CN105315704B - A kind of method reclaiming organic acid from the waste liquid that Calyx Hibisci Sabdariffae is extracted after pigment - Google Patents

A kind of method reclaiming organic acid from the waste liquid that Calyx Hibisci Sabdariffae is extracted after pigment Download PDF

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CN105315704B
CN105315704B CN201510088053.8A CN201510088053A CN105315704B CN 105315704 B CN105315704 B CN 105315704B CN 201510088053 A CN201510088053 A CN 201510088053A CN 105315704 B CN105315704 B CN 105315704B
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organic acid
pigment
hibisci sabdariffae
calyx hibisci
calyx
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CN105315704A (en
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展亚莉
展康华
李进超
周红
刘晓波
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QINGDAO PENGYUANKANGHUA NATURAL SOURCE Co Ltd
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Abstract

The invention discloses a kind of method of organic acid that reclaims from the waste liquid that Calyx Hibisci Sabdariffae is extracted after pigment is it is characterised in that specifically include following steps:(1)Extract;(2)Resin absorption pigment;(3)Calyx Hibisci Sabdariffae pigment processed;(4)Resin absorption organic acid;(5)Eluting;(6)Organic acid sodium salt is transformed into organic acid;(7)Calyx Hibisci Sabdariffae organic acid processed.The present invention is the technology that a kind of Calyx Hibisci Sabdariffae organic acid isolates and purifies, using tap water, Calyx Hibisci Sabdariffae and holder are carried out with the extraction of pigment and organic acid, present invention macroporous resin adsorption pigment, from the waste liquid of the complete roselle calyx red pigment of separation and Extraction, using ion exchange resin adsorption recovery organic acid, can be used as acid condiment, improve the added value of Calyx Hibisci Sabdariffae and holder pigment product.

Description

A kind of method reclaiming organic acid from the waste liquid that Calyx Hibisci Sabdariffae is extracted after pigment
Technical field
The invention belongs to food additive production technical field and in particular to a kind of from Calyx Hibisci Sabdariffae extract pigment after waste liquid The middle method reclaiming organic acid, especially from the waste liquid of the complete roselle calyx red pigment of separation and Extraction, is returned using ion exchange resin Receive organic acid, improve the added value of Calyx Hibisci Sabdariffae and holder pigment product.
Background technology
Calyx Hibisci Sabdariffae(Hibiscus SabdariffaLinn)It is Malvaceae Hibiscuses annual herb plant or perennial Shrub, is widely used in treatment heart and the disease of nerve in African Territories.A large amount of organic acid are contained in Calyx Hibisci Sabdariffae and holder, Content up to 15%~30% about, mainly includes oxalic acid, tartaric acid, malic acid, succinic acid, citric acid, malonic acid etc.(Li Sheng Cutting edge of a knife or a sword, Liu Xueming, Zhu Zhiwei, Huang Ruqiang, Wu Jijun, Chen Zhiyi. the exploitation of Calyx Hibisci Sabdariffae resource. food science and technology, 2003,11: 87-94).Calyx Hibisci Sabdariffae organic acid can be added in food as organic acid flavoring agent.Modern pharmacology research shows, Roselle flower Organic acid in calyx and holder has the function of inhibiting bacteria and diminishing inflammation, antioxidation, antitumor, hepatoprotective, relieving constipation and diuresis.Ground in recent years Study carefully and the method for organic acid extracted although utilizing waste water to a certain extent using supercritical extraction, but operation is more complicated, It is not easily controlled, cost is also higher.Therefore research worker is exploring a kind of low input, simple method always.
Both at home and abroad the research of Calyx Hibisci Sabdariffae is concentrated mainly on the exploitation of Calyx Hibisci Sabdariffae food at present, such as Roselle eight-flavor rice dumpling(Shen Please number:200810058938.3), Roselle mooncake(Application number:200810058939.8)Patent application described in, and Flos Rosae Rugosae The extraction research such as roselle calyx red pigment and preparation method of lycopene(Application number:200910197981.2)Patent application institute State, and the extraction research to organic acid in Calyx Hibisci Sabdariffae and holder has no report.
