CN105085318A - Purification method of acetonitrile for high performance liquid chromatographic analysis - Google Patents
Purification method of acetonitrile for high performance liquid chromatographic analysis Download PDFInfo
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- CN105085318A CN105085318A CN201410209251.0A CN201410209251A CN105085318A CN 105085318 A CN105085318 A CN 105085318A CN 201410209251 A CN201410209251 A CN 201410209251A CN 105085318 A CN105085318 A CN 105085318A
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Abstract
The invention discloses a purification method of acetonitrile for high performance liquid chromatographic analysis. The method is characterized in that impurities in a waste material acetonitrile are removed through processes such as modified active carbon adsorption and the like so as to obtain acetonitrile for high performance liquid chromatographic analysis. By the purification method of acetonitrile for high performance liquid chromatographic analysis, the waste material acetonitrile with the purity being only 15 wt% can be purified to obtain acetonitrile with its purify being greater than or equal to 99.9 wt%. Thus, recycling and reusing of the waste material acetonitrile are realized, degree of pollution of spent liquor from polypeptide production to the environment is reduced, and production cost is saved.
Description
Technical field
The present invention relates to solvent purification field, particularly a kind of method of purification extracting efficient liquid phase chromatographic analysis acetonitrile from waste liquid acetonitrile.
Background technology
Along with the development of modern biotechnology, there is various polypeptide drug, in clinical medicine, had huge using value.Highly purified polypeptide sample is provided, medicinal liquor for its physico-chemical property, biological activity and medical function thereof has important effect, high performance liquid chromatography (HPLC) has good separating effect, resolving power is high, the rate of recovery is high feature, in the separation and purification and preparation of polypeptide, enjoy favor, be therefore current separation and purification and the Main Means preparing polypeptide.Prepare in the process of polypeptide, the moving phase that component need be used to be acetonitrile-water by polypeptide sample from wash-out chromatographic column, then by elutriant underpressure distillation, the acetonitrile in removing elutriant.The acetonitrile of the waste material that distillation produces to be purity be 15% (wt), because purity is lower, manyly discardedly not to re-use, causes great waste, also can cause very big pollution after discharge to environment.
Summary of the invention
The object of the invention is to overcome deficiency of the prior art, a kind of method of purification improving the efficient liquid phase chromatographic analysis acetonitrile of acetonitrile purity is provided.
For realizing above object, the present invention is achieved through the following technical solutions:
The method of purification of efficient liquid phase chromatographic analysis acetonitrile, is characterized in that, comprises the steps:
A. get waste material acetonitrile solution, add acid, acid salt, acidic oxide, alkali, subsalt, basic oxide or strong acid and strong base salt wherein, the polarity of waste material acetonitrile and pH value are regulated, makes pH value control in 6 ~ 10 scopes; Acid, acid salt, acidic oxide, alkali, subsalt, basic oxide or strong acid and strong base salt can react with the lipid-soluble substance in waste material acetonitrile solution or organic acid such as the impurity such as trifluoroacetic acid, make reactants dissolved at aqueous phase.Wherein, acid, acid salt, alkali, subsalt, basic oxide, strong acid and strong base salt include but not limited to sodium-chlor, sodium sulfate, Repone K, potassium sulfate, sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, sulfuric acid, nitric acid, sodium pyrosulfate etc.
B. in the solution of step a gained, add varsol, after vibration, stratification, get organic layer, remove water layer; And organic layer is distilled at the temperature lower than acetonitrile boiling point, varsol steams as cut, retains acetonitrile.Wherein, the varsol steamed is after recycling, and the acetonitrile solution internal recycle that can continue to be added into step a gained utilizes.
C. add oxygenant in the solution obtained to above-mentioned distillation and stir, carrying out oxide treatment; Post-heating steams acetonitrile.Unsaturated hydrocarbons impurity is removed as the impurity such as ethanamide and the impurity affecting transmitance in this step.Be used in particular for removing the impurity close with acetonitrile boiling point as vinyl cyanide etc.
D. by the acetonitrile after oxide treatment with 0.5 ~ 30 column volume/hour speed pass into the sorbent material post that modified activated carbon is housed and carry out adsorption treatment, for removing the unsaturated organic compound of carbon-carbon double bonds as heterocyclic arene and heavy metal ion etc.; Namely the efficient liquid phase chromatographic analysis acetonitrile of purity >=99.9% (wt) is obtained.
