CN1059512A - From antibiotic waste water, reclaim the method for oxalic acid - Google Patents
From antibiotic waste water, reclaim the method for oxalic acid Download PDFInfo
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- CN1059512A CN1059512A CN 90107556 CN90107556A CN1059512A CN 1059512 A CN1059512 A CN 1059512A CN 90107556 CN90107556 CN 90107556 CN 90107556 A CN90107556 A CN 90107556A CN 1059512 A CN1059512 A CN 1059512A
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- oxalic acid
- waste water
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- calcium
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
From antibiotic waste water, reclaim the method for oxalic acid, relate to the processing of the waste water that produces in the antibiotic production process, and therefrom reclaim a kind of method of oxalic acid, the present invention adopts the compound of calcium to replace the lead salt precipitation agent that adopts in traditional removal process, the whole recovery process has been avoided the plumbous pollution that brings and has been reclaimed efficient, rapidly, thorough.The oxalic acid final product quality can reach country-level standard, greatly reduces production cost, has alleviated the pollution of oxalic acid waste water to environment, is the method for the recovery waste water mesoxalic acid of the general practicality of a kind of antibiotic factory.
Description
The present invention relates to the processing of the waste water that produces in the antibiotic production process, and therefrom reclaim a kind of method of oxalic acid.
Oxalic acid is a kind of important chemical material, the annual hundreds of ton that needs of middle-size and small-size terramycin or tsiklomitsin factory consumption of oxalic acid, wherein except that minority is consumed, major part is then discharged from waste water, because of oxalic acid has certain corrodibility, with contaminate environment seriously behind the discharge of wastewater, bring great harm to people's life.
At present, domestic some antibiotic manufacturer has done to reclaim the trial of oxalic acid, and its method is: add the lead sulfate of q.s and the precipitation that waste water mesoxalic acid ion forms lead oxalate in waste water, reaction formula is:
Filtration, collecting precipitation thing add the vitriol oil in throw out, add intensification in 30 minutes, and it is seethed with excitement under normal pressure, keep 2 hours, then make the lead oxalate acidolysis become oxalic acid, reaction formula to be
Remove by filter lead sulfate, filtrate is obtained finished product after crystallization, decolorizing and refining, drying.
Reclaim oxalic acid through aforesaid method, occur following problem inevitably:
1. seriously polluted: with lead salt (lead sulfate) is precipitation agent, and the toxicity of itself can cause that operator poison, and simultaneously, owing to leaded in the waste water, can bring the secondary pollution environment of waste discharge.
2. the oxalic acid rate of recovery is low: in the acidolysis process, need to carry out under boiling state, sulfuric acid then easily plays carburizing reagent, and the H in the oxalic acid molecule, O atomic adsorption are come out, and makes C dissociate out, like this, has just seriously influenced the rate of recovery.
3. cost recovery height: in the process of acidolysis lead oxalate, need heat, make the mixture boiling, because oxalic acid, sulfuric acid have certain corrodibility, thereby very high to equipment requirements, in addition, the price of lead sulfate is higher, and the rate of recovery is low, so the whole recovery process cost is higher.
The purpose of this invention is to provide a kind of method that reclaims oxalic acid from antibiotic waste water, this method can prevent secondary pollution, rate of recovery height, and cost is low.
The object of the present invention is achieved like this: low with price, free of contamination calcium is done compound and is replaced lead sulfate as precipitation agent, the compound of antibiotic waste water with calcium precipitated at normal temperatures and pressures, collection contains the compound of caoxalate, carry out acidolysis with sulfuric acid below 90 ° being heated to again, make the oxalic acid reduction, remove by filter calcium sulfate, again the acidolysis thing that contains oxalic acid is carried out freezing and crystallizing, decolouring, purify the oxalic acid finished product.The compound of used calcium is the mixture of calcium chloride or nitrocalcite or calcium chloride, nitrocalcite, Losantin.
The principle of this legal system oxalic acid is such: because of the oxalic acid in the antibiotic factory effluent is to exist with ammonium salts, so can use compound calcium salt to make it to be converted into the calcium oxalate precipitation of indissoluble.Its chemical equation is:
And then under suitable condition, with strong acid such as sulfuric acid oxalic acid is cemented out, its reaction formula is:
Collect filtrate, wherein main component is an oxalic acid, under 0 ℃～5 ℃ conditions, the oxalic acid crude product is crystallized out according to oxalic acid solubility with temperature variation characteristics greatly.At last crude product is decoloured, refining can obtain the high oxalic acid finished product of purity.
Its process flow sheet is as follows:
Method provided by the present invention has overcome the problem that traditional recovery method occurs, and the rate of recovery is up to more than 95%, owing to make precipitation agent, prevented the recontaminate of waste water, in addition simultaneously with the compound replacement leadization thing of calcium, recovery system is also simpler, has so just lowered production cost greatly.Obtain the oxalic acid finished product after reclaiming, purity can reach 99.5% above sulfate radical＜0.1%, ignition residue＜0.1%, and heavy metal＜0.002%, iron＜0.002%, muriate＜0.005%, appearance white crystallization index meets country-level standard.