Content of the invention
For problems of the prior art, it is an object of the invention to provide a kind of useless after Calyx Hibisci Sabdariffae extracts pigment The method reclaiming organic acid in liquid, is the technology that a kind of Calyx Hibisci Sabdariffae organic acid isolates and purifies, using tap water to Calyx Hibisci Sabdariffae Carry out the extraction of pigment and organic acid with holder, present invention macroporous resin adsorption pigment, red from the complete Calyx Hibisci Sabdariffae of separation and Extraction In the waste liquid of element, using ion exchange resin adsorption recovery organic acid, can be used as acid condiment.
The technological process of production that technical solution of the present invention is adopted is:(1)Calyx Hibisci Sabdariffae processed and holder extracting solution;(2) Resin absorption pigment;(3)Calyx Hibisci Sabdariffae pigment processed;(4)Resin absorption organic acid;(5)Eluting;(6)Organic acid sodium salt has been transformed into Machine acid;(7)Calyx Hibisci Sabdariffae organic acid processed.
The technical scheme that the present invention takes is:
A kind of from Calyx Hibisci Sabdariffae extract pigment after waste liquid reclaim organic acid method it is characterised in that specifically include as Lower step:
(1)Extract:It is 1 that Calyx Hibisci Sabdariffae dry flower calyx and holder are added mass volume ratio:15~1:20 distilled water, 60 DEG C water bath with thermostatic control adverse current is extracted 2~3 times, 1~2 h every time, and united extraction liquid is centrifuged, and collects supernatant;
(2)Resin absorption pigment:Take appropriate macroporous resin, first use distilled water immersion, distillation be washed to liquid clear till, then adopt Ethanol with 95% soaks 4 h, and distillation is washed to not muddy, is poured in the adsorption column of 1 × 100 cm, supernatant upper prop is carried out Adsorption operations, collect the effluent a after adsorpting pigment;
(3)Calyx Hibisci Sabdariffae pigment processed:First with the distilled water cleaning step of 3 times of column volumes(2)In adsorption column, then with containing 0.3% The ethanol water of the 70% of citric acid carries out eluting, obtains Calyx Hibisci Sabdariffae pigment solution, concentrating under reduced pressure, is spray-dried, obtains Flos Rosae Rugosae Eggplant pigment solid product;
(4)Resin absorption organic acid:Take proper amount of weak base anion exchange resin, first use distilled water immersion, distillation washing To liquid clear, then with 4% aqueous hydrochloric acid solution soak 4 h, distillation be washed to weakly acidic pH, then the sodium hydroxide with 4% is water-soluble Immersion steeps 4 h, and distillation is washed to weakly acidic pH, and the resin that pretreatment is finished is poured in the adsorption column of 1 × 100 cm, by the (2)The effluent a that step operation is collected carries out upper prop adsorption operations, and effluent emits;
(5)Eluting:First use distilled water cleaning step(4)In adsorption column, to weakly acidic pH, then washed with NaOH aqueous solution De-, collect eluent;
(6)Organic acid sodium salt is transformed into organic acid:Take appropriate highly acid hydrogen type cation exchange resin, first with distillation water logging Bubble, distillation be washed to liquid clear till, then with 4% sodium hydrate aqueous solution soak 4 h, distill be washed to weakly acidic pH, then with 4% Aqueous hydrochloric acid solution soak 4 h, distillation be washed to weakly acidic pH, the resin that pretreatment is finished, be poured into the absorption of 1 × 100 cm In post, upper prop carries out adsorption operations, collects effluent b;
(7)Calyx Hibisci Sabdariffae organic acid processed:By step(6)In Calyx Hibisci Sabdariffae organic acid effluent b concentrated under vacuum, spray Mist is dried, and obtains Calyx Hibisci Sabdariffae organic acid powdery product.
Further, described step(2)In macroporous resin be AB-8 adsorbent resin.
Further, described step(2)In effluent a be extract organic acid raw material, be macroporous resin separation and Extraction The waste liquid of complete roselle calyx red pigment.
Further, described step(4)The weak-base anion-exchange resin that middle Adsorption organic acid is adopted is that D296 is weak Basic anion exchange resin.
Further, described step(5)NaOH concentration in middle eluent is 0.5~3.0 mol/L.
Further, described step(6)The adopted highly acid hydrogen type cation exchange resin of middle organic acid transition is D001 × 7 highly acid hydrogen type cation exchange resin.
Further, described step(3)And step(7)The condition of middle spray drying is:Feeding liquid concentration 22~25 Baume Degree, described Baume degrees are to measure at 50 DEG C, 270~280 DEG C of PG-5 type spray dryer inlet temperature, outlet temperature 70~80 DEG C, centrifugal head operating pressure 2~2.5 kgf/cm2.