Preferably, in described step c, oxygenant comprises potassium permanganate, Sodium Persulfate, clorox, Losantin or superoxide.Superoxide includes but not limited to hydrogen peroxide.
Preferably, in described step a, the volumetric concentration of acid, acid salt, alkali, subsalt or strong acid and strong base salts solution is all in 0.5 ~ 2% scope.
Preferably, in described step b, varsol comprises methylene dichloride, hexane, toluene or benzene.
Preferably, in described step c, while adding potassium permanganate or superoxide, add alkaline hydrated oxide and basic oxide, slow down the oxidisability of potassium permanganate, the acidic substance that neutralization oxidation simultaneously produces, adjust ph is in 8 ~ 14 scopes.Alkaline hydrated oxide includes but not limited to sodium hydroxide, potassium hydroxide, and basic oxide include but not limited to calcium oxide.
Preferably, in described steps d, modified activated carbon is a kind of or several arbitrarily particle diameter in surface attachment aluminum oxide, aluminium hydroxide, ethylenediamine tetraacetic acid (EDTA), trolamine, nitric acid, hypochlorite is 20 ~ 100 object activated carbon.The mass concentration of aluminium hydroxide, ethylenediamine tetraacetic acid (EDTA), trolamine, nitric acid or hypochlorite solutions is all in 5% ~ 30% scope.
Preferably, in described steps d, after acetonitrile being passed into the sorbent material post that modified activated carbon is housed, then pass into the sorbent material post that molecular sieve is housed, go out moisture further.
Preferably, also comprise step e, the acetonitrile of adsorption treatment gained is carried out rectifying; Rectifying still Heating temperature is 80 ~ 95 DEG C, acetonitrile liquid temperature 76 ~ 85 DEG C in still, distill out liquid temp and be 75 ~ 83 DEG C, control reflux ratio 15: 1 ~ 5:1.
The method of purification of efficient liquid phase chromatographic analysis acetonitrile provided by the invention, through the operation that a series of energy consumptions of varsol extraction, oxides, modification activated carbon adsorption are low, waste material acetonitrile purity being only 15% (wt) is purified to the acetonitrile of purity >=99.9% (wt), realize the recycling to waste material acetonitrile, reduce waste liquid in polypeptide production and, to the pollution level of environment, save production cost.Method of purification provided by the invention also has that energy consumption is low, production process is easy, stable, be applicable to the advantages such as suitability for industrialized production.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail:
Embodiment 1
The method of purification of efficient liquid phase chromatographic analysis acetonitrile, comprises the steps:
A. get waste material acetonitrile solution, add the sodium chloride solution that volumetric concentration is 2% wherein, the polarity of waste material acetonitrile solution and pH value are regulated, makes pH value be 7.5; Lipid-soluble substance in sodium-chlor and waste material acetonitrile solution or organic acid such as the impurity such as trifluoroacetic acid react, and make reactants dissolved at aqueous phase.
B. in the solution of step a gained, add methylene dichloride, retain organic layer after vibration, stratification, discard water layer, thus remove the impurity such as lipid-soluble substance, organic acid and the water in waste material acetonitrile solution.Distilled at the temperature lower than acetonitrile boiling point by organic layer, the boiling point due to acetonitrile is greater than the boiling point of methylene dichloride, and by distillation, methylene dichloride steams as cut, and acetonitrile then retains as liquid.Wherein, the methylene dichloride steamed is after recycling, and the solution internal recycle that can continue to be added into step a gained utilizes.
C. in aforesaid liquid, add potassium permanganate carry out oxide treatment; While adding potassium permanganate, add sodium hydroxide and calcium oxide, slow down the oxidisability of potassium permanganate, the acidic substance that neutralization oxidation simultaneously produces, adjust ph is 8.Heating distills out acetonitrile.
D. by the acetonitrile of step c gained with 15 column volumes/hour speed pass into and surface attachment is housed has the sorbent material post of the activated carbon of aluminum hydroxide solution to carry out adsorption treatment, for removing the unsaturated organic compound of carbon-carbon double bonds as heterocyclic arene and heavy metal ion etc.The mass concentration of aluminum hydroxide solution is 5%, and the particle diameter of activated carbon is 100 orders.
Again the acetonitrile of gained is passed into the sorbent material post that molecular sieve is housed, go out moisture further.
