substance that from mother liquor, reclaims of bed of material weight 2-20% or the gas that the acetic acid humidification enters strainer, and suction filtration 6-8 hour again.
Phase III: the stop suction filtration, close bleeder valve, in the strainer chuck, feed steam heating, make bed of material fusing, send rectifying tower excision low-boiling-point substance or acetic acid, make content≤0.3% of its low-boiling-point substance or acetic acid.
The quadravalence section: the product behind excision low-boiling-point substance or the acetic acid is sent into finished product and is steamed tower and steam, steam thing through condenser condenses to 70-80 ℃ of high-purity chloro acetate finished product that send flaker promptly to obtain purity 〉=99.0% in flakes.
High purity preparation process for chloroacetic acid of the present invention, owing in crystallization product suction filtration process, adopt recovery low-boiling-point substance or acetic acid humidification to enter the gas of strainer, the dichloro acetic acid of carrying secretly in the product is reduced greatly, adopt simultaneously rectification under vacuum excision low-boiling-point substance or acetic acid make its content in product be reduced to≤0.3%, and shortened the suction filtration time, the ton product 100-150 degree that can economize on electricity, and reduced the water-content in the product; Then product steams tower by finished product and all steams, steam thing and arrive 70-80 ℃ through condenser condenses, send flaker in blocks, thoroughly like this removed inorganic impurity and the carbide in the product, make product appearance pure white, flaked product is compared with crystalline particle shape product in addition, its specific surface area reduces greatly, this has just reduced the water regain of product in packing and transportation, guarantee the quality of product, can realize that packing is semi-automatic simultaneously again, reduced working strength of workers, improve work situation, make production of chloroacetic acid be suitable for scale operation.
Embodiment 1,
Get chlorated liquid 700g, consist of: Monochloro Acetic Acid 91.43%, dichloro acetic acid 7.15%, acetate 1.41%, join mother liquor 350g, crystallization in super Water Tank with Temp.-controlled, crystal solution adds a small amount of kind when reducing to 45 ℃, uniform decrease in temperature to 20 ℃ crystallization under agitation finishes, then crystal solution is changed in the strainer, first suction filtration one hour, it consists of: Monochloro Acetic Acid 94.6%, dichloro acetic acid 2.55%, acetate 2.85% is used 20% low-boiling-point substance humidification suction filtration gas of bed of material weight then, takes out 4 hours again, surveying it consists of: Monochloro Acetic Acid 94.94%, dichloro acetic acid 0.21%, acetate 4.85% is with this solid phase prod fusing, add in the distilling flask, decompression excision acetate on the filling extract rectification post, cut acetate after, group of products becomes at the bottom of the still: Monochloro Acetic Acid 99.6%, dichloro acetic acid 0.22%, acetate 0.18%, kettle base solution under reduced pressure all steams, and is condensed to 70-80 ℃ of knot sheet, get pure white high-purity chloro acetic acid product 575g, Monochloro Acetic Acid content is 99.6%.
Embodiment 2,
Add Glacial acetic acid in reactor, use chlorinated with chlorine about 100 ℃, after chlorination finished, chlorated liquid was sent into the crystallizer crystallization, and crystal solution is cooled to 25 ℃ of crystallizations and finishes.Solidliquid mixture is put into the special strainer that scribbles impregnating material, elder generation's suction filtration 3 hours, make most mother liquor filterings, enter the gas of strainer then with 2% the acetic acid humidification that accounts for the bed of material, suction filtration is 8 hours again, the stop suction filtration, close bleeder valve, in the strainer chuck, feed steam heating, make bed of material fusing, send rectifying tower excision acetic acid, make and contain acetic acid amount≤0.3% in the product, the product of excision behind the acetic acid sent into finished product and steamed tower and steam, and steams thing and ℃ delivers to flaker knot sheet through condenser condenses to 70, can obtain purity and be the high-purity chloro acetic acid product more than 99.0%.
