CN102516112A - Preparation method for chromatographic grade N,N-dimethyl formamide - Google Patents
Preparation method for chromatographic grade N,N-dimethyl formamide Download PDFInfo
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- CN102516112A CN102516112A CN2011104409521A CN201110440952A CN102516112A CN 102516112 A CN102516112 A CN 102516112A CN 2011104409521 A CN2011104409521 A CN 2011104409521A CN 201110440952 A CN201110440952 A CN 201110440952A CN 102516112 A CN102516112 A CN 102516112A
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Abstract
The present invention relates to a preparation method for chromatographic grade N,N-dimethyl formamide. The method comprises the following steps that: (1) a raw material N,N-dimethyl formamide flows through a calcium hydroxide adsorption column; (2) the N,N-dimethyl formamide after the adsorption and alumina are subjected to vacuum distillation, wherein the distillation is performed under a condition of 5-10 mmHg; (3) the distilled liquid is filtered by using a 0.45 mum microporous filtration membrane, and is subjected to bottling and storing through nitrogen filling to obtain the chromatographic grade N,N-dimethyl formamide. According to the present invention, the N,N-dimethyl formamide with the content of about 99.5% is adopted as the raw material, the calcium hydride column is adopted to adsorb the water and other impurities in the N,N-dimethyl formamide, the alumina is adopted to presinter to the temperature of 500-600 DEG C, and the vacuum distillation treatment is performed, such that the N,N-dimethyl formamide product with the purity more than 99.9% is prepared through the treatments of adsorbing, drying, and vacuum distillation, and the product can meet the chromatographic grade (HPLC) N,N-dimethyl formamide application requirements of the user.
Description
Technical field:
The invention belongs to chemical technology field, relate to the preparation method of organic solvent, especially a kind of chromatographic grade N, the preparation method of dinethylformamide.
Background technology:
N, dinethylformamide are most widely used amide solvents, use reagent like nonaqueous titration, the solvent of ethenoid resin and acetylene; Organic synthesis, photometry, gc stationary liquid; Compartment analysis C2-C5 hydrocarbon; Just separate, iso-butylene-[1] and suitable, anti-butylene-[2]; Pesticide residue analysis; Organic synthesis etc.But commercially available N, dinethylformamide reagent content is merely about 99.5%, and major impurity is impurity such as water and micro ethanol, primary amine, secondary amine.Because ultraviolet absorptivity is high, can not satisfy the needs of related scientific research test, so this kind N, dinethylformamide must pass through further preparation, and making its each item technical indicator all reach high-purity chromatographic grade index can use.
At present, domestic about high-purity chromatographic grade N, the data that dinethylformamide prepares the aspect seldom, in order to remove N, small amount of impurities in the dinethylformamide the present invention is directed to this technical barrier, proposes effective solution.
Summary of the invention:
The objective of the invention is to overcome the weak point of prior art, the chromatographic grade N that a kind of method is simple, impurity is easily separated, product purity is high is provided, the preparation method of dinethylformamide.
The present invention realizes that the technical scheme of purpose is:
A kind of chromatographic grade N, the preparation method of dinethylformamide, step is following:
(1) with raw material N, dinethylformamide is through being equipped with the adsorption column of sorbent material, flow velocity 50mL/min～140mL/min;
(2) absorption fluid in the step (1) is squeezed into still kettle, the adding weight ratio is 5～20% aluminum oxide in the still, 500～600 ℃ of pre-burnings, about 1-2 of time hour, underpressure distillation under 5～10mmHg pressure;
(3) with distillation fluid warp 0.45 μ m filtering with microporous membrane, bottling in the step (2), inflated with nitrogen is preserved, and promptly gets chromatographic grade N, dinethylformamide.
And the sorbent material of described step (1) is the hydrolith of particle diameter 5mm～15mm.
And the dress post amount of the hydrolith of described step (1) is 4/5 of a column length.
And, 500～600 ℃ of the aluminum oxide elder generation pre-burnings of said step (2), about 1-2 of time hour.
And, said step (2) N, the weight ratio of dinethylformamide and aluminum oxide is 5～20%.
