CN108794348A - A kind of method that the useless acetonitrile of biopharmaceutical production prepares high-purity acetonitrile - Google Patents
A kind of method that the useless acetonitrile of biopharmaceutical production prepares high-purity acetonitrile Download PDFInfo
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- CN108794348A CN108794348A CN201810628498.4A CN201810628498A CN108794348A CN 108794348 A CN108794348 A CN 108794348A CN 201810628498 A CN201810628498 A CN 201810628498A CN 108794348 A CN108794348 A CN 108794348A
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- acetonitrile
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- biopharmaceutical production
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- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 title claims abstract description 324
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 35
- 229960000074 biopharmaceutical Drugs 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000001179 sorption measurement Methods 0.000 claims abstract description 20
- 239000002131 composite material Substances 0.000 claims abstract description 14
- 238000010992 reflux Methods 0.000 claims abstract description 11
- 238000010533 azeotropic distillation Methods 0.000 claims abstract description 10
- 230000018044 dehydration Effects 0.000 claims abstract description 10
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 238000010521 absorption reaction Methods 0.000 claims abstract description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 18
- 239000002808 molecular sieve Substances 0.000 claims description 15
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000003039 volatile agent Substances 0.000 claims description 8
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 5
- 239000004917 carbon fiber Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 5
- 239000003463 adsorbent Substances 0.000 claims description 4
- 239000013065 commercial product Substances 0.000 description 11
- 238000000926 separation method Methods 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 238000002360 preparation method Methods 0.000 description 7
- 239000002699 waste material Substances 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 239000005416 organic matter Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000009835 boiling Methods 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 238000007689 inspection Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- 235000011121 sodium hydroxide Nutrition 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229920001184 polypeptide Polymers 0.000 description 1
- 102000004196 processed proteins & peptides Human genes 0.000 description 1
- 108090000765 processed proteins & peptides Proteins 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/32—Separation; Purification; Stabilisation; Use of additives
- C07C253/34—Separation; Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Epoxy Compounds (AREA)
Abstract
The present invention provide it is a kind of given up the method that acetonitrile prepares high-purity acetonitrile using biopharmaceutical production, include the following steps：Pretreatment, azeotropic distillation, dehydrating tower dehydration, the absorption of composite adsorption tower and highly efficient distilling step.The pretreatment：The biopharmaceutical production acetonitrile that gives up is adjusted into pH value to 7-9.The azeotropic distillation：The low liquid temperature control of rectifying still is at 83-87 DEG C, and the tower top temperature of rectifying column is 75-80 DEG C, and reflux ratio is adjusted to 5：1.The present invention is given up the high-purity acetonitrile that acetonitrile produces by biopharmaceutical production, and purity is up to 99.99%；Moisture is 0.012-0.013%.
Description
Technical field
It is given up the method that acetonitrile prepares high-purity acetonitrile using biopharmaceutical production the present invention relates to a kind of, belongs to fine chemical technology
Field.
Background technology
With using monoclonal antibody and target polypeptide drug as the fast development of the designative species of representative, acetonitrile conduct
Must solvent be used widely in bio-pharmaceutical industry production, useless acetonitrile solution yield also increases year by year accordingly.
However, in recent years, as the policy requirements of national environmental protection, resource-effective, circular economy etc. are increasingly tight
Lattice, rationally disposition becomes the conspicuous contradiction for restricting industry development with recycling to the acetonitrile solvent that gives up.
The useless main processing method of acetonitrile of this biopharmaceutical production is burning disposal, causes the serious waste of resource, and
Environment is polluted, and causes a large amount of greenhouse gas emissions.
It there is no both at home and abroad at present and such prepare the report of high-purity acetonitrile from the biopharmaceutical production acetonitrile that gives up.
In conclusion research and development are a kind of efficient, energy saving, green, environmentally friendly to prepare high-purity acetonitrile with the biopharmaceutical production acetonitrile that gives up
Method it is very necessary.
Invention content：
It is given up the method that acetonitrile prepares high-purity acetonitrile using biopharmaceutical production the purpose of the present invention is to provide a kind of, by biological medicine
The useless acetonitrile of production, turns waste into wealth, micro- useless comprehensive utilization.