Beneficial effects of the present invention are:
(1)The present invention extracts Calyx Hibisci Sabdariffae pigment from Calyx Hibisci Sabdariffae and holder raw material, and the Extraction solvent of use is from the beginning Water, eluant is acidic ethanol aqueous solution, and the macroporous resin adopting during adsorpting pigment has higher preferential chelating absorption property, Directly pigment and organic acid waste liquid can be separated, make the reclaimer operation of organic acid convenient;Using Calyx Hibisci Sabdariffae and Holder carries out the extraction of pigment and organic acid for raw material, and the Calyx Hibisci Sabdariffae pigment extracting can be used for functional food and functional food Additive is developed, and the added value brought is higher, has and compares wide application prospect.
(2)From the waste liquid of the complete roselle calyx red pigment of separation and Extraction, organic acid is reclaimed using ion exchange resin, be available for eating Product industry, as acidity regulator, realizes the comprehensive utilization of Calyx Hibisci Sabdariffae and holder, improves value-added content of product;Using ion Exchanger resin absorption method separation and Extraction organic acid, resin easily regenerates reuse, low production cost.
(3)The present invention, from the waste liquid of the complete roselle calyx red pigment of separation and Extraction, is had using ion exchange resin adsorption recovery Machine acid, carries out pretreatment to the weak-base anion-exchange resin extracting organic acid employing, is first washed till liquid with distilled water immersion clear Till, then soaked with aqueous hydrochloric acid solution, it is washed to weakly acidic pH, then soaked with sodium hydrate aqueous solution, be washed to weakly acidic pH, carry The high absorbability to organic acid for the resin, equipment is simple, and easy to operate, cost input is low, and the physical method energy being adopted Enough pollutions reducing to environment, safe, as acid condiment, improve the quality percentage of food, increase food enterprise Economic benefit.
(4)Organic acid the adopted highly acid hydrogen type cation exchange resin of transition, the active ion in its functional group is- SO3H, pKa<1, pH value is on the impact of its eluting power less;Eluting power is mainly relevant with the concentration of sodium hydroxide eluting agent, Sodium hydroxide its to absorption on strongly acidic cation-exchange the eluting power of material larger, the amount of the organic acid being recovered to More.
Specific embodiment
Below in conjunction with technical scheme, describe the concrete production stage of the present invention in detail:
Embodiment 1
A kind of from Calyx Hibisci Sabdariffae extract pigment after waste liquid reclaim organic acid method it is characterised in that specifically include as Lower step:
(1)Extract:It is 1 that Calyx Hibisci Sabdariffae dry flower calyx and holder are added mass volume ratio:15 distilled water, in 60 DEG C of constant temperature Water-bath adverse current is extracted 3 times, 1 h every time, and united extraction liquid is centrifuged, and collects supernatant;
(2)Resin absorption pigment:Take appropriate macroporous resin, first use distilled water immersion, distillation be washed to liquid clear till, then adopt Ethanol with 95% soaks 4 h, and distillation is washed to not muddy, is poured in the adsorption column of 1 × 100 cm, supernatant upper prop is carried out Adsorption operations, collect the effluent a after adsorpting pigment;
(3)Calyx Hibisci Sabdariffae pigment processed:First with the distilled water cleaning step of 3 times of column volumes(2)In adsorption column, then with containing 0.3% The ethanol water of the 70% of citric acid carries out eluting, obtains Calyx Hibisci Sabdariffae pigment solution, concentrating under reduced pressure, is spray-dried, obtains Flos Rosae Rugosae Eggplant pigment solid product;
(4)Resin absorption organic acid:Take proper amount of weak base anion exchange resin, first use distilled water immersion, distillation washing To liquid clear, then with 4% aqueous hydrochloric acid solution soak 4 h, distillation be washed to weakly acidic pH, then the sodium hydroxide with 4% is water-soluble Immersion steeps 4 h, and distillation is washed to weakly acidic pH, and the resin that pretreatment is finished is poured in the adsorption column of 1 × 100 cm, by the (2)The effluent a that step operation is collected carries out upper prop adsorption operations, and effluent emits;
(5)Eluting:First use distilled water cleaning step(4)In adsorption column, to weakly acidic pH, then washed with NaOH aqueous solution De-, collect eluent;
(6)Organic acid sodium salt is transformed into organic acid:Take appropriate highly acid hydrogen type cation exchange resin, first with distillation water logging Bubble, distillation be washed to liquid clear till, then with 4% sodium hydrate aqueous solution soak 4 h, distill be washed to weakly acidic pH, then with 4% Aqueous hydrochloric acid solution soak 4 h, distillation be washed to weakly acidic pH, the resin that pretreatment is finished, be poured into the absorption of 1 × 100 cm In post, upper prop carries out adsorption operations, collects effluent b;
(7)Calyx Hibisci Sabdariffae organic acid processed:By step(6)In Calyx Hibisci Sabdariffae organic acid effluent b concentrated under vacuum, spray Mist is dried, and obtains Calyx Hibisci Sabdariffae organic acid powdery product.
