CN105061191B - A kind of method that diene alcohol ketone acetic ester waste acid water recycles - Google Patents
A kind of method that diene alcohol ketone acetic ester waste acid water recycles Download PDFInfo
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- CN105061191B CN105061191B CN201510504637.9A CN201510504637A CN105061191B CN 105061191 B CN105061191 B CN 105061191B CN 201510504637 A CN201510504637 A CN 201510504637A CN 105061191 B CN105061191 B CN 105061191B
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- waste acid
- acid water
- acetic ester
- diene
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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
- C07C51/41—Preparation of salts of carboxylic acids
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G37/00—Compounds of chromium
- C01G37/02—Oxides or hydrates thereof
- C01G37/033—Chromium trioxide; Chromic acid
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of method that diene alcohol ketone acetic ester waste acid water recycles, the method is circulated utilization from diene production technology, the waste acid water applied mechanically recyclable to each link.The side-product of gained has highly purified chromic oxide gel and sodium acetate, all can sell；The method is compared with diene alcohol ketone acetic ester tradition waste acid water processing method, and simple, energy consumption is low, improves the utilization rate of waste acid water, reduces industrial water amount, while reducing cost and the burden of sewage disposal, also reduces the waste acid water pollution to environment.
Description
Technical field
The present invention relates to recycling of the circulation utilization method of a kind of waste water, specially diene alcohol ketone acetic ester waste acid water
Method.
Background technology
Diene, English name: 16-pregnadien-20-one acetate, chemical name: 3 beta-hydroxies-pregnant
Steroid-5,16-diene-20-ketone-3-acetate, molecular formula is C23H32O3.Diene is produce steroid hormone class medicine important
Beginning raw material, can be used for synthesizing the multi-medicaments such as adrenal gland's parahormone medicine, steroidal anti-inflammatory medicine, glucocorticoid medicine, gonadal hormone medicine.State
Nei Ge manufacturer is typically with diosgenin as raw material, and, oxydrolysis acylated through open loop synthesizes diene, often produces 1 ton of diene, meeting
Produce 20 tons of waste acid waters, cause the significant waste of water resource, also pollute environment.Hexamethylene extraction diene be washed to neutrality
Link can produce substantial amounts of containing chromium waste acid water, traditional handicraft will be received by high concentration sour water produced by washing hexamethylene layer for the first time
Collection, second, low concentration waste acid water Han chromium drains in sewage for the third time, even if qualified discharge after treatment, contains weight too
Crome metal, while polluting environment, also result in the waste of water resource.
The patent No. 200910063423.7, a kind of method that chromium slag utilized after producing diene alcohol ketone prepares chrome oxide green is public
Open and utilized diene waste liquid to prepare chrome oxide green, but from waste liquid, do not isolated sodium acetate；Cause the wasting of resources, increase
The difficulty of the follow-up use of waste water.
Patent CN 103274923 B method recycling diene alcohol ketone acetic ester waste liquid, although prepared acetic acid
Sodium, but be the use of etoh solvent and carry out alcohol analysis, add processing cost, and the method is not by the low concentration acid of last consignment of
Water is for washing the applying mechanically of hexamethylene layer of next group, thus being underutilized of waste acid water in system.
The documents and materials recycled about diene alcohol ketone acetic ester waste acid water have not been reported.
Summary of the invention
It is an object of the invention to provide a kind of method that diene alcohol ketone acetic ester waste acid water recycles, its simple process,
Low cost, energy consumption are low, industrial water amount is little, it is little to pollute, provide cost savings for industrialized production.
The object of the present invention is achieved like this: a kind of method that diene alcohol ketone acetic ester waste acid water recycles, specifically
Step is:
1) for containing high concentration acetic acid diene waste acid water I, add sodium carbonate being neutralized to PH is 8 ~ 9, adds hydrazine hydrate
Stirring reaction, is filtrated to get Cr(OH)3And sodium acetate solution；By sodium acetate solution concentrate, dense go out liquid be low-concentration waste acid water IV,
Collect recycled；Reaction bulb cooling crystallize is filtrated to get Sodium acetate trihydrate solid；
2) for containing middle concentration acetic acid diene waste acid water II with containing low-concentration acetic acid waste acid water III, adding sodium carbonate under stirring
Being 8 ~ 9 to PH, add hydrazine hydrate, stirring reaction, after filtration, filtrate cycle utilizes；
Recycling of diene alcohol ketone acetic ester waste acid water is completed by above-mentioned steps.
Further it is improved by: sodium carbonate described in step 1): hydrazine hydrate: mass ratio=0.05 ~ 0.08 of waste acid water:
0.001 ~ 0.0015:1.
Further it is improved by: the degree of concentrating under reduced pressure described in step 1) is be concentrated into original volume 2/5 ~ 3/5.
Further it is improved by: crystallization parameter of lowering the temperature described in step 1) is temperature: 10 ~ 15 DEG C, the time is: 4 ~ 6h.
Further it is improved by: step 2) described sodium carbonate: hydrazine hydrate: mass ratio=0.002 ~ 0.005 of waste acid water:
0.0005 ~ 0.0008:1.
Beneficial effect:
The side-product purity height Cr(OH that the present invention obtains) 3 content 98%；Sodium acetate trihydrate content 60%.
The recycled of waste acid water can make the industrial water of diene alcohol ketone acetic ester save more than 50%.
Described in step 1) dense go out low-concentration waste acid water IV for next group diene produce extraction washing link the 3rd
Secondary washing.
Step 2) filtrate after described filtration may be used for the extraction washing link that next group diene produces first time and
Second time washing.
Method is easy, easy to operate, without complicated production equipment, be suitable to industrialized production.