Specify below in conjunction with embodiment:
Embodiment one: reclaim oxalic acid from tetracycline wastewater:
The combined process schema illustrates step by step:
Precipitation process: receive the antibiotic exhausted water and put into settling tank, stir the mixture that adds precipitation agent calcium chloride 90% Losantin 5%, nitrocalcite 5% and added in 5 minutes, after stirring evenly, left standstill 7 hours, precipitated and separated is put supernatant liquor, collects hypostasis, and its main component is:
Precipitation agent calcium compounds weight and tetracycline wastewater magnitude relation are: the 1000ml tetracycline wastewater adds mixture precipitation agent 0.5 gram.Acidolysis process: precipitation process is formed the throw out that contains caoxalate, put into acidolysis equipment, as enamel reactor.The water that adds three times of weight of precipitate stirs evenly, slow again half the sulfuric acid of weight of precipitate that adds, and sulfuric acid is 95% industrial goods; Added acid and finish in 20 minutes, continue stirring and be warmed up to 80 ℃, keep elimination half an hour throw out, filtrate is put into crystallizer.Crystallisation process: in crystallizer such as crystallizer tank, 0 ℃ or 5 ℃ is descended rapid crystallizations to go out the oxalic acid crude product.The decolorizing and refining process: after the oxalic acid crude product dries after filtration, enter the decolorizing and refining process, the discoloring agent prescription is:
| Title | Weight | Title | Weight |
| The oxalic acid crude product does not have particle water gac | 100g 100g 5g | Barium carbonate polyacrylamide EDTA | 1g 0.1g 0.1g |
Recrystallization, drying process: with the crude product behind the decolorizing and refining, when 0 ℃ or 5 ℃, recrystallization, crystallisate is dry in the drying plant of 40 ℃ or 80 ℃, get final product dry product, i.e. finished product.
Waste water after recycling, the waste water mesoxalic acid rate of recovery reaches 100%, and oxalic acid finished product per ton only needs 1,000 five hundred yuan of costs.
Embodiment 2: reclaim oxalic acid from terramycin wastewater.
This process, identical with recovery oxalic acid from tetracycline wastewater, different substantially just precipitation process, precipitation agent adopts CaCl
2, add CaCl in every 100ml terramycin wastewater liquid
20.5 gram.Acidolysis is warmed up to 90 ℃.
In addition, crystallization and recrystallization process, temperature is carried out in the time of 3 ℃, and drying process, temperature are controlled at 75 ℃.
Do not contained oxalic acid in the processed waste water, the rate of recovery reaches 100%, 2,000 yuan of oxalic acid costs per ton.
Claims (2)
1, a kind of method that from antibiotic waste water, reclaims oxalic acid, earlier in waste water, add precipitation agent and get the oxalate precipitation thing, with strong acid throw out is carried out acidolysis, get acidolysis thing oxalic acid, again the acidolysis thing is carried out freezing and crystallizing, decolorization and purification and obtain the method for oxalic acid, it is characterized in that: precipitation agent adopts the compound with calcium.
2, the method that reclaims oxalic acid from antibiotic waste water according to claim 1 is characterized in that the compound of calcium is CaCl
2Or Ca(NO
3)
2Or CaCl
2, Ca(NO
3)
2Mixture.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90107556 CN1059512A (en) | 1990-09-06 | 1990-09-06 | From antibiotic waste water, reclaim the method for oxalic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90107556 CN1059512A (en) | 1990-09-06 | 1990-09-06 | From antibiotic waste water, reclaim the method for oxalic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1059512A true CN1059512A (en) | 1992-03-18 |
Family
ID=4880608
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 90107556 Pending CN1059512A (en) | 1990-09-06 | 1990-09-06 | From antibiotic waste water, reclaim the method for oxalic acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1059512A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103450008A (en) * | 2013-09-02 | 2013-12-18 | 江苏宝众宝达药业有限公司 | Method for recovering mandelic acid from waste water |
| CN109626532A (en) * | 2019-01-22 | 2019-04-16 | 四川高绿平环境科技有限公司 | A kind of oxalic acid scavenger and preparation method thereof and application method |
-
1990
- 1990-09-06 CN CN 90107556 patent/CN1059512A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103450008A (en) * | 2013-09-02 | 2013-12-18 | 江苏宝众宝达药业有限公司 | Method for recovering mandelic acid from waste water |
| CN103450008B (en) * | 2013-09-02 | 2015-02-25 | 江苏宝众宝达药业有限公司 | Method for recovering mandelic acid from waste water |
| CN109626532A (en) * | 2019-01-22 | 2019-04-16 | 四川高绿平环境科技有限公司 | A kind of oxalic acid scavenger and preparation method thereof and application method |
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