Further, described step(2)In macroporous resin be AB-8 adsorbent resin.
Further, described step(2)In effluent a be extract organic acid raw material, be macroporous resin separation and Extraction The waste liquid of complete roselle calyx red pigment.
Further, described step(4)The weak-base anion-exchange resin that middle Adsorption organic acid is adopted is that D296 is weak Basic anion exchange resin.
Further, described step(5)NaOH concentration in middle eluent is 0.5 mol/L.
Further, described step(6)The adopted highly acid hydrogen type cation exchange resin of middle organic acid transition is D001 × 7 highly acid hydrogen type cation exchange resin.
Further, described step(3)And step(7)The condition of middle spray drying is:Feeding liquid concentration 22~25 Baume Degree, described Baume degrees are to measure at 50 DEG C, 270 DEG C of PG-5 type spray dryer inlet temperature, 70 DEG C of outlet temperature, and centrifugation turns Head operating pressure 2 kgf/cm2.
Embodiment 2
A kind of from Calyx Hibisci Sabdariffae extract pigment after waste liquid reclaim organic acid method it is characterised in that specifically include as Lower step:
(1)Extract:It is 1 that Calyx Hibisci Sabdariffae dry flower calyx and holder are added mass volume ratio:18 distilled water, in 60 DEG C of constant temperature Water-bath adverse current is extracted 3 times, 1.5 h every time, and united extraction liquid is centrifuged, and collects supernatant;
(2)Resin absorption pigment:Take appropriate macroporous resin, first use distilled water immersion, distillation be washed to liquid clear till, then adopt Ethanol with 95% soaks 4 h, and distillation is washed to not muddy, is poured in the adsorption column of 1 × 100 cm, supernatant upper prop is carried out Adsorption operations, collect the effluent a after adsorpting pigment;
(3)Calyx Hibisci Sabdariffae pigment processed:First with the distilled water cleaning step of 3 times of column volumes(2)In adsorption column, then with containing 0.3% The ethanol water of the 70% of citric acid carries out eluting, obtains Calyx Hibisci Sabdariffae pigment solution, concentrating under reduced pressure, is spray-dried, obtains Flos Rosae Rugosae Eggplant pigment solid product;
(4)Resin absorption organic acid:Take proper amount of weak base anion exchange resin, first use distilled water immersion, distillation washing To liquid clear, then with 4% aqueous hydrochloric acid solution soak 4 h, distillation be washed to weakly acidic pH, then the sodium hydroxide with 4% is water-soluble Immersion steeps 4 h, and distillation is washed to weakly acidic pH, and the resin that pretreatment is finished is poured in the adsorption column of 1 × 100 cm, by the (2)The effluent a that step operation is collected carries out upper prop adsorption operations, and effluent emits;
(5)Eluting:First use distilled water cleaning step(4)In adsorption column, to weakly acidic pH, then washed with NaOH aqueous solution De-, collect eluent;
(6)Organic acid sodium salt is transformed into organic acid:Take appropriate highly acid hydrogen type cation exchange resin, first with distillation water logging Bubble, distillation be washed to liquid clear till, then with 4% sodium hydrate aqueous solution soak 4 h, distill be washed to weakly acidic pH, then with 4% Aqueous hydrochloric acid solution soak 4 h, distillation be washed to weakly acidic pH, the resin that pretreatment is finished, be poured into the absorption of 1 × 100 cm In post, upper prop carries out adsorption operations, collects effluent b;
(7)Calyx Hibisci Sabdariffae organic acid processed:By step(6)In Calyx Hibisci Sabdariffae organic acid effluent b concentrated under vacuum, spray Mist is dried, and obtains Calyx Hibisci Sabdariffae organic acid powdery product.