Advantage of the present invention and positively effect are:
1, the present invention is about 99.5% N with content; Dinethylformamide is raw material, adsorbs impurity such as water wherein with the hydrolith post, adopts 500～600 ℃ of aluminum oxide pre-burnings, underpressure distillation together then; Through absorption, drying, underpressure distillation, to prepare purity be 99.9% N; The dinethylformamide product, its each item index meets chromatographic grade N, the requirement of dinethylformamide.
2, this preparation method promotes N; Dinethylformamide content; From about 99.5% to 99.9%, yield rate is increased to more than 90% by original 75%, method is simple, impurity is easily separated, product purity is high, stable, reduce energy consumption; More be applicable to suitability for industrialized production, have remarkable economic efficiency.
3, the product of this preparation method production is through detecting, and its N, dinethylformamide content are greater than 99.9%, and the recovery is greater than 94%, and yield rate reaches 95%, can satisfy chromatographic grade (HPLC) N, dinethylformamide user's application demand.
Embodiment:
Through specific embodiment the present invention is made further detailed description below, following examples are descriptive, are not determinate, can not limit protection scope of the present invention with this.
Embodiment 1
A kind of chromatographic grade N, the preparation method of dinethylformamide, step is following:
(1) with raw material N, dinethylformamide (content is about 99.5%) is the hydrolith adsorption column of 5mm～10mm through particle diameter, and dress post amount is 4/5 of a column length; Flow velocity is about 50mL/min; N, the dinethylformamide raw material fully contacts with hydrolith, absorption impurity such as moisture wherein; Fluid to be adsorbed is up to the standards, and (be the approaching chromatographic grade technical requirement of effluent each item index, concrete technical requirement is seen table 1.) back entering next-step operation;
(2) absorption fluid in the step (1) is squeezed into still kettle, add 5% aluminum oxide (weight ratio) in the still, 500～600 ℃ of pre-burnings, about 1 hour.Underpressure distillation under 5～10mmHg pressure makes N, and dinethylformamide further dehydrates and remove a small amount of amine impurity, discards front-end volatiles;
(3) distillation fluid in the step (2) is collected finished product after the assay was approved, in the reagent bottle that is filled with nitrogen, preserve, promptly get chromatographic grade N, dinethylformamide with 0.45 μ mNYL filtering with microporous membrane.
Embodiment 2
A kind of chromatographic grade N, the preparation method of dinethylformamide, step is following:
(1) with raw material N, dinethylformamide (content is about 99.5%) is the hydrolith adsorption column of 10mm～15mm through particle diameter, and hydrolith dress post amount is 4/5 of a column length; Flow velocity is about 140mL/min; N, the dinethylformamide raw material fully contacts with hydrolith, absorption impurity such as moisture wherein; Fluid to be adsorbed is up to the standards, and (be the approaching chromatographic grade technical requirement of effluent each item index, concrete technical requirement is seen table 1.) back entering next-step operation;
(2) above-mentioned absorption fluid is squeezed into still kettle, add about 20% aluminum oxide (weight ratio) in the still, 500～600 ℃ of pre-burnings; About 2 hours, underpressure distillation under 5～10mmHg pressure made N; Dinethylformamide further dehydrates and removes a small amount of amine impurity, and discards front-end volatiles.
(3) collect finished product after the assay was approved, in the reagent bottle that is filled with nitrogen, preserve, promptly get chromatographic grade N, dinethylformamide with 0.45 μ mNYL filtering with microporous membrane.
Effect detection:
Chromatographic grade reagent N after preparation, dinethylformamide, (the quartzy cuvette of 1cm in ultraviolet wavelength 270nm～400nm scope; Water is made reference), absorbancy satisfies the index request in the table 1, and content is greater than 99.9%; Moisture≤0.05%; The recovery is greater than 94%, and yield rate reaches more than 95% approximately, and all other indexs meet the requirements.Compare with raw material, moisture and absorbancy are significantly improved.