To realize above goal of the invention, the technical solution used for：
A method of high-purity acetonitrile being prepared using the biopharmaceutical production acetonitrile that gives up, is included the following steps：
Step 1, pretreatment
The biopharmaceutical production acetonitrile that gives up is added liquid caustic soda and adjusts pH value to 7-9.
The biopharmaceutical production gives up acetonitrile：Ethane nitrile content is 18%-22%, water content 77%-81%, pH about 4-6.
The liquid caustic soda is
Step 2, azeotropic distillation
Waste liquid is sent into rectifying column rectifying, for the low liquid temperature control of rectifying still at 83-87 DEG C, the tower top temperature of rectifying column is 75-80
DEG C, reflux ratio is adjusted to 5：1；Protein, salt and the organic impurities in solvent are removed, 85% acetonitrile solution is obtained.
Step 3, dehydrating tower dehydration
It is taken off 4A molecular sieve water separation towers are sent to by acetonitrile solution after azeotropic distillation with the speed of 40-60ml/min
Water, the drying pillar height 2-3m of dehydrating tower, internal diameter 3-5cm, built-in drier, dress column amount are the 4/5 of pillar height；Obtain moisture
< 500ppm contents are more than 99.5% crude acetonitrile.
The drier is using one or both of 4A molecular sieves, aluminium oxide.
Step 4, the absorption of composite adsorption tower
The crude acetonitrile of extraction is sent to composite adsorption tower with the speed of 50-70ml/min to adsorb, the column of composite adsorption tower
High 2-3m, internal diameter 3-5cm, built-in adsorbent, dress column amount are the 4/5 of pillar height；What removal rectifying column can not detach boils with acetonitrile
The similar organic matter of point, obtains 99.9% commercial product acetonitrile.
The adsorbent uses carbon fiber.
Step 5, highly efficient distilling
The commercial product acetonitrile that composite adsorption tower is produced is sent to high-efficient spiral-screen column and carries out rectifying, temperature control in rectifying still bottom exists
83-87 DEG C, the tower top temperature of rectifying column is 75-80 DEG C, and reflux ratio is adjusted to 15：1-10：1, the front-end volatiles of 5-10% amounts are removed,
Take the fraction of intermediate 80-90% amounts, as preparation scale high-purity acetonitrile；Specific trace impurity in solvent is removed, obtaining content is
99.99% high-purity acetonitrile.
The present invention is given up the high-purity acetonitrile that acetonitrile produces by biopharmaceutical production, high income, and indices are fully able to reach
The product standard of preparation scale acetonitrile, purity is up to 99.99%；Moisture is 0.012-0.013%, evaporation residue 0.25-
0.3mg/kg, density（20℃）For 0.782g/ml, titratable acid 0.0003mmol/g, UV light transmittance：200nm 93.6-
94.3%, 230nm 98.6-98.8%, 240nm 99.0-99.2%.The method of the present invention is simple, production cost is low；Low energy consumption；Ton production
1-2 tons of steam of product, ton product 1-200kw；High-purity acetonitrile quality obtained is good, purity 99.99%；Optical index：It can be back to
Biological medicine produces；Yield is high.
Description of the drawings
Fig. 1 it is a kind of using biopharmaceutical production give up acetonitrile prepare high-purity acetonitrile method operating process schematic diagram.
Specific implementation mode
Embodiment 1 is a kind of to be given up the method that acetonitrile prepares high-purity acetonitrile using biopharmaceutical production
Step 1, pretreatment
It takes biopharmaceutical production to give up acetonitrile, detects pH value；Then use the sodium hydroxide solution that mass percentage is 30% by pH value tune
Section obtains the waste liquid that pH value is 8 to 8.
The biopharmaceutical production gives up acetonitrile：Ethane nitrile content is 18%-22%, water content 77%-81%, pH about 4-6.
