CN110483251A - The recycling of Carbaspirin mother liquor of calcium serialization ethyl alcohol and salicylic acid removing sulfuldioxide - Google Patents
The recycling of Carbaspirin mother liquor of calcium serialization ethyl alcohol and salicylic acid removing sulfuldioxide Download PDFInfo
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- CN110483251A CN110483251A CN201910838440.7A CN201910838440A CN110483251A CN 110483251 A CN110483251 A CN 110483251A CN 201910838440 A CN201910838440 A CN 201910838440A CN 110483251 A CN110483251 A CN 110483251A
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- Prior art keywords
- ethyl alcohol
- mother liquor
- salicylic acid
- calcium
- carbaspirin
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 99
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 235000019441 ethanol Nutrition 0.000 title claims abstract description 51
- 229960004889 salicylic acid Drugs 0.000 title claims abstract description 48
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 239000012452 mother liquor Substances 0.000 title claims abstract description 37
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 239000011575 calcium Substances 0.000 title claims abstract description 31
- 229910052791 calcium Inorganic materials 0.000 title claims abstract description 31
- 238000004064 recycling Methods 0.000 title claims abstract description 25
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 238000005516 engineering process Methods 0.000 claims abstract description 10
- 239000007787 solid Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 239000002253 acid Substances 0.000 claims description 18
- 239000000047 product Substances 0.000 claims description 16
- 240000000203 Salix gracilistyla Species 0.000 claims description 14
- 238000000605 extraction Methods 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 9
- 239000000428 dust Substances 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 5
- 238000004821 distillation Methods 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 241000219000 Populus Species 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 238000005057 refrigeration Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 13
- 230000008901 benefit Effects 0.000 abstract description 3
- 235000001465 calcium Nutrition 0.000 description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- BSYNRYMUTXBXSQ-UHFFFAOYSA-N Aspirin Chemical compound CC(=O)OC1=CC=CC=C1C(O)=O BSYNRYMUTXBXSQ-UHFFFAOYSA-N 0.000 description 5
- 229960004105 carbasalate calcium Drugs 0.000 description 5
- VYMUGTALCSPLDM-UHFFFAOYSA-L carbasalate calcium Chemical compound [Ca+2].NC(N)=O.CC(=O)OC1=CC=CC=C1C([O-])=O.CC(=O)OC1=CC=CC=C1C([O-])=O VYMUGTALCSPLDM-UHFFFAOYSA-L 0.000 description 5
- 229960001138 acetylsalicylic acid Drugs 0.000 description 4
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 235000011132 calcium sulphate Nutrition 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000010826 pharmaceutical waste Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- NZZLTKHBCHMMOJ-UHFFFAOYSA-N 2-acetyloxybenzoic acid;urea Chemical compound NC(N)=O.CC(=O)OC1=CC=CC=C1C(O)=O NZZLTKHBCHMMOJ-UHFFFAOYSA-N 0.000 description 1
- LODHFNUFVRVKTH-ZHACJKMWSA-N 2-hydroxy-n'-[(e)-3-phenylprop-2-enoyl]benzohydrazide Chemical compound OC1=CC=CC=C1C(=O)NNC(=O)\C=C\C1=CC=CC=C1 LODHFNUFVRVKTH-ZHACJKMWSA-N 0.000 description 1
- VHBSECWYEFJRNV-UHFFFAOYSA-N 2-hydroxybenzoic acid Chemical compound OC(=O)C1=CC=CC=C1O.OC(=O)C1=CC=CC=C1O VHBSECWYEFJRNV-UHFFFAOYSA-N 0.000 description 1
- 208000002874 Acne Vulgaris Diseases 0.000 description 1
- 208000020154 Acnes Diseases 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 101000783577 Dendroaspis angusticeps Thrombostatin Proteins 0.000 description 1
- 101000783578 Dendroaspis jamesoni kaimosae Dendroaspin Proteins 0.000 description 1
- 206010020649 Hyperkeratosis Diseases 0.000 description 1
- 206010066295 Keratosis pilaris Diseases 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 201000004681 Psoriasis Diseases 0.000 description 1
- 208000000260 Warts Diseases 0.000 description 1
- WLQXPAUZYVXSNE-UHFFFAOYSA-N [Ca].O[N+]([O-])=O Chemical compound [Ca].O[N+]([O-])=O WLQXPAUZYVXSNE-UHFFFAOYSA-N 0.000 description 1
- 206010000496 acne Diseases 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229940121363 anti-inflammatory agent Drugs 0.000 description 1
- 239000002260 anti-inflammatory agent Substances 0.000 description 1
- 229940127218 antiplatelet drug Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 239000001175 calcium sulphate Substances 0.000 description 1
- KRALOLGXHLZTCW-UHFFFAOYSA-L calcium;2-acetyloxybenzoate Chemical compound [Ca+2].CC(=O)OC1=CC=CC=C1C([O-])=O.CC(=O)OC1=CC=CC=C1C([O-])=O KRALOLGXHLZTCW-UHFFFAOYSA-L 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- ZWWCURLKEXEFQT-UHFFFAOYSA-N dinitrogen pentoxide Inorganic materials [O-][N+](=O)O[N+]([O-])=O ZWWCURLKEXEFQT-UHFFFAOYSA-N 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 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
