CN102584706B - Recovery process of analginum finished product centrifugal mother liquid - Google Patents

Abstract

The invention belongs to the field of medicine chemical and particularly relates to a recovery process of analginum finished product centrifugal mother liquid. Firstly, the analginum finished product centrifugal mother liquid is concentrated, then, organic solvents are added into concretes for dissolution, and analginum primary recovery materials and secondary recovery mother liquid are prepared through temperature reduction, crystallization and centrifugation. The recovery process provided by the invention has the advantages that the process is simple, the content in the analginum primary recovery materials can reach 77 to 80 percent, and the crystallization rate of the finished product centrifugation mother liquid reaches 84 to 92 percent. The centrifugation rate is improved, the analginum content in the secondary recovery mother liquid only accounts for 3 to 5 percent of the total theoretical quantity of the analginum, and the secondary recovery mother liquid can be directly delivered to aminopyrine waste mother liquid methylation posts. The recovery temperature reduction problem of secondary recovery mother liquid to quartic recovery mother liquid is avoided. An open type stainless steel groove can be directly removed, the in-site environment is obviously improved, and the recovery process more perfectly conforms to the environment-protection and audit requirement. The analginum recovery purity is high, the crystallization rate is high, the pollution is avoided, and the industrial production is easily realized.

Description

The recovery process of analginum finished product centrifugal mother liquid

Technical field

The invention belongs to field of medicine and chemical technology, particularly a kind of recovery process of analginum finished product centrifugal mother liquid.

Background technology

Sulpyrine finished product percent crystallization in massecuite is about 73%, have an appointment 27% Sulpyrine enter into centrifuge mother liquor, existing mother liquid recovery process is: by concentrated for finished product centrifuge mother liquor, cooling, crystallization, centrifugal must Sulpyrine reclaimed materials and secondary recovery mother liquor, secondary recovery mother liquor is through concentrated, cooling, crystallization, centrifugal the rewinding of Sulpyrine secondary returning and Sulpyrine three recovery mother liquors, Sulpyrine secondary returning rewinding content is about 75%, percent crystallization in massecuite is about 35%, continuation like this, until be recycled to Sulpyrine No. four reclaimed materials.The content of No. three reclaimed materials and No. four reclaimed materials is all about 45%, and percent crystallization in massecuite is about 30%, reclaims mother liquors for five times of final step and transfers to the pyramidon mother post that methylates of giving up to use.Give the Sulpyrine that useless mother methylates post and account for about 4.65% of the total theoretical amount of Sulpyrine.Production process is as Fig. 1.

Because containing a large amount of impurity in Sulpyrine mother liquor, crystallization condition is harsher, and the cooling of other mother liquor is all carried out in the stainless steel tank of open type except finished product centrifuge mother liquor, does not have heat sink, and can not stir, only reach centrifuging temperature by naturally leaving standstill cooling.Cooling rate is slow, and the temperature fall time of usual secondary recovery mother liquor is 5 days, and reclaiming mother liquor for three times, reclaiming the temperature fall time of mother liquor for four times is 6.5 days.Long processing period, the not only human and material resources of at substantial, also occupy a large amount of spaces.Hold material with the stainless steel tank of open type and there is the risk that foreign matter is mixed into, do not meet GMP management expectancy.Not only there is potential safety hazard but also do not meet current environmental requirement in the gases such as the ethanol that the uncovered placement of material comes out.

Summary of the invention

The object of the present invention is to provide a kind of recovery process of analginum finished product centrifugal mother liquid, not only increase the percent crystallization in massecuite that analginum finished product centrifugal mother liquid reclaims, decrease secondary recovery mother liquor scale; And improve Sulpyrine reclaimed materials quality, reduce organic impurity content in Sulpyrine reclaimed materials.

The recovery process of described analginum finished product centrifugal mother liquid is first concentrated by analginum finished product centrifugal mother liquid; In enriched material, add organic solvent again dissolve, through cooling, crystallization, centrifugal obtained Sulpyrine reclaimed materials and secondary recovery mother liquor.

It is 1.20-1.23g/ml that described analginum finished product centrifugal mother liquid is first concentrated into density with recovery tower, then is concentrated into density 1.30-1.90g/ml with thickener.

Described analginum finished product centrifugal mother liquid is directly concentrated into density 1.30-1.90g/ml with thickener.

The weight loss on drying 5-18% of described enriched material.

When concentrating with thickener, thickening temperature is 60-110 DEG C.