E. the acetonitrile of above-mentioned adsorption treatment gained is carried out rectifying, rectifying still Heating temperature is 85 DEG C, acetonitrile liquid temperature 85 DEG C in still, distill out liquid temp and be 80 DEG C, control reflux ratio 10: 1 fluid, remove front-end volatiles, rectifying fluid detects qualified rear bottling, inflated with nitrogen is preserved, and namely obtains the efficient liquid phase chromatographic analysis acetonitrile of purity >=99.9% (wt).
Embodiment 2
The method of purification of efficient liquid phase chromatographic analysis acetonitrile, comprises the steps:
A. get waste material acetonitrile solution, add the potassium hydroxide solution that volumetric concentration is 0.5% wherein, the polarity of waste material acetonitrile solution and pH value are regulated, makes pH value be 8; Lipid-soluble substance in potassium hydroxide and waste material acetonitrile solution or organic acid such as the impurity such as trifluoroacetic acid react, and make reactants dissolved at aqueous phase.
B. in the solution of step a gained, add hexane, get organic layer after vibration, stratification, discard water layer, thus remove the impurity such as lipid-soluble substance, organic acid and the water in waste material acetonitrile solution.Organic layer is distilled at the temperature lower than acetonitrile boiling point.Boiling point due to acetonitrile is greater than the boiling point of hexane, and by distillation, hexane steams as cut, and acetonitrile then retains as liquid.Wherein, the hexane steamed is after recycling, and the solution internal recycle that can continue to be added into step a gained utilizes.
C. in aforesaid liquid, add hydrogen peroxide carry out oxide treatment; While adding hydrogen peroxide, add sodium hydroxide and calcium oxide, slow down the oxidisability of hydrogen peroxide, the acidic substance that neutralization oxidation simultaneously produces, adjust ph is 10.Heating distills out acetonitrile.
D. by the acetonitrile of step c gained with 30 column volumes/hour speed pass into and surface attachment is housed has the sorbent material post of the activated carbon of aluminum oxide to carry out adsorption treatment, for removing the unsaturated organic compound of carbon-carbon double bonds as heterocyclic arene and heavy metal ion etc.The particle diameter of activated carbon is 54 orders.
Again the acetonitrile of gained is passed into the sorbent material post that molecular sieve is housed, go out moisture further.
E. the acetonitrile of above-mentioned adsorption treatment gained is carried out rectifying, rectifying still Heating temperature is 85 DEG C, acetonitrile liquid temperature 80 DEG C in still, distill out liquid temp and be 75 DEG C, control reflux ratio 15: 1 fluid, remove front-end volatiles, rectifying fluid detects qualified rear bottling, inflated with nitrogen is preserved, and namely obtains the efficient liquid phase chromatographic analysis acetonitrile of purity >=99.9% (wt).
Embodiment 3
The method of purification of efficient liquid phase chromatographic analysis acetonitrile, comprises the steps:
A. get waste material acetonitrile solution, add the sulphuric acid soln that volumetric concentration is 1.3% wherein, the polarity of waste material acetonitrile solution and pH value are regulated, makes pH value be 6.
B. in the solution of step a gained, add toluene, get organic layer after vibration, stratification, discard water layer, thus remove the impurity such as lipid-soluble substance, organic acid and the water in waste material acetonitrile solution.Organic layer is distilled at the temperature lower than acetonitrile boiling point.Boiling point due to acetonitrile is greater than the boiling point of toluene, and by distillation, toluene steams as cut, and acetonitrile then retains as liquid.Wherein, the toluene steamed is after recycling, and the solution internal recycle that can continue to be added into step a gained utilizes.
C. in aforesaid liquid, add clorox carry out oxide treatment; While adding clorox, add sodium hydroxide and calcium oxide, slow down the oxidisability of clorox, the acidic substance that neutralization oxidation simultaneously produces, adjust ph is 14.Heating distills out acetonitrile.
D. by the acetonitrile of step c gained with 0.5 column volume/hour speed pass into and surface attachment is housed has the sorbent material post of the activated carbon of edta solution to carry out adsorption treatment, for removing the unsaturated organic compound of carbon-carbon double bonds as heterocyclic arene and heavy metal ion etc.The mass concentration of edta solution is 15%, and the particle diameter of activated carbon is 20 orders.
Again the acetonitrile of gained is passed into the sorbent material post that molecular sieve is housed, go out moisture further.