Step 2, azeotropic distillation
The waste liquid that pH value is 8 is sent into azeotropy rectification column and carries out rectification process, the rectifying still bottom temperature control of azeotropy rectification column
System is at 87 DEG C, and the tower top temperature of rectifying column is 80 DEG C, and reflux ratio is adjusted to 5：1, remove the front-end volatiles of 10% amount；Collect intermediate 80%
The fraction of amount, i.e. acetonitrile solution.The acetonitrile solution purity is 85%；Above-mentioned percentage is mass percent.
Step 3, dehydrating tower dehydration
A clean drying column is taken, dry pillar height 2m, internal diameter 5cm, interior that drier is housed, the drier is 4A molecular sieves
With aluminium oxide, dress column amount is the 4/5 of pillar height, obtains 4A molecular sieve water separation towers.When filling, 4A molecular sieves and each 1 meter of aluminium oxide.
The acetonitrile solution at room temperature prepared by step 2 is sent to 4A molecular sieve water separation towers with the speed of 40ml/min and carries out
Dehydration, obtains crude acetonitrile.The crude acetonitrile moisture < 500ppm, content are more than 99.5%.
Step 4, the absorption of composite adsorption tower
A clean adsorption column is taken, adsorbs pillar height 2m, internal diameter 5cm, built-in carbon fiber, dress column amount is the 4/5 of pillar height, is answered
Close adsorption tower.
Crude acetonitrile is sent to composite adsorption tower with the speed of 70ml/min at room temperature, is adsorbed, removal rectifying column without
Method separation with organic matter similar in acetonitrile boiling point, obtain commercial product acetonitrile.The commercial product acetonitrile purity is higher than 99.9%.
Step 5, highly efficient distilling
The commercial product acetonitrile that above-mentioned steps obtain is sent in highly efficient distilling device and carries out rectification process, the temperature control of rectifying still bottom
System is at 83 DEG C, and the tower top temperature of rectifying column is 76 DEG C, and reflux ratio is adjusted to 10：1, the front-end volatiles of 5% amount are removed, collect intermediate 90%
The fraction of amount, as preparation scale high-purity acetonitrile.
Every inspection value is shown in Table 1；
Table 1
Note：It is ultraviolet to do reference with 1cm quartz cuvette water.
Embodiment 2 is a kind of to be given up the method that acetonitrile prepares high-purity acetonitrile using biopharmaceutical production
Step 1, pretreatment
It is same as Example 1.
Step 2, azeotropic distillation
The waste liquid that pH value is 8 is sent into azeotropy rectification column and carries out rectification process, the rectifying still bottom temperature control of azeotropy rectification column
System is at 83 DEG C, and the tower top temperature of rectifying column is 76 DEG C, and reflux ratio is adjusted to 5：1, remove the front-end volatiles of 5% amount；Take intermediate 90% amount
Fraction, i.e. acetonitrile solution.The acetonitrile solution purity is 85%；Above-mentioned percentage is mass percent.
Step 3, dehydrating tower dehydration
A clean drying column is taken, dry pillar height 2m, internal diameter 3cm, interior that drier is housed, the drier is 4A molecular sieves
With silica gel, dress column amount is the 4/5 of pillar height, obtains 4A molecular sieve water separation towers.When filling, 4A molecular sieves and each 1 meter of aluminium oxide.
The acetonitrile solution at room temperature prepared by step 2 is sent to 4A molecular sieve water separation towers with the speed of 50ml/min and carries out
Dehydration, obtains crude acetonitrile.The crude acetonitrile moisture < 500ppm, content are more than 99.5%.
Step 4, the absorption of composite adsorption tower
A clean adsorption column is taken, adsorbs pillar height 2m, internal diameter 3cm, built-in carbon fiber, dress column amount is the 4/5 of pillar height, is answered
Close adsorption tower.
Crude acetonitrile is sent to composite adsorption tower with the speed of 60ml/min at room temperature to adsorb, removal rectifying column can not
Separation with organic matter similar in acetonitrile boiling point, obtain commercial product acetonitrile.The commercial product acetonitrile purity is higher than 99.9%.