Described organic solvent is C ₁-C ₈alcohol, particular methanol, ethanol, propyl alcohol, Virahol or octanol, most preferred ethanol.

Described organic solvent purity is 95-100%, preferred 99-100%.

The purity of above-mentioned organic solvent refers to the effective content of this organic solvent, content >=99.5% of ethanol in such as dehydrated alcohol, content >=95.0% of ethanol in industrial alcohol.

In concentration process:

After concentrated with thickener, if enriched material weight loss on drying does not reach 5-18%, need to add organic solvent again and again concentrate, organic solvent adds volume and enriched material volume ratio is 1: 0.5; After having concentrated, then when adding organic solvent in enriched material, organic solvent add-on is as the criterion can dissolve enriched material, does not do strict control to add-on.

The organic solvent used in above-mentioned technique can be reclaimed by evaporation, and the organic solvent be evaporated utilizes cooling, the solvent be evaporated reclaims, then by concentrated or membrane separation technique concentrate, reaches production technique demand by condensing works.

The present invention carries out efficient concentration to analginum finished product centrifugal mother liquid and organic solvent (Sulpyrine solvability is wherein slightly soluble) assists concentrated mode, first the moisture in analginum finished product centrifugal mother liquid is fully steamed, then Sulpyrine enriched material density is regulated with this organic solvent, dissolve wherein organic impurity, then through cooling, crystallization, centrifugal Sulpyrine reclaimed materials and secondary recovery mother liquor.

It is the characteristic utilizing Sulpyrine very easily water-soluble that the present invention improves Sulpyrine percent crystallization in massecuite, is realized by the content reducing water in analginum finished product centrifugal mother liquid; The quality of an obtained Sulpyrine reclaimed materials is by adding organic solvent (anhydrous or containing minor amount of water), making dissolve organic contaminants realize in organic solvent.

Beneficial effect of the present invention is as follows:

Present invention process is simple, and the content in Sulpyrine reclaimed materials can reach 77-80%, and finished product centrifuge mother liquor percent crystallization in massecuite reaches 84-92%.Percent crystallization in massecuite improves, and in secondary recovery mother liquor, Sulpyrine amount only accounts for the 3-5% of the total theoretical amount of Sulpyrine, directly can give the pyramidon mother that gives up and to methylate post.There is not the recovery cooling problem that secondary recovery mother liquor to four reclaims mother liquor.The stainless steel tank of open type can directly be removed, and significantly improves site environment, more meets environmental protection and audit requirement.It is high that Sulpyrine reclaims purity, and percent crystallization in massecuite is high, pollution-free, is easy to suitability for industrialized production.

Accompanying drawing explanation

Fig. 1 traditional processing technology figure.

Fig. 2 production technique figure of the present invention.

Embodiment

Below in conjunction with embodiment, the invention will be further described:

Embodiment 1

Measure 4000ml analginum finished product centrifugal mother liquid, being first concentrated into density with recovery tower is 1.21g/ml, then concentrates with thickener, and controlling thickening temperature is 70 ± 10 DEG C, and vacuum tightness is-0.05MP, and being concentrated into density is 1.30g/ml, and its weight loss on drying is 18.0%; Add anhydrous methanol (methanol purity >=99%) to dissolve; After material all dissolves, open interlayer circulating water cooling, after 1.5 hours, be cooled to 67 DEG C, use salt water for cooling instead, be cooled to 35 DEG C through 3.5 hours, close salt solution and prepare centrifugal; Adjust centrifuge speed be 1200 turns/min, charging is carried out centrifugal, after centrifugal 40 minutes, stops whizzer, with 230g anhydrous methanol washing after centrifugal 40 minutes again, discharging.In Sulpyrine reclaimed materials, Sulpyrine content in crude product is 77.28%, and finished product centrifuge mother liquor percent crystallization in massecuite is 84.65%.

Embodiment 2

Measure 4000ml analginum finished product centrifugal mother liquid, concentrate with thickener, controlling thickening temperature is 81.5 ± 10.5 DEG C, and vacuum tightness is-0.07MP, and being concentrated into density is 1.40g/ml; Add anhydrous isopropyl alcohol 90kg, continuing to be concentrated into weight loss on drying is 14.5%, adds Virahol (Virahol purity >=99%) and dissolves; After material all dissolves, open interlayer circulating water cooling, after 2.0 hours, be cooled to 60 DEG C, use salt water for cooling instead, be cooled to 25 DEG C through 4.5 hours, close salt solution and prepare centrifugal; Adjust centrifuge speed be 1200 turns/min, charging is carried out centrifugal, after centrifugal 40 minutes, stops whizzer, with 230g anhydrous isopropyl alcohol washing after centrifugal 40 minutes again, discharging.In Sulpyrine reclaimed materials, Sulpyrine content in crude product is 78.33%, and finished product centrifuge mother liquor percent crystallization in massecuite is 86.53%.

