CN103497100A - Double-stage purification method of long chain dicarboxylic acid aqueous phase - Google Patents
Double-stage purification method of long chain dicarboxylic acid aqueous phase Download PDFInfo
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- 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
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- 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
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Abstract
The invention discloses a double-stage purification method of a long chain dicarboxylic acid aqueous phase. The double-stage purification method comprises the following steps: (1) heating and demulsifying terminated fermentation broth of long chain dicarboxylic acid produced by a fermentation method, and filtering the terminated fermentation broth through a ceramic microfiltration membrane to obtain a microfiltration membrane supernatant layer; (2) diluting the microfiltration membrane supernatant, and adding an oxidizing agent under a weak alkaline condition to react to obtain supernatant; or diluting the microfiltration membrane supernatant, and adding the oxidizing agent under a weak acidic condition to react to obtain the supernatant; or diluting the microfiltration membrane supernatant, filtering the microfiltration membrane supernatant through a microfiltration membrane, diluting, and adding the oxidizing agent to react to obtain the supernatant; (3) regulating the pH value of the supernatant to 3.0-5.0 through an acid, maintaining the temperature for 1 h, filter pressing through a plate frame, washing a long chain dicarboxylic acid filter cake layer through acidic washing water of a saturated sodium salt, press filtering the acidic water of saturated salt in the dicarboxylic acid filter cake, removing the sodium salt from the pure water, and drying to obtain a long chain dicarboxylic acid product. The double-stage purification method disclosed by the invention is short in process route, low in production cost, high in yield, high in purity, good in aqueous phase crystal morphology, capable of solving the defects of a current aqueous phase method product of low purity, high protein content and bad color and luster, and beneficial for large-scale industrial production.
Description
Technical field
The present invention relates to alkane fermentation and prepare water process for purification in the long-chain biatomic acid process, be specifically related to the two stage methods of purification of long-chain biatomic acid water.
Background technology
With C
11-C
18straight-chain paraffin is raw material, by P450 enzyme in the Candida tropicalis born of the same parents, is the Straight chain diatomic acid that oxidation generates the both-end carboxyl.Biological fermentation process mild condition, simple process, product are easy to get, but polymerization-grade product purification method still is confined to organic solvent process for refining technology, and there is drawbacks such as polluting weight, severe operational environment in it, and high-quality diprotic acid water purifying technique is still in groping.This is due to fermentation system, to be the mixture of residual alkane, emulsion, thalline, substratum and various meta-bolitess.Because long-chain biatomic acid solubleness in water is very low, often with the bag of carrying the organic impuritys such as pigment, nitrogen compound secretly, starch phenomenon in the acid out process, and the organic impuritys such as the contained yellow pigment of dicarboxylic acid product are difficult to wash-out in water; Simultaneously, long-chain biatomic acid two ends-COOH group easily and the reductibility group generation esterification such as amino nitrogen etc., directly affects index and the visual appearance of water refined product.
By water treatment processs such as centrifugal separation, filtration method, salting-out process, ion exchange method and membrane separation processes or exist product purity not high, or product recovery rate is low, or the problem such as complex disposal process.CN1351006A utilizes the technique of an acidifying and melting decolouring effectively to reduce the foreign matter content such as protein, organic pigment in product, product appearance is white in color, but when high temperature, can't avoid reacting with the reductibility group, product color is not as good as the organic solvent purified product, and product yield is lower, the melting energy consumption is high, is unsuitable for suitability for industrialized production.
CN1255483A utilizes long-chain biatomic acid list salt crystallisation step effectively to reduce the foreign matter content such as protein and pigment in product, prepares the long-chain biatomic acid product that total acid content is greater than 99%, outward appearance is white in color.This method major part has solved that the long-chain biatomic acid acidifying is separated out and the problem of not wrapping slurry, being mingled with.Due to its single sodium salt still have a side-COOH, under the H+ condition, with the reductibility group, react, therefore product colourity, nitrogen content are higher, be unsuitable for the index request of polymerization-grade product.
The technology that CN1255483A utilizes long-chain biatomic acid list sodium salt crystal and saltouts and combine, overcome above-mentioned single sodium filtrate recycling step, part eliminated-COOH group and reductibility group generation esterification, and quality product increases.Only by single sodium salt crystal technology, still can't eliminate the long-chain biatomic acid product color, quality can not reach the polymerization-grade index.