Step 5, highly efficient distilling
The commercial product acetonitrile that above-mentioned steps obtain is sent in highly efficient distilling device and carries out rectification process, the temperature control of rectifying still bottom
System is at 84 DEG C, and the tower top temperature of rectifying column is 77 DEG C, and reflux ratio is adjusted to 15：1, the front-end volatiles of 5% amount are removed, intermediate 90% amount is taken
Fraction, as preparation scale high-purity acetonitrile.
Every inspection value is shown in Table 2；
Table 2
Note：It is ultraviolet to do reference with 1cm quartz cuvette water.
Embodiment 3 is a kind of to be given up the method that acetonitrile prepares high-purity acetonitrile using biopharmaceutical production
Step 1, pretreatment
It is same as Example 1.
Step 2, azeotropic distillation
The waste liquid that pH value is 8 is sent into azeotropy rectification column and carries out rectification process, the rectifying still bottom temperature control of azeotropy rectification column
System is at 85 DEG C, and the tower top temperature of rectifying column is 78 DEG C, and reflux ratio is adjusted to 5：1, the front-end volatiles of 5% amount are removed, intermediate 90% amount is taken
Fraction, i.e. acetonitrile solution.The acetonitrile solution purity is 85%；Above-mentioned percentage is mass percent.
Step 3, dehydrating tower dehydration
A clean drying column is taken, dry pillar height 2m, internal diameter 3cm, interior that drier is housed, the drier is 4A molecular sieves
With silica gel, dress column amount is the 4/5 of pillar height, obtains 4A molecular sieve water separation towers.When filling, 4A molecular sieves and each 1 meter of aluminium oxide.
The acetonitrile solution at room temperature prepared by step 2 is sent to 4A molecular sieve water separation towers with the speed of 60ml/min and carries out
Dehydration, obtains crude acetonitrile.The crude acetonitrile moisture < 500ppm, content are more than 99.5%.
Step 4, the absorption of composite adsorption tower
A clean adsorption column is taken, adsorbs pillar height 2m, internal diameter 3cm, built-in carbon fiber, dress column amount is the 4/5 of pillar height, is answered
Close adsorption tower.
Crude acetonitrile is sent to composite adsorption tower with the speed of 50ml/min at room temperature to adsorb, removal rectifying column can not
Separation with organic matter similar in acetonitrile boiling point, obtain commercial product acetonitrile.The commercial product acetonitrile purity is higher than 99.9%.
Step 5, highly efficient distilling
The commercial product acetonitrile that above-mentioned steps obtain is sent in highly efficient distilling device and carries out rectification process, the temperature control of rectifying still bottom
System is at 87 DEG C, and the tower top temperature of rectifying column is 80 DEG C, and reflux ratio is adjusted to 15：1.2, the front-end volatiles of 5% amount are removed, centre 90% is taken
The fraction of amount, as preparation scale high-purity acetonitrile.
Every inspection value is shown in Table 3；
Table 3
Note：It is ultraviolet to do reference with 1cm quartz cuvette water.
The preparation scale acetonitrile of 1-3 preparations of the embodiment of the present invention is can be seen that in UV transmittance, moisture, evaporation from table 1-3
The high-purity acetonitrile standard of residue, titratable soda acid and the equal superstate setting of light transmittance.
It particularly points out the present invention and is not limited to above-mentioned specific implementation mode, it is all under the inspiration of the technology of the present invention invention, if
Similar technical solution is counted out, is each fallen within protection scope of the present invention.
Claims (9)
1. a kind of given up the method that acetonitrile prepares high-purity acetonitrile using biopharmaceutical production, it is characterised in that：Include the following steps：Pre- place
Reason, azeotropic distillation, dehydrating tower dehydration, the absorption of composite adsorption tower and highly efficient distilling step.
2. it is according to claim 1 it is a kind of given up the method that acetonitrile prepares high-purity acetonitrile using biopharmaceutical production, feature exists
In：The biopharmaceutical production gives up acetonitrile：Ethane nitrile content is 18%-22%, water content 77%-81%, pH about 4-6.
3. it is according to claim 1 it is a kind of given up the method that acetonitrile prepares high-purity acetonitrile using biopharmaceutical production, feature exists
In：The pretreatment：The biopharmaceutical production acetonitrile that gives up is adjusted into pH value to 7-9.