E. the acetonitrile of above-mentioned adsorption treatment gained is carried out rectifying, rectifying still Heating temperature is 80 DEG C, acetonitrile liquid temperature 79 DEG C in still, distill out liquid temp and be 79 DEG C, control reflux ratio 5: 1 fluid, remove front-end volatiles, rectifying fluid detects qualified rear bottling, inflated with nitrogen is preserved, and namely obtains the efficient liquid phase chromatographic analysis acetonitrile of purity >=99.9% (wt).
Embodiment 4
The method of purification of efficient liquid phase chromatographic analysis acetonitrile, comprises the steps:
A. get waste material acetonitrile solution, add the sodium hydrogen carbonate solution that volumetric concentration is 0.8% wherein, the polarity of waste material acetonitrile solution and pH value are regulated, makes pH value be 10; Lipid-soluble substance in sodium bicarbonate and waste material acetonitrile solution or organic acid such as the impurity such as trifluoroacetic acid react, and make reactants dissolved at aqueous phase.
B. in the solution of step a gained, add benzene, get organic layer after vibration, stratification, discard water layer, thus remove the impurity such as lipid-soluble substance, organic acid and the water in waste material acetonitrile solution.Organic layer is distilled at the temperature lower than acetonitrile boiling point.Boiling point due to acetonitrile is greater than the boiling point of benzene, and by distillation, benzene steams as cut, and acetonitrile then retains as liquid.Wherein, the benzene steamed is after recycling, and the solution internal recycle that can continue to be added into step a gained utilizes.
C. in aforesaid liquid, add Potassium Persulphate carry out oxide treatment; While adding Potassium Persulphate, add sodium hydroxide and calcium oxide, slow down the oxidisability of Potassium Persulphate, the acidic substance that neutralization oxidation simultaneously produces, adjust ph is 11.Heating distills out acetonitrile.
D. by the acetonitrile of step c gained with 22 column volumes/hour speed pass into and surface attachment is housed has the sorbent material post of the activated carbon of triethanolamine solution to carry out adsorption treatment, for removing the unsaturated organic compound of carbon-carbon double bonds as heterocyclic arene and heavy metal ion etc.The mass concentration of triethanolamine solution is 24%, and the particle diameter of activated carbon is 90 orders.
Again the acetonitrile of gained is passed into the sorbent material post that molecular sieve is housed, go out moisture further.
E. the acetonitrile of above-mentioned adsorption treatment gained is carried out rectifying, rectifying still Heating temperature is 85 DEG C, acetonitrile liquid temperature 76 DEG C in still, distill out liquid temp and be 75 DEG C, control reflux ratio 12: 1 fluid, remove front-end volatiles, rectifying fluid detects qualified rear bottling, inflated with nitrogen is preserved, and namely obtains the efficient liquid phase chromatographic analysis acetonitrile of purity >=99.9% (wt).
Embodiment 5
The method of purification of efficient liquid phase chromatographic analysis acetonitrile, comprises the steps:
A. get waste material acetonitrile solution, add the metabisulfite solution that volumetric concentration is 1.9% wherein, the polarity of waste material acetonitrile solution and pH value are regulated, make pH value control 8; Lipid-soluble substance in sodium sulfate and waste material acetonitrile solution or organic acid such as the impurity such as trifluoroacetic acid react, and make reactants dissolved at aqueous phase.
B. in the solution of step a gained, add methylene dichloride, get organic layer after vibration, stratification, discard water layer, thus remove the impurity such as lipid-soluble substance, organic acid and the water in waste material acetonitrile solution.Organic layer is distilled at the temperature lower than acetonitrile boiling point.Boiling point due to acetonitrile is greater than the boiling point of methylene dichloride, and by distillation, methylene dichloride steams as cut, and acetonitrile then retains as liquid.Wherein, the methylene dichloride steamed is after recycling, and the solution internal recycle that can continue to be added into step a gained utilizes.
C. in aforesaid liquid, add potassium permanganate carry out oxide treatment; While adding potassium permanganate, add sodium hydroxide and calcium oxide, slow down the oxidisability of potassium permanganate, the acidic substance that neutralization oxidation simultaneously produces, adjust ph is 9.Heating distills out acetonitrile.
D. by the acetonitrile of step c gained with 30 column volumes/hour speed pass into and surface attachment is housed has the sorbent material post of the activated carbon of salpeter solution to carry out adsorption treatment, for removing the unsaturated organic compound of carbon-carbon double bonds as heterocyclic arene and heavy metal ion etc.The mass concentration of salpeter solution is 24%, and the particle diameter of activated carbon is 90 orders.