CN1292072C proposes centrifugal or membrane filtration pre-treatment fermented liquid, acidizing crystal obtains the diprotic acid crude product, the crude product obtained is dropped in acetate solvate to heating by a certain percentage and melt, at 60-100 ℃ of insulation crystallisation by cooling after 30-180 minute, obtain product after solid-liquid separation, drying.Though this method has solved the design that current fermentation method prepares long-chain biatomic acid polymerization-grade Product Process route, the production problem such as have in actual production process that equipment corrosion is serious, severe operational environment, environmental pollution are serious.
Summary of the invention
The object of the invention is to: provide a kind of long-chain biatomic acid water two stage methods of purification, make its product index reach the requirement of polymerization-grade product index, operational path is short, production cost is low, product yield is high, and purity is high, has good water crystal habit, the existing water method product purity of solution is low, protein content is high, the shade deviation shortcoming, is conducive to large-scale industrial production.
Technical solution of the present invention is: the step of the two stage methods of purification of this long-chain biatomic acid water is as follows:
(1) after long-chain biatomic acid is stopped to the fermented liquid heating demulsification type, adopt the ceramic micro filter membrane filtration to remove unconverted alkane, yeast, pigment macromole, obtain the microfiltration membrane supernatant liquid;
(2) getting the microfiltration membrane clear liquid is processed by following a certain method:
(a) the microfiltration membrane clear liquid being diluted to the salinity value is 4% ~ 10%, under weakly alkaline pH7 ~ pH9 condition, and oxidizer after heating, shielding diprotic acid carboxyl reacts with reducing impurity, and after reaction, Plate Filtration goes out clear liquid;
(b) the microfiltration membrane clear liquid being diluted to the salinity value is 4% ~ 10%, under slightly acidic pH5 ~ pH7 condition, and oxidizer after heating, shielding diprotic acid carboxyl reacts with reducing impurity, and after reaction, Plate Filtration goes out clear liquid;
(c) by the microfiltration membrane clear liquid further through ultrafiltration membrance filter, remove most of pigment, protein organic matter, being diluted to the salinity value is 4% ~ 10%, under pH5 ~ pH9 condition, oxidizer after heating, shielding diprotic acid carboxyl reacts with reducing impurity, and after reaction, Plate Filtration goes out clear liquid;
(3) the pending long-chain biatomic acid clear liquid of stirring heating step (2), with acid for adjusting pH value Zhi Jiewen district; After press filtration, with the acidic cleaning water washing long-chain biatomic acid cake layer of saturated sodium salt sodium sulfate, sodium-chlor, sodium carbonate, acid wash water reclaims pending; Press in clean diprotic acid filter cake after saturated hydrochloric acid water, by the further secondary washing of pure water, remove wherein sodium salt, drying, obtain the long-chain biatomic acid product.
Wherein, the heating demulsification type temperature of step (1) is 80 ~ 95 ℃.
Wherein, in (a, b, the c) of step (2), heating and temperature control is at 80 ~ 100 ℃, and oxygenant is clorox or ozone, and its consumption is 2 ~ 8% of microfiltration membrane clear liquid.
Wherein, the temperature of the pending long-chain biatomic acid clear liquid of the stirring heating step (2) of step (3) is 80 ~ 100 ℃, acid is adjusted to Jie Wen district between pH2.5 ~ 7.0, sodium salt is sodium sulfate, sodium-chlor or sodium carbonate, and the acid wash water of saturated sodium salt is chosen a certain or mixing acid of sulfuric acid, phosphoric acid, acetic acid, oxalic acid.
Wherein, it is as follows that acid wash water reclaims pending method: heat the acid wash water to 60 of saturated sodium salt ~ 90 ℃, the gac that adds its amount 1 ~ 3% stirs insulation 30 ~ 60 minutes, whether detect the sodium salt solution salinity after filtering meets the demands, if salinity is added a certain amount of identical sodium salt through the water dilution, pH adds a certain amount of acid when not enough, and sulfuric acid, hydrochloric acid, acetic acid, oxalic acid be one or more mixing acid wherein.
The present invention has the following advantages:
1, shielding reductibility group: for long-chain biatomic acid two ends active group (COOH), there is oxidisability, easily in the acidizing crystal process with fermented liquid in reductibility group generation esterification, thereby the problem that causes the reductibility nitrogen compound to remove, the present invention, by the esterification between oxygenant (clorox, ozone) shielding diprotic acid carboxyl and reducing impurity group, avoids the reductibility group impurity that is difficult to remove to be entrained in product through chemisorption.