4. it is according to claim 1 it is a kind of given up the method that acetonitrile prepares high-purity acetonitrile using biopharmaceutical production, feature exists
In：The azeotropic distillation：The low liquid temperature control of rectifying still is at 83-87 DEG C, and the tower top temperature of rectifying column is 75-80 DEG C, reflux
Than being adjusted to 5：1.
5. it is according to claim 1 it is a kind of given up the method that acetonitrile prepares high-purity acetonitrile using biopharmaceutical production, feature exists
In：The dehydrating tower dehydration：4A molecules will be sent to the speed of 40-60ml/min by acetonitrile solution after azeotropic distillation
Sieve dehydrating tower is dehydrated to obtain crude acetonitrile；The drying pillar height 2-3m of dehydrating tower, internal diameter 3-5cm, built-in drier fill column amount
It is the 4/5 of pillar height.
6. it is according to claim 5 it is a kind of given up the method that acetonitrile prepares high-purity acetonitrile using biopharmaceutical production, feature exists
In：The drier is using one or both of 4A molecular sieves, aluminium oxide.
7. it is according to claim 1 it is a kind of given up the method that acetonitrile prepares high-purity acetonitrile using biopharmaceutical production, feature exists
In：The composite adsorption tower absorption：The pillar height 2-3m of composite adsorption tower, internal diameter 3-5cm, built-in adsorbent, dress column amount are
The 4/5 of pillar height.
8. it is according to claim 7 it is a kind of given up the method that acetonitrile prepares high-purity acetonitrile using biopharmaceutical production, feature exists
In：The adsorbent uses carbon fiber.
9. it is according to claim 1 it is a kind of given up the method that acetonitrile prepares high-purity acetonitrile using biopharmaceutical production, feature exists
In：The highly efficient distilling：The temperature control of rectifying still bottom is at 83-87 DEG C, and the tower top temperature of rectifying column is 75-80 DEG C, reflux
Than being adjusted to 15：1-10：1, the front-end volatiles of 5-10% amounts are removed, the fraction of intermediate 80-90% amounts is taken.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110526834A (en) * | 2019-09-20 | 2019-12-03 | 北京宇极科技发展有限公司 | A method of preparing high-purity perfluor isobutyronitrile |
| CN111138319A (en) * | 2018-11-06 | 2020-05-12 | 江苏九天高科技股份有限公司 | Method and device for recovering and refining high-purity acetonitrile in polypeptide synthesis |
| CN111413441A (en) * | 2020-05-06 | 2020-07-14 | 湖北弗顿生化科技有限公司 | Acetonitrile purification process for improved ultra-high liquid chromatography-mass spectrometer |
| CN113582875A (en) * | 2021-08-10 | 2021-11-02 | 上海应用技术大学 | Treatment process of acetonitrile waste liquid containing methanol, ethanol and water |
| CN115368274A (en) * | 2022-09-15 | 2022-11-22 | 重庆中吉达环保科技有限公司 | Method for purifying and recovering waste acetonitrile solvent |
| CN116120210A (en) * | 2022-12-29 | 2023-05-16 | 南通立洋化学有限公司 | Purification method for preparing acetonitrile by acetic acid ammoniation method and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111138319A (en) * | 2018-11-06 | 2020-05-12 | 江苏九天高科技股份有限公司 | Method and device for recovering and refining high-purity acetonitrile in polypeptide synthesis |
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| CN113582875A (en) * | 2021-08-10 | 2021-11-02 | 上海应用技术大学 | Treatment process of acetonitrile waste liquid containing methanol, ethanol and water |
| CN115368274A (en) * | 2022-09-15 | 2022-11-22 | 重庆中吉达环保科技有限公司 | Method for purifying and recovering waste acetonitrile solvent |
| CN116120210A (en) * | 2022-12-29 | 2023-05-16 | 南通立洋化学有限公司 | Purification method for preparing acetonitrile by acetic acid ammoniation method and application thereof |
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| CN108794348B (en) | 2021-02-23 |
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