CN108863766A - A method of lactic acid is extracted using the solvent way of distillation - Google Patents

A method of lactic acid is extracted using the solvent way of distillation Download PDF

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Publication number
CN108863766A
CN108863766A CN201810745613.6A CN201810745613A CN108863766A CN 108863766 A CN108863766 A CN 108863766A CN 201810745613 A CN201810745613 A CN 201810745613A CN 108863766 A CN108863766 A CN 108863766A
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lactic acid
organic solvent
solvent
variety
solution
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CN201810745613.6A
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Chinese (zh)
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李荣杰
潘声龙
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Anhui BBCA Fermentation Technology Engineering Research Co Ltd
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Anhui BBCA Fermentation Technology Engineering Research Co Ltd
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Priority to CN201810745613.6A priority Critical patent/CN108863766A/en
Publication of CN108863766A publication Critical patent/CN108863766A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42Separation; Purification; Stabilisation; Use of additives
    • C07C51/43Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
    • C07C51/44Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation

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  • 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 invention belongs to chemical fields, propose a kind of method for extracting lactic acid using the solvent way of distillation, include the following steps:1) crude product solution containing lactic acid is sufficiently mixed with organic solvent, make lactic acid molecules be effectively transferred to organic solvent by the method for distillation or lactic acid is made, simultaneously from distilling in mixture or distilling lactic acid individually from organic solvent, to obtain the lactic acid of the organic phase containing lactic acid or purifying with organic solvent;2) it directly acquires lactic acid obtained in step 1) or is further purified to obtain the lactic acid of high-purity or mixes the organic solvent containing lactic acid with water, obtain lactic acid aqueous solution, it further obtains the lactic acid of high-purity or mixes the organic solvent containing lactic acid with alkaline solution, lactate solution is obtained, the lactate of high-purity is further obtained.More pure lactic acid, lactate and/or other lactic products can be made by a variety of traditional methods known to industry technical staff into the lactic acid in organic phase.