Further, described step(2)In macroporous resin be AB-8 adsorbent resin.
Further, described step(2)In effluent a be extract organic acid raw material, be macroporous resin separation and Extraction The waste liquid of complete roselle calyx red pigment.
Further, described step(4)The weak-base anion-exchange resin that middle Adsorption organic acid is adopted is that D296 is weak Basic anion exchange resin.
Further, described step(5)NaOH concentration in middle eluent is 2 mol/L.
Further, described step(6)The adopted highly acid hydrogen type cation exchange resin of middle organic acid transition is D001 × 7 highly acid hydrogen type cation exchange resin.
Further, described step(3)And step(7)The condition of middle spray drying is:Feeding liquid concentration 22~25 Baume Degree, described Baume degrees are to measure at 50 DEG C, 275 DEG C of PG-5 type spray dryer inlet temperature, 75 DEG C of outlet temperature, and centrifugation turns Head operating pressure 2.3 kgf/cm2.
Embodiment 3
A kind of from Calyx Hibisci Sabdariffae extract pigment after waste liquid reclaim organic acid method it is characterised in that specifically include as Lower step:
(1)Extract:It is 1 that Calyx Hibisci Sabdariffae dry flower calyx and holder are added mass volume ratio:20 distilled water, in 60 DEG C of constant temperature Water-bath adverse current is extracted 3 times, 1 h every time, and united extraction liquid is centrifuged, and collects supernatant;
(2)Resin absorption pigment:Take appropriate macroporous resin, first use distilled water immersion, distillation be washed to liquid clear till, then adopt Ethanol with 95% soaks 4 h, and distillation is washed to not muddy, is poured in the adsorption column of 1 × 100 cm, supernatant upper prop is carried out Adsorption operations, collect the effluent a after adsorpting pigment;
(3)Calyx Hibisci Sabdariffae pigment processed:First with the distilled water cleaning step of 3 times of column volumes(2)In adsorption column, then with containing 0.3% The ethanol water of the 70% of citric acid carries out eluting, obtains Calyx Hibisci Sabdariffae pigment solution, concentrating under reduced pressure, is spray-dried, obtains Flos Rosae Rugosae Eggplant pigment solid product;
(4)Resin absorption organic acid:Take proper amount of weak base anion exchange resin, first use distilled water immersion, distillation washing To liquid clear, then with 4% aqueous hydrochloric acid solution soak 4 h, distillation be washed to weakly acidic pH, then the sodium hydroxide with 4% is water-soluble Immersion steeps 4 h, and distillation is washed to weakly acidic pH, and the resin that pretreatment is finished is poured in the adsorption column of 1 × 100 cm, by the (2)The effluent a that step operation is collected carries out upper prop adsorption operations, and effluent emits;
(5)Eluting:First use distilled water cleaning step(4)In adsorption column, to weakly acidic pH, then washed with NaOH aqueous solution De-, collect eluent;
(6)Organic acid sodium salt is transformed into organic acid:Take appropriate highly acid hydrogen type cation exchange resin, first with distillation water logging Bubble, distillation be washed to liquid clear till, then with 4% sodium hydrate aqueous solution soak 4 h, distill be washed to weakly acidic pH, then with 4% Aqueous hydrochloric acid solution soak 4 h, distillation be washed to weakly acidic pH, the resin that pretreatment is finished, be poured into the absorption of 1 × 100 cm In post, upper prop carries out adsorption operations, collects effluent b;
(7)Calyx Hibisci Sabdariffae organic acid processed:By step(6)In Calyx Hibisci Sabdariffae organic acid effluent b concentrated under vacuum, spray Mist is dried, and obtains Calyx Hibisci Sabdariffae organic acid powdery product.
Further, described step(2)In macroporous resin be AB-8 adsorbent resin.
Further, described step(2)In effluent a be extract organic acid raw material, be macroporous resin separation and Extraction The waste liquid of complete roselle calyx red pigment.
Further, described step(4)The weak-base anion-exchange resin that middle Adsorption organic acid is adopted is that D296 is weak Basic anion exchange resin.
Further, described step(5)NaOH concentration in middle eluent is 3.0 mol/L.
Further, described step(6)The adopted highly acid hydrogen type cation exchange resin of middle organic acid transition is D001 × 7 highly acid hydrogen type cation exchange resin.