- 238000010438 heat treatment Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 230000000474 nursing effect Effects 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000000106 platelet aggregation inhibitor Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 239000002453 shampoo Substances 0.000 description 1
- 201000010153 skin papilloma Diseases 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention provides a kind of recycling of Carbaspirin mother liquor of calcium serialization ethyl alcohol and salicylic acid removing sulfuldioxides.The technology realizes the recycling of Carbaspirin mother liquor of calcium serialization ethyl alcohol and salicylic acid removing, develops the feasibility process route suitable for the recycling of Carbaspirin mother liquor of calcium serialization ethyl alcohol and salicylic acid removing sulfuldioxide, which guarantees concentration of alcohol >=95% of recycling；Ethanol content is lower than 100ppm in liquid after removing ethyl alcohol, and salicylic acid content is lower than 3g/L in liquid after removing ethyl alcohol, and the solid salicylic acid purity of recycling reaches 95% or more.The advantages that this method has simple process, and device is simple, and product purity is high.
Description
[technical field]
The invention belongs to field of medicine and chemical technology, and in particular to a kind of recycling of Carbaspirin mother liquor of calcium serialization ethyl alcohol and bigcatkin willow
Sour removing sulfuldioxide.
[background technique]
Carbasalate calcium (Carbasalate calcium) it be tylcalsin (calcium salt of aspirin) and urea
Chelate, be aspirin derivatives, the same aspirin of curative effect, side effect is low, good water solubility, thus is weighed extensively
Depending on.It is clinically a kind of antalgesic, alexipyretic and anti-inflammatory agent and a kind of platelet aggregation inhibitor.
Salicylic acid (Salicylic acid) also known as 2 hydroxybenzoic acid (English name 2-
Hydroxybenzenecarboxylic acid), appearance is white needle-like crystals or hairy crystalline powder, is allowed slightly yellow
Color and pink are soluble in ethyl alcohol, ether, chloroform, are slightly soluble in water, dissolve in boiling water, stablize under room temperature, sharply heat resolve
For phenol and carbon dioxide, there is the general character of part acid.Clinically, salicylic acid is widely used in external application and smears class drug
In, all use salicylic acid, such as the product of many treatment acnes just to use salicylic acid in many skin nursing products.There are also one
A little treat all uses salicylic acid in the products of diseases such as psoriasis, callus, keratosis pilaris, wart, in these products, salicylic acid master
The effects of playing cutin-softening, sterilization, treatment acne, there are also be also added with salicylic acid inside some shampoos.
Salicylic acid is a kind of very wide raw material of the industrial applications such as medicine, chemical industry.And salicylic acid is in the production of carbasalate calcium
Belong to impurity in the process, salicylic acid also contained in the mother liquor of carbasalate calcium, therefore, study a kind of simple process, it is easy to operate,
Serialization recycles ethyl alcohol in slave Carbaspirin mother liquor of calcium at low cost and the bigcatkin willow acid product for obtaining higher quality has centainly
Economy and environmental benefit.
Chinese patent CN201811268231.5 discloses a kind of preparation method of carbasalate calcium, but does not relate to
The recycling of Carbaspirin mother liquor of calcium.
Chinese patent CN201410530287.9 discloses a kind of method that pyridine is recycled from pharmaceutical waste liquor, related
Pharmaceutical waste liquor is different.
Chinese patent CN201610791621.5 discloses a kind of aspirin raffinate treatment process, and related pharmacy is useless
Liquid is different.
The present invention realizes the recycling of Carbaspirin mother liquor of calcium serialization ethyl alcohol and salicylic acid removing, develops suitable for kappa
The feasibility process route of the recycling of woods mother liquor of calcium serialization ethyl alcohol and salicylic acid removing sulfuldioxide, the technique guarantee continuous fine fraction
Separate out overhead ethanol concentration >=95%；Tower bottom ethanol content is lower than 100ppm, and the salicylic acid content after removing is lower than 3g/L, recycling
Solid salicylic acid purity reach 95% or more.
[summary of the invention]
[technical problems to be solved]
Technical problem to be solved by the invention is to provide a kind of recycling of Carbaspirin mother liquor of calcium serialization ethyl alcohol and bigcatkin willows
Sour removing sulfuldioxide, by carrying out purification removal impurity serialization recycling ethyl alcohol to Carbaspirin mother liquor of calcium and obtaining higher quality
Bigcatkin willow acid product.