Table 1: raw material, chromatographically pure N, the technical indicator of dinethylformamide
Claims (5)
1. chromatographic grade N, the preparation method of dinethylformamide is characterized in that: step is following:
(1) with raw material N, dinethylformamide is through being equipped with the adsorption column of sorbent material, flow velocity 50mL/min～140mL/min;
(2) absorption fluid in the step (1) is squeezed into still kettle, the adding weight ratio is 5～20% aluminum oxide in the still, 500～600 ℃ of pre-burnings, about 1-2 of time hour, underpressure distillation under 5～10mmHg pressure;
(3) with distillation fluid warp 0.45 μ m filtering with microporous membrane, bottling in the step (2), inflated with nitrogen is preserved, and promptly gets chromatographic grade N, dinethylformamide.
2. chromatographic grade N according to claim 1, the preparation method of dinethylformamide is characterized in that: the sorbent material of described step (1) is the hydrolith of particle diameter 5mm～15mm.
3. chromatographic grade N according to claim 2, the preparation method of dinethylformamide is characterized in that: the dress post amount of the hydrolith of described step (1) is 4/5 of a column length.
4. chromatographic grade N according to claim 1, the preparation method of dinethylformamide is characterized in that: 500～600 ℃ of the aluminum oxide elder generation pre-burnings of said step (2), about 1-2 of time hour.
5. chromatographic grade N according to claim 1, the preparation method of dinethylformamide is characterized in that: said step (2) N, the weight ratio of dinethylformamide and aluminum oxide is 5～20%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106045872A (en) * | 2016-06-06 | 2016-10-26 | 南京工业大学 | System for recovering DMF (dimethylformamid) waste liquor with pervaporation method and method |
| CN107337614A (en) * | 2017-08-29 | 2017-11-10 | 湖北工程学院 | Chromatographically pure N, N dimethyl acetamide and preparation method thereof, production system |
| CN108976144A (en) * | 2018-08-31 | 2018-12-11 | 潍坊中汇化工有限公司 | A kind of method of biopharmaceutical production DMF waste liquid purification |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101157626A (en) * | 2007-10-26 | 2008-04-09 | 合肥工业大学 | Method for purifying N,N-dimethyl formamide |
| CN101993387A (en) * | 2010-11-03 | 2011-03-30 | 天津大学 | Purifying method for electronic-grade N,N-dimethylformamide |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101157626A (en) * | 2007-10-26 | 2008-04-09 | 合肥工业大学 | Method for purifying N,N-dimethyl formamide |
| CN101993387A (en) * | 2010-11-03 | 2011-03-30 | 天津大学 | Purifying method for electronic-grade N,N-dimethylformamide |
Non-Patent Citations (4)
| Title |
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| JAN S. JAWORSKI: "Entropy of Electrochemical Formation of p-Semiquinones in Dimethylformamide", 《MONATSHEFTE FÜR CHEMIE》, vol. 117, no. 2, 28 February 1986 (1986-02-28) * |
| PROESPUN KANATHARAN ET AL.: "EVALUATION OF DMF FOR CYCLIC VOLTAMMETRY AT THE PGE", 《ANALYTICAL LETTERS》, vol. 6, no. 5, 31 May 1973 (1973-05-31), pages 421 - 433 * |
| 段长强等: "《现代化学试剂手册 第一分册 通用试剂》", 30 June 1988, article "二甲基甲酰胺", pages: 841 * |
| 罗代暄等: "《化学试剂与精细化学品合成基础（有机分册）》", 31 May 1991, article "N,N-二甲基甲酰胺", pages: 551-552 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106045872A (en) * | 2016-06-06 | 2016-10-26 | 南京工业大学 | System for recovering DMF (dimethylformamid) waste liquor with pervaporation method and method |
| CN107337614A (en) * | 2017-08-29 | 2017-11-10 | 湖北工程学院 | Chromatographically pure N, N dimethyl acetamide and preparation method thereof, production system |
| CN108976144A (en) * | 2018-08-31 | 2018-12-11 | 潍坊中汇化工有限公司 | A kind of method of biopharmaceutical production DMF waste liquid purification |
| CN108976144B (en) * | 2018-08-31 | 2021-04-02 | 潍坊中汇化工有限公司 | Method for purifying waste liquid of biological medicine DMF production |
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