2 ,Jie Wen district acidizing crystals are controlled: choose the trickle Jie Wen district between long-chain biatomic acid and single sodium salt thereof, do not repeat long-chain biatomic acid list sodium salt crystal stable region in CN1255483A, not only fully retain the dual nature that long-chain biatomic acid list sodium salt removes pigment, albumen, also reduce to the full extent diprotic acid list sodium salt residual quantity in crystalline mother solution, avoid the cost that mother liquor reclaims to increase and the not high problem of product yield.
3, two stage wash regulation and control: by the difficulties such as the easy residual yellow pigment of acid wash water solution pure water wash-out long-chain biatomic acid filter cake of saturated sodium salt, remove the pigment problem, utilize pure water secondary washing long-chain biatomic acid filter cake, and this type of yellow pigment is also to contain more pigment in the substratum such as yeast extract paste, corn steep liquor, directly affect quality product; Simultaneously, micro-single sodium salt in the further acidifying filter cake of acid wash water, the complete acidifying of long-chain biatomic acid is finished, a saturated brine washing process is also the secondary crystal acidization, complete the after-souring crystallisation process under low impurity environment, and saturated salt acid wash water use repeatly after activated carbon decolorizing is processed.
Embodiment
Further illustrate technical solution of the present invention below in conjunction with specific embodiment, these embodiment can not be interpreted as it is the restriction to technical scheme.
Embodiment 1: according to following steps purification long-chain biatomic acid
(1) SL-AH of concentration 160g/L, pH8.5 is stopped to 95 ℃ of heating demulsification types of fermented liquid, adopt the ceramic micro filter membrane filtration to remove unconverted alkane, yeast, pigment macromole, obtain the microfiltration membrane supernatant liquid;
(2) the microfiltration membrane clear liquid being diluted to the salinity value is 10%, under weakly alkaline pH9.0 condition, is heated to after 100 ℃ add 8% oxygenant clorox of microfiltration membrane clear liquid amount, and shielding diprotic acid carboxyl reacts with reducing impurity, stand-by after reaction;
(3) the pending long-chain biatomic acid clear liquid to 100 ℃ of stirring heating step (2), be adjusted to Jie Wen district pH4.0 with acetic acid; Insulation 1h filter press, with the acidic cleaning water washing long-chain biatomic acid cake layer of saturated sodium sulfate, acid wash water reclaims pending; Press in clean diprotic acid filter cake after saturated hydrochloric acid water, by the further secondary washing of pure water, remove wherein sodium salt, drying, obtain the long-chain biatomic acid product.
Embodiment 2: according to following steps purification long-chain biatomic acid
(1) tridecanyldicarboxylic acid of concentration 160g/L, pH8.5 is stopped to 80 ℃ of heating demulsification types of fermented liquid, adopt the ceramic micro filter membrane filtration to remove unconverted alkane, yeast, pigment macromole, obtain the microfiltration membrane supernatant liquid;
(2) the microfiltration membrane clear liquid being diluted to the salinity value is 4%, under weakly alkaline pH7.8 condition, is heated to after 80 ℃ add 2% oxygenant clorox of microfiltration membrane clear liquid amount, and shielding diprotic acid carboxyl reacts with reducing impurity, stand-by after reaction;
(3) the pending long-chain biatomic acid clear liquid to 80 ℃ of stirring heating step (2), be adjusted to pH 3.5Jie Wen district with sulfuric acid; Insulation 1h filter press, with the acidic cleaning water washing long-chain biatomic acid cake layer of saturated sodium sodium-chlor, acid wash water reclaims pending; Press in clean diprotic acid filter cake after saturated hydrochloric acid water, by the further secondary washing of pure water, remove wherein sodium salt, drying, obtain the long-chain biatomic acid product.
Embodiment 3: according to following steps purification long-chain biatomic acid
(1) 15 carbon dicarboxylic acids of concentration 160g/L, pH8.5 are stopped to 90 ℃ of heating demulsification types of fermented liquid, adopt the ceramic micro filter membrane filtration to remove unconverted alkane, yeast, pigment macromole, obtain the microfiltration membrane supernatant liquid;
(2) the microfiltration membrane clear liquid being diluted to the salinity value is 7%, under weakly alkaline pH8.0 condition, is heated to after 90 ℃ add 5% oxidant, ozone of microfiltration membrane clear liquid amount, and shielding diprotic acid carboxyl reacts with reducing impurity, and after reaction, Plate Filtration goes out clear liquid;
(3) the pending long-chain biatomic acid clear liquid to 95 ℃ of stirring heating step (2), be adjusted to pH5.0 Jie Wen district with the mixing acid of phosphoric acid and oxalic acid; Insulation 1h filter press, with the acidic cleaning water washing long-chain biatomic acid cake layer of saturated sodium carbonate, acid wash water reclaims pending; Press in clean diprotic acid filter cake after saturated hydrochloric acid water, by the further secondary washing of pure water, remove wherein sodium salt, drying, obtain the long-chain biatomic acid product.