[technical solution]
Carbaspirin mother liquor of calcium serialization ethyl alcohol recycling of the present invention and salicylic acid removing sulfuldioxide, the Carbaspirin
Mother liquor of calcium is to sequentially add aspirin, ammonium hydroxide, anhydrous nitric acid calcium, urea using ethyl alcohol or methanol as solvent, and heating stirring is molten
Solution, the mother liquor obtained after filtering, it is characterised in that include the following steps:
(1) rectifying: by the mixture rectifying of Carbaspirin mother liquor of calcium and water, the mixture of overhead extraction second alcohol and water；
(2) secondary rectifying: the rectifying again of tower bottom mixture, the mixture of tower bottom recovered water and salicylic acid and ammonium nitrate；
(3) adjust pH: kettle liquid is cooled to room temperature, and adds water to solid dissolution, with dust technology tune pH to acidity, analysis in acid out tank
Salicylic acid out stirs evenly, and stands；
(4) it filters: said mixture is obtained into the higher bigcatkin willow acid product of purity after being filtered, washed, drying.
The recycling of Carbaspirin mother liquor of calcium serialization ethyl alcohol and salicylic acid removing sulfuldioxide, it is characterised in that the rectifying of step (1)
For conventional distillation, several times plus water takes the ethyl alcohol in kappa mother liquor out of, and the mass values of mother liquor and water are 5~10, guarantees tower top
The ethyl alcohol mass fraction of extraction is 95%.
The recycling of Carbaspirin mother liquor of calcium serialization ethyl alcohol and salicylic acid removing sulfuldioxide, it is characterised in that the rectifying of step (2)
For conventional distillation, guarantee that the concentration of alcohol of tower bottom is less than 100ppm.
The recycling of Carbaspirin mother liquor of calcium serialization ethyl alcohol and salicylic acid removing sulfuldioxide, it is characterised in that the nitric acid of step (3)
For dust technology, mass concentration is that 40%~68%, pH is adjusted to 1~3.
The recycling of Carbaspirin mother liquor of calcium serialization ethyl alcohol and salicylic acid removing sulfuldioxide, it is characterised in that the filtering of step (4)
It is to use diatomite for filtrate circulating filtration 30~60 minutes, drying machine is using vacuum freeze drier, obtained bigcatkin willow
The purity of acid product is 99% or more, and salicylic acid content is lower than 3g/L in filtrate.
It is of the invention containing ingredients such as ethyl alcohol, water, ammonium nitrate and carbasalate calciums in Carbaspirin mother liquor of calcium in the present invention
It is mainly characterized by and recycles ethyl alcohol with rectification process serialization and obtain the bigcatkin willow acid product of higher quality in acid condition.
Ethyl alcohol can preferably be recycled using two-tower rectification in distillation process in the present invention, reduce the concentration of alcohol of tower bottom,
Convenient for obtaining the bigcatkin willow acid product of higher quality.
Ammonium nitrate solid can be precipitated after kettle liquid is cooled to room temperature after rectifying in the present invention, water need to be added to make it dissolve.
Dust technology is used in the present invention in pH adjustment process, has ammonium nitrate in liquid mixture, will not be introduced new miscellaneous
Matter.It is because calcium sulfate precipitation can be generated without using dilute sulfuric acid, calcium sulphate solid slightly soluble will lead to the bigcatkin willow acid product of recycling
Purity reduces；It is the volatility because of hydrochloric acid without using hydrochloric acid, will lead to a large amount of hydrochloric acid volatilization in use process, waste raw material
And it will cause pollution.
PH is adjusted to 1~3 in the present invention, and dust technology dosage is very few to will lead to salicylic precipitating not exclusively, Carbaspirin
Salicylic acid removing in mother liquor of calcium is incomplete.
The filter type that well known diversified forms can be used in the present invention, such as pore type filter, it is therefore an objective to remove molten
Salicylic acid solid in liquid.It is filtering agent circulating filtration 30~60 minutes present invention preferably employs diatomite.The heap of the diatomite
Density is 0.36~0.40g/cm3, permeability is 0.30~0.35 darcy.The purpose of circulating filtration is preferably to remove in solution
Salicylic acid solid.
Vacuum freeze drier is used in the present invention in the drying process, the reason is that salicylic acid distils at 76 DEG C, high temperature
The phenomenon that distils can occur for lower dry salicylic acid, and the yield of bigcatkin willow acid product is caused to decline.
[beneficial effect]
Advantages of the present invention:
Production process is simply convenient for operating, and number of devices is few, and production capacity is big, and energy consumption is small；Operator is few, labour
Intensity is low；Production environment is good, and pollution is few；Consumption of raw materials is few, high income；Product purity is high, stability is good, convenient for industrial metaplasia
It produces, serialization can recycle ethyl alcohol from Carbaspirin mother liquor of calcium and obtain the bigcatkin willow acid product of higher quality.