Further, described step(3)And step(7)The condition of middle spray drying is:Feeding liquid concentration 22~25 Baume Degree, described Baume degrees are to measure at 50 DEG C, 280 DEG C of PG-5 type spray dryer inlet temperature, 80 DEG C of outlet temperature, and centrifugation turns Head operating pressure 2.5 kgf/cm2.

Claims (5)

1. a kind of method of organic acid that reclaims from the waste liquid that Calyx Hibisci Sabdariffae is extracted after pigment is it is characterised in that specifically include as follows Step:
(1) extract:It is 1 that Calyx Hibisci Sabdariffae dry flower calyx and holder are added mass volume ratio:15~1:20 distilled water, in 60 DEG C of constant temperature Water-bath adverse current is extracted 2~3 times, 1~2h every time, and united extraction liquid is centrifuged, and collects supernatant;
(2) resin absorption pigment:Take appropriate macroporous resin, first use distilled water immersion, distillation be washed to liquid clear till, then adopt 95% ethanol soaks 4h, and distillation is washed to not muddy, is poured in the adsorption column of 1 × 100cm, supernatant upper prop is adsorbed Operation, collects the effluent a after adsorpting pigment;
(3) Calyx Hibisci Sabdariffae pigment processed:First with the adsorption column in the distilled water cleaning step (2) of 3 times of column volumes, then with containing 0.3% lemon The ethanol water of the 70% of lemon acid carries out eluting, obtains Calyx Hibisci Sabdariffae pigment solution, concentrating under reduced pressure, is spray-dried, obtains Flos Rosae Rugosae Eggplant pigment solid product;
(4) resin absorption organic acid:Take appropriate D296 weak-base anion-exchange resin, first use distilled water immersion, distillation washing To liquid clear, then with 4% aqueous hydrochloric acid solution soak 4h, distillation be washed to weakly acidic pH, then the sodium hydroxide with 4% is water-soluble Immersion steeps 4h, and distillation is washed to weakly acidic pH, and the resin that pretreatment is finished is poured in the adsorption column of 1 × 100cm, by (2nd) step The effluent a collecting is operated to carry out upper prop adsorption operations, effluent emits;
(5) eluting:First use the adsorption column in distilled water cleaning step (4), to weakly acidic pH, then carry out eluting with NaOH aqueous solution, Collect eluent;
(6) organic acid sodium salt is transformed into organic acid:Take appropriate D001 × 7 highly acid hydrogen type cation exchange resin, first with distillation Water soak, distillation be washed to liquid clear till, then with 4% sodium hydrate aqueous solution soak 4h, distill be washed to weakly acidic pH, then Aqueous hydrochloric acid solution with 4% soaks 4h, and distillation is washed to weakly acidic pH, and the resin that pretreatment is finished is poured into the suction of 1 × 100cm In attached column, upper prop carries out adsorption operations, collects effluent b;
(7) Calyx Hibisci Sabdariffae organic acid processed:Calyx Hibisci Sabdariffae organic acid effluent b in step (6) is concentrated under vacuum, spray dried Dry, obtain Calyx Hibisci Sabdariffae organic acid powdery product.
2. the method reclaiming organic acid according to claim 1 the waste liquid after a kind of extraction pigment from Calyx Hibisci Sabdariffae, its feature It is, the macroporous resin in described step (2) is AB-8 adsorbent resin.
3. the method reclaiming organic acid according to claim 1 the waste liquid after a kind of extraction pigment from Calyx Hibisci Sabdariffae, its feature It is, the effluent a in described step (2) is the raw material extracting organic acid, be that the complete Calyx Hibisci Sabdariffae of macroporous resin separation and Extraction is red The waste liquid of element.
4. the method reclaiming organic acid according to claim 1 the waste liquid after a kind of extraction pigment from Calyx Hibisci Sabdariffae, its feature It is, the NaOH concentration in eluent in described step (5) is 0.5~3.0mol/L.
5. the method reclaiming organic acid according to claim 1 the waste liquid after a kind of extraction pigment from Calyx Hibisci Sabdariffae, its feature It is, the condition being spray-dried in described step (3) and step (7) is:Feeding liquid concentration 22~25 Baume degrees, described Baume Degree is to measure at 50 DEG C, 270~280 DEG C of PG-5 type spray dryer inlet temperature, 70~80 DEG C of outlet temperature, centrifugal head work Make pressure 2~2.5kgf/cm2.
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