Description

A method of lactic acid is extracted using the solvent way of distillation
Technical field
The present invention relates to chemical fields, specifically, relating to the use of the method that the solvent way of distillation extracts lactic acid.
Background technique
Lactic acid (D-ALPHA-Hydroxypropionic acid, Pfansteihl, DL-LACTIC ACID) is also known as Lactic acid mainly using starch biomass as raw material It is produced through microbial fermentation or using chemical synthesis, it is all multiple to be widely used in food, medicine, chemical industry, new material, feed etc. Want industrial field.Existing lactic acid (D-ALPHA-Hydroxypropionic acid, Pfansteihl, DL-LACTIC ACID) production technology is mostly that fermentation method produces, lactic acid (D-ALPHA-Hydroxypropionic acid, Pfansteihl, DL-LACTIC ACID) extractive technique mainly has solvent extraction technology, molecular distillation technique, membrane separation technique, chromatographic isolation skill Art etc..
As the industries such as food, medicine, chemical industry, new material are to the product of lactic acid (D-ALPHA-Hydroxypropionic acid, Pfansteihl, DL-LACTIC ACID) product Matter requires higher and higher, the especially application and development of polylactic acid (D-ALPHA-Hydroxypropionic acid, Pfansteihl, DL-LACTIC ACID) material, to monomer original More stringent requirements are proposed for the quality of material lactic acid (D-ALPHA-Hydroxypropionic acid, Pfansteihl, DL-LACTIC ACID).
More economical and effective high-pure lactic acid (D-ALPHA-Hydroxypropionic acid, Pfansteihl, DL-LACTIC ACID) is prepared method proposes a kind of Method.
Summary of the invention
The invention proposes a kind of to extract the side of lactic acid (D-ALPHA-Hydroxypropionic acid, Pfansteihl, DL-LACTIC ACID) using the solvent way of distillation Method.The solvent way of distillation be exactly distilled using solvent be dehydrated or (and) de- volatile material to be to reach point of target product From, purifying and extract purpose.Volatile material includes inorganic matter, organic matter, can also be solvent itself.
Technical scheme is as follows:
A method of lactic acid being extracted using the solvent way of distillation, the lactic acid is D-ALPHA-Hydroxypropionic acid, in Pfansteihl, DL-LACTIC ACID It is one or more;It includes the following steps:
1) crude product solution containing lactic acid is sufficiently mixed with organic solvent, by the method for distillation lactic acid molecules is had It is transferred to organic solvent or distills lactic acid from mixture simultaneously with organic solvent or make lactic acid individually from organic to effect It is distilled in solvent, obtains lactic acid (the D- cream of the organic phase containing lactic acid (D-ALPHA-Hydroxypropionic acid, Pfansteihl, DL-LACTIC ACID) or purifying Acid, Pfansteihl, DL-LACTIC ACID);
2) it directly acquires lactic acid obtained in step 1) or is further purified to obtain the lactic acid of high-purity or lactic acid will be contained Organic solvent mixed with water, obtain lactic acid aqueous solution, further obtain high-purity lactic acid or will be organic molten containing lactic acid Agent is mixed with alkaline solution, obtains lactate solution, further obtains the lactate of high-purity.
Wherein, the crude product solution containing lactic acid (D-ALPHA-Hydroxypropionic acid, Pfansteihl, DL-LACTIC ACID) includes one in following solution Kind is a variety of:(1) lactic acid (D-ALPHA-Hydroxypropionic acid, Pfansteihl, DL-LACTIC ACID) fermentation liquid being directly prepared by fermentation;(2) containing cream Lactic acid (D-ALPHA-Hydroxypropionic acid, Pfansteihl, DL-LACTIC ACID) fermentation liquid of sour (D-ALPHA-Hydroxypropionic acid, Pfansteihl, DL-LACTIC ACID) salt, passes through acidolysis lactic acid Raw lactic acid (D-ALPHA-Hydroxypropionic acid, the Pfansteihl, DL-LACTIC ACID) solution obtained after (D-ALPHA-Hydroxypropionic acid, Pfansteihl, DL-LACTIC ACID) salt;(3) pass through The solution containing lactic acid (D-ALPHA-Hydroxypropionic acid, Pfansteihl, DL-LACTIC ACID) that other approach obtain.
Wherein, the organic solvent is selected from the mixture of a kind of following organic compound or a variety of organic compounds:
Esters, ketone, ethers, alcohols, phosphoric acid ester, phosphorus oxygen class, sulphur oxygen class, phosphine sulphur class, amine, amides, alkanes And other organic compounds;The boiling point of the organic compound is all larger than 100 DEG C under normal pressure.