Again the acetonitrile of gained is passed into the sorbent material post that molecular sieve is housed, go out moisture further.
E. the acetonitrile of above-mentioned adsorption treatment gained is carried out rectifying, rectifying still Heating temperature is 81 DEG C, acetonitrile liquid temperature 80 DEG C in still, distill out liquid temp and be 76 DEG C, control reflux ratio 6: 1 fluid, remove front-end volatiles, rectifying fluid detects qualified rear bottling, inflated with nitrogen is preserved, and namely obtains the efficient liquid phase chromatographic analysis acetonitrile of purity >=99.9% (wt).
Embodiment 1 ~ 5 purify after efficient liquid phase chromatographic analysis acetonitrile technical indicator as shown in Table 1:
Table one
As shown in Table 1, by method provided by the invention, the waste liquid acetonitrile solution realizing purity to be only 15% purifies to the efficient liquid phase chromatographic analysis acetonitrile of purity >=99.9%, and the water content of efficient liquid phase chromatographic analysis acetonitrile is extremely low, can ignore.Waste liquid yield is also not less than 80% simultaneously, and the yield of more traditional method of purification 70% improves greatly.To wavelength be the incident light of 200nm, 210nm, 220nm and 260nm transmittance comparatively raw material also greatly improve, improve the optical property of efficient liquid phase chromatographic analysis acetonitrile.
Embodiment in the present invention, only for the present invention will be described, does not form the restriction to right, other equivalent in fact substituting, all in scope that those skilled in that art can expect.
Claims (8)
1. the method for purification of efficient liquid phase chromatographic analysis acetonitrile, is characterized in that, comprises the steps:
A. get waste material acetonitrile solution, add acid solution, acid salt solution, acidic oxide, alkaline solution, subsalt solution, basic oxide or strong acid and strong base salts solution wherein;
B. in the solution of step a gained, varsol is added, vibration, stratification; Discard water layer, and heat organic layer and steam varsol, retain acetonitrile;
C. in the solution of step b gained, add oxygenant and stir, heating distills out acetonitrile;
D. above-mentioned acetonitrile is passed into the sorbent material post that modified activated carbon is housed and carry out adsorption treatment; Obtain the efficient liquid phase chromatographic analysis acetonitrile of purity >=99.99% (wt).
2. the method for purification of efficient liquid phase chromatographic analysis acetonitrile according to claim 1, is characterized in that, in described step a, the volumetric concentration of acid solution, acid salt solution, alkaline solution, subsalt solution or strong acid and strong base salts solution is 0.5 ~ 2%.
3. the method for purification of efficient liquid phase chromatographic analysis acetonitrile according to claim 1, is characterized in that, in described step b, varsol comprises methylene dichloride, hexane, toluene or benzene.
4. method of purification according to claim 1, is characterized in that, in described step c, oxygenant comprises potassium permanganate, Potassium Persulphate, clorox, Losantin or superoxide.
5. the method for purification of efficient liquid phase chromatographic analysis acetonitrile according to claim 1, is characterized in that, in described step c, while adding oxygenant, adds alkaline hydrated oxide and basic oxide.
6. the method for purification of efficient liquid phase chromatographic analysis acetonitrile according to claim 1, it is characterized in that, in described steps d, modified activated carbon is a kind of or several arbitrarily activated carbon in surface attachment aluminum oxide, aluminium hydroxide, hypochlorite, ethylenediamine tetraacetic acid (EDTA), trolamine, nitric acid.
7. the method for purification of efficient liquid phase chromatographic analysis acetonitrile according to claim 1, is characterized in that, also comprises in steps d, after acetonitrile being passed into the sorbent material post that modified activated carbon is housed, then passes into the sorbent material post that molecular sieve is housed.
8. the method for purification of the efficient liquid phase chromatographic analysis acetonitrile according to above-mentioned any one claim, is characterized in that, also comprise step e, and the acetonitrile of adsorption treatment gained is carried out rectifying; Rectifying still Heating temperature is 80 ~ 95 DEG C, acetonitrile liquid temperature 76 ~ 85 DEG C in still, distill out liquid temp and be 75 ~ 83 DEG C, control reflux ratio 15: 1 ~ 5:1.
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| CN114133342A (en) * | 2021-12-20 | 2022-03-04 | 潍坊中汇化工有限公司 | Acetonitrile working solution for preparing chromatograph and preparation method thereof |
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Application publication date: 20151125 |