Embodiment 3

Measure 4000ml analginum finished product centrifugal mother liquid, first being concentrated into density with recovery tower is 1.225g/ml, concentrate with thickener again, controlling thickening temperature is 89 ± 2 DEG C, vacuum tightness is-0.08MP, being concentrated into density is 1.45g/ml, add dehydrated alcohol (purity of alcohol >=99%) 89kg, continuing to be concentrated into weight loss on drying is 12.5%, then adds anhydrous alcohol solution, after material all dissolves, open interlayer circulating water cooling, after 1.5 hours, be cooled to 68 DEG C, use salt water for cooling instead, be cooled to 25 DEG C through 5.5 hours, close salt solution and prepare centrifugal; Adjust centrifuge speed to be 1200 turns/min, charging is carried out centrifugal, after centrifugal 40 minutes, stops whizzer, with after 230g absolute ethanol washing centrifugal 40 minutes again, and discharging.In Sulpyrine reclaimed materials, Sulpyrine content in crude product is 79.87%, and finished product centrifuge mother liquor percent crystallization in massecuite is 88.10%.

Embodiment 4

Measure 4000ml analginum finished product centrifugal mother liquid, being first concentrated into density with recovery tower is 1.23g/ml, then concentrates with efficient concentration device, and controlling thickening temperature is 95 ± 15 DEG C, and vacuum tightness is-0.08MP, and being concentrated into density is 1.70g/ml, and its weight loss on drying is 7.5%; Add dehydrated alcohol (purity of alcohol >=99%) to dissolve; After material all dissolves, open interlayer circulating water cooling, after 2.5 hours, be cooled to 60 DEG C, use salt water for cooling instead, be cooled to 15 DEG C through 7.0 hours, close salt solution and prepare centrifugal; Adjust centrifuge speed to be 1200 turns/min, charging is carried out centrifugal, after centrifugal 40 minutes, stops whizzer, with after 230g absolute ethanol washing centrifugal 40 minutes again, and discharging.In Sulpyrine reclaimed materials, Sulpyrine content in crude product is 78.28%, and finished product centrifuge mother liquor percent crystallization in massecuite is 90.25%.

Embodiment 5

Measure 4000ml analginum finished product centrifugal mother liquid, being first concentrated into density with recovery tower is 1.23g/ml, then concentrates with efficient concentration device, and controlling thickening temperature is 95 ± 15 DEG C, and vacuum tightness is-0.08MP, and being concentrated into density is 1.90g/ml, and its weight loss on drying is 5%; Add anhydrous octanol (octanol purity >=99%) to dissolve; After material all dissolves, open interlayer circulating water cooling, after 2.5 hours, be cooled to 60 DEG C, use salt water for cooling instead, be cooled to 15 DEG C through 7.3 hours, close salt solution and prepare centrifugal; Adjust centrifuge speed be 1200 turns/min, charging is carried out centrifugal, after centrifugal 40 minutes, stops whizzer, with 230g anhydrous octanol washing after centrifugal 40 minutes again, discharging.In Sulpyrine reclaimed materials, Sulpyrine content in crude product is 78.43%, and finished product centrifuge mother liquor percent crystallization in massecuite is 92%.

Claims (3)

1. a recovery process for analginum finished product centrifugal mother liquid, is characterized in that first being concentrated by analginum finished product centrifugal mother liquid; In enriched material, add organic solvent again dissolve, through cooling, crystallization, centrifugal obtained Sulpyrine reclaimed materials and secondary recovery mother liquor;

Described enriched material weight loss on drying 5-18%;

When concentrating with thickener, thickening temperature is 60-110 DEG C;

Described organic solvent is methyl alcohol, ethanol, propyl alcohol, Virahol or octanol;

Described organic solvent purity is 95-100%;

It is 1.20-1.23g/ml that described analginum finished product centrifugal mother liquid is first concentrated into density with recovery tower, then is concentrated into density 1.30-1.90g/ml with thickener.

2. recovery process according to claim 1, is characterized in that described organic solvent is ethanol.

3. recovery process according to claim 1, is characterized in that described organic solvent purity is 99-100%.