Preferably, the esters include one of amyl acetate, tributyl citrate or a variety of;Ketone includes 2- heptan Ketone;Ethers includes butyl ether;Alcohols includes one of the higher alcohols of octanol, certain herbaceous plants with big flowers alcohol, laruyl alcohol, carbon atom number from 14 to 24 or more The mixture of kind;Phosphoric acid ester includes one of tributyl phosphate, P507, P204 or a variety of;Phosphorus oxygen class includes trioctylphosphine oxygen Phosphine;Sulphur oxygen class includes one of dimethyl sulfone, dimethyl sulfoxide or a variety of;Phosphine sulphur class includes triisobutyl phosphine sulfide;Amine Including one of trioctylamine, three certain herbaceous plants with big flowers amine, Alamine 304, three pungent certain herbaceous plants with big flowers alkyl tertiary amines or a variety of mixtures;Amides include N.N- dibutyl formamide;Alkanes include one of the alkane of octane, certain herbaceous plants with big flowers alkane, carbon atom number from 12 to 24 or a variety of mixed Close object.
Wherein, the mixing ratio of the crude product solution containing lactic acid (D-ALPHA-Hydroxypropionic acid, Pfansteihl, DL-LACTIC ACID) and organic solvent Example is 1:100~100:1.
Wherein, the condition of the solvent distillation is vacuum distillation, and vapo(u)rizing temperature is 0 DEG C~250 DEG C.
Wherein, the step 2) is specially:The organic solvent and water of lactic acid (D-ALPHA-Hydroxypropionic acid, Pfansteihl, DL-LACTIC ACID) will be contained Mixing, lactic acid (D-ALPHA-Hydroxypropionic acid, the Pfansteihl, DL-LACTIC ACID) aqueous solution purified;Or will containing lactic acid (D-ALPHA-Hydroxypropionic acid, Pfansteihl, DL-LACTIC ACID) organic solvent mixed with alkaline solution, obtain lactic acid (D-ALPHA-Hydroxypropionic acid, Pfansteihl, DL-LACTIC ACID) salting liquid.
Organic solvent after separating lactic acid (D-ALPHA-Hydroxypropionic acid, Pfansteihl, DL-LACTIC ACID) can return in step 1) and be recycled.
The present invention relates to operation be unless otherwise specified this field routine operation, related distillation equipment can be Known Conventional vaporizer (such as single effect evaporator or multi-effect evaporator or MVR evaporator etc.) or highly efficient in industry Evaporator (such as scraper evaporator, short-path evaporator, molecular distillation equipment etc.).Distillation equipment referred to above can be independent Use, can also multiple combinations carry out using.
On the basis of common knowledge of the art, above-mentioned each optimum condition, can be combined with each other, obtain specific embodiment party Formula.
The beneficial effects of the present invention are:
The solvent way of distillation of the present invention extracts lactic acid (D-ALPHA-Hydroxypropionic acid, Pfansteihl, DL-LACTIC ACID), short with process route, Easy to operate, the features such as product purity is high, extract yield is high, environmental pollution is small, avoid traditional lactic acid (D-ALPHA-Hydroxypropionic acid, Pfansteihl, DL-LACTIC ACID) operating process complicated in production technology.It can into the lactic acid (D-ALPHA-Hydroxypropionic acid, Pfansteihl, DL-LACTIC ACID) in organic phase By a variety of traditional methods known to industry technical staff be made more pure lactic acid (D-ALPHA-Hydroxypropionic acid, Pfansteihl, DL-LACTIC ACID), lactic acid (D-ALPHA-Hydroxypropionic acid, Pfansteihl, DL-LACTIC ACID) salt and/or other lactic acid (D-ALPHA-Hydroxypropionic acid, Pfansteihl, DL-LACTIC ACID) produce Product.
Specific embodiment
The preferred embodiment of the present invention is described in detail below in conjunction with embodiment.It will be appreciated that following real Providing merely to play the purpose of explanation for example is applied, is not used to limit the scope of the present invention.The skill of this field Without departing from the spirit and purpose of the present invention, the various modifications and replacement carry out to the present invention are accordingly to be regarded as this to art personnel The technology scope of invention.
Embodiment 1
Taking concentration is 50% crude product Pfansteihl solution 100g, organic solvent 455g (wherein three pungent ammonium 182g, eight charcoal alcohol 45g, kerosene 228g) it is put in three-necked flask;
Above-mentioned mixed liquor is concentrated in vacuo in 80 DEG C, is concentrated into that there is no condensed waters to go out, obtains containing Pfansteihl Organic solvent.Organic solvent containing Pfansteihl is transferred in another three-necked flask.Add water with it is organic molten containing Pfansteihl Agent is in 90 DEG C of mixing then by the isolated solution containing Pfansteihl of organic solvent.
It is computed, the yield of Pfansteihl is 92.5%;
Through detecting, the purity of isolated Pfansteihl is 99%.
Although above having used general explanation, specific embodiment and example, the present invention is made to retouch in detail It states, but on the basis of the present invention, certain supplement and optimization can be made to the discrimination model of this method.Therefore, without departing from These modifications or improvements on the basis of spirit of that invention, fall within the scope of the claimed invention.