Embodiment 4: step (1,3) is with embodiment 1, step (2) is: it is 4% that the microfiltration membrane clear liquid is diluted to the salinity value, under slightly acidic pH6.5 condition, be heated to after 80 ℃ to add 2% oxygenant clorox of microfiltration membrane clear liquid amount, shielding diprotic acid carboxyl reacts with reducing impurity, stand-by after reaction.
Embodiment 5: step (1,3) is with embodiment 2, step (2) is: it is 7% that the microfiltration membrane clear liquid is diluted to the salinity value, under slightly acidic pH6 condition, be heated to after 90 ℃ to add 5% oxygenant clorox of microfiltration membrane clear liquid amount, shielding diprotic acid carboxyl reacts with reducing impurity, stand-by after reaction.
Embodiment 6: step (1,3) is with embodiment 3, step (2) is: it is 10% that the microfiltration membrane clear liquid is diluted to the salinity value, under slightly acidic pH6.8 condition, be heated to after 100 ℃ to add 8% oxidant, ozone of microfiltration membrane clear liquid amount, shielding diprotic acid carboxyl reacts with reducing impurity, stand-by after reaction.
Embodiment 7: step (1,3) is with embodiment 1, step (2) is: by the microfiltration membrane clear liquid further through ultrafiltration membrance filter, remove most of pigment, protein organic matter, being diluted to the salinity value is 4%, under the pH5 condition, be heated to after 80 ℃ 2% the oxygenant clorox with the clear liquid amount, shielding diprotic acid carboxyl react with reducing impurity, reacts Plate Filtration afterwards and goes out clear liquid.
Embodiment 8: step (1,3) is with embodiment 2, step (2) is: by the microfiltration membrane clear liquid further through ultrafiltration membrance filter, remove most of pigment, protein organic matter, being diluted to the salinity value is 7%, under the pH7 condition, be heated to after 90 ℃ 5% the oxygenant clorox with the clear liquid amount, shielding diprotic acid carboxyl react with reducing impurity, reacts Plate Filtration afterwards and goes out clear liquid.
Embodiment 9: step (1,3) is with embodiment 3, step (2) is: by the microfiltration membrane clear liquid further through ultrafiltration membrance filter, remove most of pigment, protein organic matter, being diluted to the salinity value is 5%, under the pH9 condition, be heated to after 100 ℃ 8% the oxidant, ozone with the clear liquid amount, shielding diprotic acid carboxyl react with reducing impurity, reacts Plate Filtration afterwards and goes out clear liquid.
Embodiment 10: it is as follows that acid wash water reclaims pending method: the acid wash water to 60 ℃ that heats saturated sodium salt, the gac that adds its amount 1% stirs insulation 60 minutes, whether detect the sodium salt solution salinity after filtering meets the demands, if salinity is added a certain amount of identical sodium salt through the water dilution, pH adds a certain amount of sulfuric acid when not enough.Press example 1 method and process the long-chain biatomic acid clear liquid, with reclaiming the acid solution washing.
Embodiment 11: it is as follows that acid wash water reclaims pending method: the acid wash water to 75 ℃ that heats saturated sodium salt, the gac that adds its amount 2% stirs insulation 45 minutes, whether detect the sodium salt solution salinity after filtering meets the demands, if salinity is added a certain amount of identical sodium salt through the water dilution, pH adds a certain amount of hydrochloric acid when not enough.Press example 2 methods and process the long-chain biatomic acid clear liquid, with reclaiming the acid solution washing.
Embodiment 12: it is as follows that acid wash water reclaims pending method: the acid wash water to 90 ℃ that heats saturated sodium salt, the gac that adds its amount 3% stirs insulation 30 minutes, whether detect the sodium salt solution salinity after filtering meets the demands, if salinity is added a certain amount of identical sodium salt through the water dilution, pH adds a certain amount of acetic acid when not enough.Press example 3 methods and process the long-chain biatomic acid clear liquid, with reclaiming the acid solution washing.
