CN101033199A - Method of recovering terramycin from terramycin production mother liquid - Google Patents

Abstract

This invention relates to a method for recovering terramycin from terramycin mother liquid, which adds acid or alkali to a terramycin mother liquid to adjust pH to 2-9 to be filtered and get the clarified mother liquid, and puts strong polarity large hole adsorption resin into an adsorption post to adsorb terramycin from the clarified mother liquid controlling the temperature at 10-15deg.C and flow rate at 2-16BV/h, takes ethanol, methanol or acetone organic solvent as the eluent and controls the temperature at 25-60deg.C and flow rate at 1-4BV/h to carry out desorption, then the desorption solution is distilled to separate out terramycin and recovers organic solvent.

Description

From terramycin production mother liquid, reclaim the method for terramycin

Technical field

The present invention relates to the production of terramycin, specifically, is the method that reclaims terramycin with polymeric adsorbent from the mother liquor of producing terramycin.

Background technology

In the terramycin production mother liquid, the terramycin that contains the 0.05-0.08% that has an appointment, also contain protein, polysaccharide compound, oxalic acid, inorganics of higher concentration etc., after the terramycin recycling with mother liquor, carry out wastewater treatment again, can reduce the wasting of resources on the one hand, obtain economic benefit, also reduce the difficulty and the cost of wastewater treatment on the other hand.Have not yet to see the report that from terramycin production mother liquid, reclaims terramycin.

Summary of the invention

The purpose of this invention is to provide a kind of method that from terramycin production mother liquid, reclaims terramycin.

The objective of the invention is to be achieved through the following technical solutions:

A kind of method that from terramycin production mother liquid, reclaims terramycin, it is made up of the following step:

Steps A: terramycin is refined mother liquor add acid or alkali adjusting pH to 2-9, filter, obtain clarified mother liquor;

Step B: the strong polar macroporous adsorption resin of in adsorption column, packing into, after conventional pre-treatment, with the terramycin clarified mother liquor of steps A gained, it is under the 2-8BV/h condition with flow velocity that controlled temperature is 10-25 ℃, by polymeric adsorbent, terramycin is adsorbed;

Step C: with ethanol, methyl alcohol or acetone organic solvent is elutriant, and controlled temperature is 25-60 ℃, and flow velocity is 1-4BV/h, carries out desorption;

Step D: the desorption liquid of step C gained is gone out terramycin and reclaims organic solvent through fractionation by distillation.

Materials such as the mycelium that contain oxalic acid in the waste water, the back of fermenting produces, terramycin, when waste water adsorbed in iso-electric point, mycelium was electronegative, and oxalic acid exists with ionic species, and terramycin exists with molecular form, and can be by resin absorption, adsorption selectivity is good.

Adopt the inventive method, the rate of recovery of terramycin is 50-80%, and absorption effluent is easier to administer than original nut liquid.The inventive method is simple, and resin can be reused, and cost is low.

Embodiment

The invention will be further described by the following examples.

Embodiment 1

Terramycin is refined mother liquor add alkali adjusting pH to 5.4, filter, obtain the terramycin clarified mother liquor, the mycin clarified mother liquor 500ml that fetches earth, terramycin concentration is 526mg/l; (the NKA-2 type of producing with Chemical Plant of Nankai Univ. is an example to get strong polar macroporous adsorption resin, NKA-2 is vinylbenzene-diethylbenzene structure) 10ml adorns post, handle and be washed to neutrality with 4% hydrochloric acid, acetone, 4% sodium hydroxide solution successively, the terramycin clarified mother liquor is passed through macroporous adsorptive resins, 10 ℃ of adsorption temps, flow velocity 2BV/h, absorption effluent terramycin concentration is 211mg/l, the rate of recovery 59.9%.Adsorb saturated back with 95% ethanol 25 ℃ of temperature, desorption during flow velocity 4BV/h obtains terramycin and reclaims ethanol through rectifying separation again, desorption rate 97.5%.Through experiment, foreign matter content is lower than 8.9% in the desorption liquid.

Embodiment 2

The mycin that fetches earth refines mother liquor and adds alkali adjusting pH to 9.0, filters, and obtains the terramycin clarified mother liquor, the mycin clarified mother liquor 500ml that fetches earth, and terramycin concentration is 526mg/l; (the NKA-2 type of producing with Chemical Plant of Nankai Univ. is an example to get strong polar macroporous adsorption resin, NKA-2 is vinylbenzene-diethylbenzene structure) 10ml adorns post, handle and be washed to neutrality with 4% hydrochloric acid, acetone, 4% sodium hydroxide solution successively, the terramycin clarified mother liquor is passed through macroporous adsorptive resins, 25 ℃ of adsorption temps, flow velocity 8BV/h, absorption effluent terramycin concentration is 125mg/l, the rate of recovery 76.2%.Adsorb saturated back with 95% ethanol 60 ℃ of temperature, desorption during flow velocity 1BV/h obtains terramycin and reclaims ethanol through aftertreatment again, desorption rate 98.8%.Through experiment, foreign matter content is lower than 15% in the desorption liquid.

Embodiment 3

The mycin that fetches earth refines mother liquor and adds alkali adjusting pH to 2.0, filters, and obtains the terramycin clarified mother liquor, the mycin clarified mother liquor 500ml that fetches earth, and terramycin concentration is 526mg/l; (the NKA-2 type of producing with Chemical Plant of Nankai Univ. is an example to get strong polar macroporous adsorption resin, NKA-2 is vinylbenzene-diethylbenzene structure) 10ml adorns post, handle and be washed to neutrality with 4% hydrochloric acid, acetone, 4% sodium hydroxide solution successively, the terramycin clarified mother liquor is passed through macroporous adsorptive resins, 10 ℃ of adsorption temps, flow velocity 5BV/h, absorption effluent terramycin concentration is 125mg/l, the rate of recovery 68.0%.Adsorb saturated back with 95% ethanol 60 ℃ of temperature, desorption during flow velocity 1BV/h obtains terramycin and reclaims ethanol through aftertreatment again, desorption rate 98.8%.Through experiment, foreign matter content is lower than 10% in the desorption liquid.

Claims (1)

1. method that reclaims terramycin from terramycin production mother liquid is characterized in that it is made up of the following step:

Steps A: terramycin is refined mother liquor add acid or alkali adjusting pH to 2-9, filter, obtain clarified mother liquor;

Step B: the strong polar macroporous adsorption resin of in adsorption column, packing into, after conventional pre-treatment, with the terramycin clarified mother liquor of steps A gained, it is under the condition of 2-16BV/h with flow velocity that controlled temperature is 10-50 ℃, by adsorption resin column, terramycin is adsorbed;

Step C: with ethanol, methyl alcohol or acetone organic solvent is elutriant, and controlled temperature is 25-60 ℃, and flow velocity is 1-4BV/h, carries out desorption;

Step D: the desorption liquid of step C gained is gone out terramycin and reclaims organic solvent through fractionation by distillation.