Claims (7)

1. a kind of method for extracting lactic acid using the solvent way of distillation, the lactic acid is D-ALPHA-Hydroxypropionic acid, Pfansteihl, one in DL-LACTIC ACID Kind is a variety of;It is characterised in that it includes following steps:
1) crude product solution containing lactic acid is sufficiently mixed with organic solvent, lactic acid molecules is made effectively by the method for distillation It is transferred to organic solvent or lactic acid and organic solvent is made to distill from mixture simultaneously or make lactic acid individually from organic solvent In distill, obtain the lactic acid of the organic phase containing lactic acid or purifying;
2) it directly acquires lactic acid obtained in step 1) or be further purified and obtains the lactic acid of high-purity or by having containing lactic acid Solvent is mixed with water, obtains lactic acid aqueous solution, further obtain high-purity lactic acid or by the organic solvent containing lactic acid with Alkaline solution mixing, obtains lactate solution, further obtains the lactate of high-purity.
2. the method according to claim 1, wherein the crude product solution containing lactic acid includes in following solution It is one or more:(1) lactic fermentation liquid being directly prepared by fermentation;(2) containing the lactic fermentation liquid of lactate, lead to Cross the raw lactic acid solution obtained after acidolysis lactate;(3) solution containing lactic acid obtained by other approach.
3. the method according to claim 1, wherein the organic solvent be selected from a kind of following organic compound or The mixture of a variety of organic compounds:
Esters, ketone, ethers, alcohols, phosphoric acid ester, phosphorus oxygen class, sulphur oxygen class, phosphine sulphur class, amine, amides, alkanes and its His organic compound;The boiling point of the organic compound is all larger than 100 DEG C under normal pressure.
4. according to the method described in claim 3, it is characterized in that, the esters include amyl acetate, in tributyl citrate It is one or more;Ketone includes 2-HEPTANONE;Ethers includes butyl ether;Alcohols include octanol, certain herbaceous plants with big flowers alcohol, laruyl alcohol, carbon atom number from One of 14 to 24 higher alcohols or a variety of mixtures;Phosphoric acid ester includes one of tributyl phosphate, P507, P204 Or it is a variety of;Phosphorus oxygen class includes trioctylphosphine oxide (TOPO);Sulphur oxygen class includes one of dimethyl sulfone, dimethyl sulfoxide or a variety of;Phosphine sulphur Class includes triisobutyl phosphine sulfide;Amine include one of trioctylamine, three certain herbaceous plants with big flowers amine, Alamine 304, three pungent certain herbaceous plants with big flowers alkyl tertiary amines or A variety of mixtures;Amides include N.N- dibutyl formamide;Alkanes include octane, certain herbaceous plants with big flowers alkane, carbon atom number from 12 to 24 One of alkane or a variety of mixtures.
5. method according to any one of claims 1 to 4, which is characterized in that the crude product solution containing lactic acid with have The mixed proportion of solvent is 1:100~100:1.
6. method according to any one of claims 1 to 4, which is characterized in that the condition of the solvent distillation is that decompression is steamed It evaporates, vapo(u)rizing temperature is 0 DEG C~250 DEG C.
7. method according to any one of claims 1 to 4, which is characterized in that the step 2) is specially:Lactic acid will be contained Organic solvent mixed with water, the lactic acid aqueous solution purified;Or mix the organic solvent containing lactic acid with alkaline solution, Obtain lactate solution.
CN201810745613.6A 2018-07-09 2018-07-09 A method of lactic acid is extracted using the solvent way of distillation Pending CN108863766A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114591164A (en) * 2022-01-29 2022-06-07 安徽丰原发酵技术工程研究有限公司 Lactic acid purification method
CN115991646A (en) * 2021-10-18 2023-04-21 上海凯赛生物技术股份有限公司 Method for separating and extracting lactic acid, lactic acid product and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107281778A (en) * 2017-06-09 2017-10-24 安徽丰原发酵技术工程研究有限公司 A kind of extraction separating method of organic acid
CN107324989A (en) * 2017-06-09 2017-11-07 安徽丰原发酵技术工程研究有限公司 It is a kind of by being dehydrated the method that extraction prepares lactic acid and lactide

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107281778A (en) * 2017-06-09 2017-10-24 安徽丰原发酵技术工程研究有限公司 A kind of extraction separating method of organic acid
CN107324989A (en) * 2017-06-09 2017-11-07 安徽丰原发酵技术工程研究有限公司 It is a kind of by being dehydrated the method that extraction prepares lactic acid and lactide

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115991646A (en) * 2021-10-18 2023-04-21 上海凯赛生物技术股份有限公司 Method for separating and extracting lactic acid, lactic acid product and preparation method thereof
CN114591164A (en) * 2022-01-29 2022-06-07 安徽丰原发酵技术工程研究有限公司 Lactic acid purification method
CN114591164B (en) * 2022-01-29 2023-11-24 安徽丰原发酵技术工程研究有限公司 Purification method of lactic acid

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Application publication date: 20181123