Claims (2)
1, a kind of high purity preparation process for chloroacetic acid, with the Glacial acetic acid chlorinated with chlorine, the chlorated liquid crystallization, after crystal solution is cooled to 20-25 °, crystallization mixture is put into separator separates, it is characterized in that when the Mono Chloro Acetic Acid crystallization separates with mother liquor, enter the gas of strainer with low-boiling-point substance that reclaims in an amount of mother liquor or acetic acid humidification, remove the dichloro acetic acid of carrying secretly in the Mono Chloro Acetic Acid product, then watery fusion is sent into residual low-boiling-point substance or the acetic acid of rectification under vacuum tower excision, then kettle base solution is sent into finished product and is steamed column distillation, steam the thing condensation after, through the knot sheet can obtain the high-purity chloro acetic acid product.
2, according to the described a kind of high purity preparation process for chloroacetic acid of claim 1, it is characterized in that concrete preparation process can be divided into four-stage:
Fs: after the Glacial acetic acid chlorination, the chlorated liquid crystallization, the solidliquid mixture after the crystallization is put into the anticorrosion strainer of special band heating jacket, takes out earlier 2-3 hour, makes most mother liquor filterings.
Subordinate phase: use and account for the low-boiling-point substance that from mother liquor, reclaims of bed of material weight 2-20% or the gas that the acetic acid humidification enters strainer, and suction filtration 6-8 hour again.
Phase III: the stop suction filtration, close bleeder valve, in the strainer chuck, feed steam heating, make bed of material fusing, send rectifying tower excision low-boiling-point substance or acetic acid.
The quadravalence section: the still liquid of excision low-boiling-point substance or acetic acid, send into finished product and steam tower and steam, steam thing and condense to 70-80 ℃, send flaker knot sheet, promptly obtain the high-purity chloro acetate finished product of purity 〉=99.0%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94101326 CN1033450C (en) | 1994-02-03 | 1994-02-03 | High-purity chloric acid producing tech. |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94101326 CN1033450C (en) | 1994-02-03 | 1994-02-03 | High-purity chloric acid producing tech. |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1096288A true CN1096288A (en) | 1994-12-14 |
| CN1033450C CN1033450C (en) | 1996-12-04 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 94101326 Expired - Fee Related CN1033450C (en) | 1994-02-03 | 1994-02-03 | High-purity chloric acid producing tech. |
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| CN (1) | CN1033450C (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101575281A (en) * | 2009-06-24 | 2009-11-11 | 何正� | Chloroacetic acid producing method and reaction equipment thereof |
| CN102838472A (en) * | 2012-10-08 | 2012-12-26 | 江苏省格林艾普化工股份有限公司 | Mother liquor emergency production process for crystallizing in chloroactic acid industrial production |
| CN104326897A (en) * | 2014-11-21 | 2015-02-04 | 河北科技大学 | Continuous crystallization method of chloroacetic acid |
| CN105949051A (en) * | 2016-05-23 | 2016-09-21 | 河南红东方化工股份有限公司 | Crystalizing process of chloroacetic acid |
-
1994
- 1994-02-03 CN CN 94101326 patent/CN1033450C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101575281A (en) * | 2009-06-24 | 2009-11-11 | 何正� | Chloroacetic acid producing method and reaction equipment thereof |
| CN101575281B (en) * | 2009-06-24 | 2013-05-29 | 何正� | Chloroacetic acid producing method and reaction equipment thereof |
| CN102838472A (en) * | 2012-10-08 | 2012-12-26 | 江苏省格林艾普化工股份有限公司 | Mother liquor emergency production process for crystallizing in chloroactic acid industrial production |
| CN104326897A (en) * | 2014-11-21 | 2015-02-04 | 河北科技大学 | Continuous crystallization method of chloroacetic acid |
| CN105949051A (en) * | 2016-05-23 | 2016-09-21 | 河南红东方化工股份有限公司 | Crystalizing process of chloroacetic acid |
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| Publication number | Publication date |
|---|---|
| CN1033450C (en) | 1996-12-04 |
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