Extract according to the method described above long-chain biatomic acid, product property is in Table 1:
table 1 example product analysis data
Claims (5)
1. two stage methods of purification of long-chain biatomic acid water is characterized in that the step that this long-chain biatomic acid purifies is as follows:
(1) long-chain biatomic acid stopped to the fermented liquid heating demulsification type or, without heating demulsification type, adopt the ceramic micro filter membrane filtration to remove unconverted alkane, yeast, pigment macromole, obtaining the microfiltration membrane supernatant liquid;
(2) getting the microfiltration membrane clear liquid is processed by following a certain method:
(a) the microfiltration membrane clear liquid being diluted to the salinity value is 4% ~ 10%, under weakly alkaline pH7 ~ pH9 condition, and oxidizer after heating, shielding diprotic acid carboxyl reacts with reducing impurity, and after reaction, Plate Filtration goes out clear liquid;
(b) the microfiltration membrane clear liquid being diluted to the salinity value is 4% ~ 10%, under slightly acidic pH5 ~ pH7 condition, and oxidizer after heating, shielding diprotic acid carboxyl reacts with reducing impurity, and after reaction, Plate Filtration goes out clear liquid;
(c) by the microfiltration membrane clear liquid further through ultrafiltration membrance filter, remove most of pigment, protein organic matter, being diluted to the salinity value is 4% ~ 10%, under pH5 ~ pH9 condition, oxidizer after heating, shielding diprotic acid carboxyl reacts with reducing impurity, and after reaction, Plate Filtration goes out clear liquid;
(3) the pending long-chain biatomic acid clear liquid of stirring heating step (2), with acid for adjusting pH value Zhi Jiewen district; After press filtration, with the acidic cleaning water washing long-chain biatomic acid cake layer of saturated sodium salt sodium sulfate, sodium-chlor, sodium carbonate, acid wash water reclaims pending; Press in clean diprotic acid filter cake after saturated hydrochloric acid water, by the further secondary washing of pure water, remove wherein sodium salt, drying, obtain the long-chain biatomic acid product.
2. two stage methods of purification of long-chain biatomic acid water according to claim 1, it is characterized in that: the heating demulsification type temperature of step (1) is 80 ~ 95 ℃.
3. two stage methods of purification of long-chain biatomic acid water according to claim 1, it is characterized in that: in (a, b, the c) of step (2), heating and temperature control is at 80 ~ 100 ℃, and oxygenant is clorox or ozone, and its consumption is 2 ~ 8% of microfiltration membrane clear liquid.
4. two stage methods of purification of long-chain biatomic acid water according to claim 1, it is characterized in that: the temperature of the pending long-chain biatomic acid clear liquid of the stirring heating step (2) of step (3) is 80 ~ 100 ℃, acid is adjusted to Jie Wen district between pH2.5 ~ 7, sodium salt is sodium sulfate, sodium-chlor or sodium carbonate, and the acid wash water of saturated sodium salt is chosen a certain or mixing acid of sulfuric acid, phosphoric acid, acetic acid, oxalic acid.
5. two stage methods of purification of long-chain biatomic acid water according to claim 1, it is characterized in that: it is as follows that acid wash water reclaims pending method: heat the acid wash water to 60 of saturated sodium salt ~ 90 ℃, the gac that adds its amount 1 ~ 3% stirs insulation 30 ~ 60 minutes, whether detect the sodium salt solution salinity after filtering meets the demands, if salinity is added a certain amount of identical sodium salt through the water dilution, pH adds a certain amount of acid when not enough, and sulfuric acid, hydrochloric acid, acetic acid, oxalic acid be one or more mixing acid wherein.
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| WO2017088218A1 (en) | 2015-11-27 | 2017-06-01 | 希锐科技（北京）有限公司 | Method of co-producing long chain amino acid and dibasic acid |
| US10065921B1 (en) | 2017-07-07 | 2018-09-04 | Vitaworks Ip, Llc | Process for producing long chain amino acids and dibasic acids |
| CN109134236A (en) * | 2017-06-19 | 2019-01-04 | 中国科学院过程工程研究所 | A kind of long-chain biatomic acid fermentation liquid decoloration and Deproteinated method |
| CN109970548A (en) * | 2017-12-28 | 2019-07-05 | 凯赛（金乡）生物材料有限公司 | A kind of long-chain biatomic acid oxidative decoloration technique |
| US10343978B2 (en) | 2017-07-07 | 2019-07-09 | Vitaworks Ip, Llc | Process for producing long chain amino acids and dibasic acids |
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| US10065921B1 (en) | 2017-07-07 | 2018-09-04 | Vitaworks Ip, Llc | Process for producing long chain amino acids and dibasic acids |
| US10343978B2 (en) | 2017-07-07 | 2019-07-09 | Vitaworks Ip, Llc | Process for producing long chain amino acids and dibasic acids |
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