[specific embodiment]
Embodiment 1:
Carbaspirin mother liquor of calcium 58kg and 3kg water is mixed, is heated to 65~100 DEG C, overhead extraction mass fraction is
95% ethyl alcohol 45kg adds the ethyl alcohol that water 2kg overhead extraction 2kg mass fraction is 95%, adds water 2kg overhead extraction
The ethyl alcohol that 2kg mass fraction is 95%.Kettle liquid is cooled to room temperature, and the dust technology that mass concentration is 50% after 10kg water dissolves is added
Adjusting pH value is 2, and salicylic acid is precipitated, stirs evenly, and the sterling salicylic acid of content 99.5% is obtained after being filtered, washed, drying after standing,
Salicylic acid content is 1.8g/L in filtrate.
Embodiment 2:
Carbaspirin mother liquor of calcium 110kg and 6kg water is mixed, is heated to 65~100 DEG C, overhead extraction mass fraction is
95% ethyl alcohol 90kg adds the ethyl alcohol that water 4kg overhead extraction 4kg mass fraction is 95%, adds water 4kg overhead extraction
The ethyl alcohol that 4kg mass fraction is 95%.Kettle liquid is cooled to room temperature, and the dust technology that mass concentration is 60% after 20kg water dissolves is added
Adjusting pH value is 1.5, and salicylic acid is precipitated, stirs evenly, and the sterling bigcatkin willow of content 99.2% is obtained after being filtered, washed, drying after standing
Acid, salicylic acid content is 2g/L in filtrate.
Embodiment 3:
Carbaspirin mother liquor of calcium 150kg and 10kg water is mixed, is heated to 65~100 DEG C, overhead extraction mass fraction is
95% ethyl alcohol 120kg adds the ethyl alcohol that water 6kg overhead extraction 6kg mass fraction is 95%, adds water 6kg tower top and adopt
The ethyl alcohol that 6kg mass fraction is 95% out.Kettle liquid is cooled to room temperature, and dilute nitre that mass concentration is 50% after 25kg water dissolves is added
It is 2.5 that acid, which adjusts pH value, and salicylic acid is precipitated, stirs evenly, the sterling water of content 99.1% is obtained after being filtered, washed, drying after standing
Poplar is sour, and salicylic acid content is 2.1g/L in filtrate.
Claims (5)
1. the recycling of Carbaspirin mother liquor of calcium serialization ethyl alcohol and salicylic acid removing sulfuldioxide, it is characterised in that include the following steps:
(1) rectifying: by the mixture rectifying of Carbaspirin mother liquor of calcium and water, the mixture of overhead extraction second alcohol and water；
(2) secondary rectifying: the rectifying again of tower bottom mixture, the mixture of tower bottom recovered water and salicylic acid and ammonium nitrate；
(3) adjust pH: kettle liquid is cooled to room temperature, and adds water to solid dissolution, and with dust technology tune pH to acidity in acid out tank, water is precipitated
Poplar acid, stirs evenly, and stands；
(4) it filters: said mixture is obtained into the higher bigcatkin willow acid product of purity after being filtered, washed, drying.
2. Carbaspirin mother liquor of calcium serialization ethyl alcohol recycling according to claim 1 and salicylic acid removing sulfuldioxide, feature
The rectifying for being step (1) is conventional distillation, and several times plus water takes the ethyl alcohol in kappa mother liquor, the volume ratio of mother liquor and water out of
It is 5~10, guarantees that the ethyl alcohol mass fraction of overhead extraction is 95%.
3. Carbaspirin mother liquor of calcium serialization ethyl alcohol recycling according to claim 1 and salicylic acid removing sulfuldioxide, feature
The rectifying for being step (2) is conventional distillation, guarantees that the concentration of alcohol of tower bottom is less than 100ppm.
4. Carbaspirin mother liquor of calcium serialization ethyl alcohol recycling according to claim 1 and salicylic acid removing sulfuldioxide, feature
The nitric acid for being step (3) is dust technology, and mass concentration is that 40%~68%, pH is adjusted to 1~3.
5. Carbaspirin mother liquor of calcium serialization ethyl alcohol recycling according to claim 1 and salicylic acid removing sulfuldioxide, feature
The filtering for being step (4) is to use diatomite for filtrate circulating filtration 30~60 minutes, and drying machine is using vacuum refrigeration
Drying machine, the purity of obtained bigcatkin willow acid product are 99% or more.
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| CN108329205A (en) * | 2018-03-09 | 2018-07-27 | 山东新华制药股份有限公司 | It is double（Aspirin）The preparation method of calcium carbamide compound |
-
2019
- 2019-09-05 CN CN201910838440.7A patent/CN110483251A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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