Energy-saving and emission-reduction, without waste residue, discharge of wastewater, without toxic exhaust emission, have interests environmental conservation.
Accompanying drawing explanation
Fig. 1 is the process chart of the present invention.
Detailed description of the invention
Further illustrate the present invention below in conjunction with embodiment and Fig. 1, but embodiment is only that the explanation present invention, and not
It is to be limited.
Example 1:
1), taking 100g Saponin through open loop, the diene alcohol ketone acetic ester of oxydrolysis synthesis, 2L hexamethylene extracts
After, with the drinking water of 2L, hexamethylene layer is washed three times to neutral, that collection separates for three times respectively sour water layer respectively.
2), in primary high-concentration waste sour water, add 125g sodium carbonate regulation pH=8, add 2.5g hydrazine hydrate, stirring
1h, filters, obtains Cr(OH) 3, content: 98.1%；Filtrate concentrate, until dense go out filtrate 2/5 time, be cooled to 10 DEG C of crystallize 4h, mistake
Filter obtains sodium acetate trihydrate, content: 60%；Dense go out 1L waste water and the fresh drinking water of 1L 2L altogether for next series-produced the
Three washings.
3), in second time and third time waste acid water, it is separately added into 4g sodium carbonate regulation pH=8, adds 1g hydrazine hydrate, stirring
1h, filters, obtains Cr(OH) 3, content: 98.3% and 98.5%, filtrate is respectively used to next series-produced first time and the
Secondary is washed.
Example 2:
1), taking 100g Saponin through open loop, the diene alcohol ketone acetic ester of oxydrolysis synthesis, 2L hexamethylene extracts
After, use batch of waste acid water respectively and carry out washing to neutral.
2), the 2L filtrate of using the washing of batch of second time carry out washing for the first time, wash layering and obtain high concentration spent acid
Water, adds 200g sodium carbonate regulation pH=9 in high-concentration waste sour water, adds 3.75g hydrazine hydrate, stir 1h, filter, obtain Cr
(OH) 3, content: 98%.Filtrate concentrate, until dense go out filtrate 3/5 time, be cooled to 15 DEG C of crystallize 6h, be filtrated to get three water acetic acid
Sodium, content: 61%.Dense go out waste water and the fresh drinking water of 1L 2L altogether wash for next series-produced third time.
3), in second time and third time waste acid water, it is separately added into 10g sodium carbonate regulation pH=9, adds 1.6g water and hydrazine,
Stirring 1h, filters, obtains Cr(OH) 3, content is respectively as follows: 98.2% and 98.1%, and it is series-produced that filtrate is respectively used to next
Wash with second time for the first time.
Example 3:
1), taking 100g Saponin through open loop, the diene alcohol ketone acetic ester of oxydrolysis synthesis, 2L hexamethylene extracts
After, use batch of waste acid water respectively and carry out washing to neutral.
2), the 2L filtrate of using the washing of batch of second time carry out washing for the first time, wash layering and obtain high concentration spent acid
Water, adds 125g sodium carbonate regulation pH=8 in high-concentration waste sour water, adds 2.5g hydrazine hydrate, stir 1h, filter, obtain Cr
(OH) 3, content: 98.3%.Filtrate concentrate, until dense go out filtrate 2/5 time, be cooled to 10 DEG C of crystallize 4h, be filtrated to get three water acetic acid
Sodium, content: 60%.Dense go out waste water for next series-produced third time wash.
3), in second time and third time waste acid water, it is separately added into 4g sodium carbonate regulation pH=8, adds 1g hydrazine hydrate, stirring
1h, filters, obtains Cr(OH) 3, content: 98.3% and 98.5%, filtrate is respectively used to next series-produced first time and the
Secondary is washed.
Claims (5)
1. the method that a diene alcohol ketone acetic ester waste acid water recycles, it is characterised in that: concretely comprise the following steps, take Saponin and pass through
Open loop, the diene alcohol ketone acetic ester of oxydrolysis synthesis, after hexamethylene extracts, washs hexamethylene layer with drinking water respectively
To neutral, collect the sour water layer separated for three times respectively three times；
1) for containing high concentration acetic acid diene waste acid water I, add sodium carbonate being neutralized to PH is 8 ~ 9, adds hydrazine hydrate stirring
Reaction, is filtrated to get Cr(OH)3And sodium acetate solution；By sodium acetate solution concentrate, dense go out liquid be low-concentration waste acid water IV, collect
Recycled；Reaction bulb cooling crystallize is filtrated to get Sodium acetate trihydrate solid；
2) for containing middle concentration acetic acid diene waste acid water II with containing low-concentration acetic acid waste acid water III, stirring lower addition sodium carbonate to PH
Being 8 ~ 9, add hydrazine hydrate, stirring reaction, after filtration, filtrate cycle utilizes；Diene alcohol ketone acetic ester is completed by above-mentioned steps
Recycling of waste acid water.
The method that a kind of diene alcohol ketone acetic ester waste acid water described in 1 recycles the most as requested, it is characterised in that: described step
Rapid 1) sodium carbonate described in: hydrazine hydrate: mass ratio=0.05 of waste acid water ~ 0.08:0.001 ~ 0.0015:1.
The method that a kind of diene alcohol ketone acetic ester waste acid water described in 1 recycles the most as requested, it is characterised in that: described step
Rapid 1) degree of concentrating under reduced pressure described in is be concentrated into original volume 2/5 ~ 3/5.
The method that a kind of diene alcohol ketone acetic ester waste acid water described in 1 recycles the most as requested, it is characterised in that: described step
Rapid 1) cooling crystallization parameter is temperature: 10 ~ 15 DEG C, the time is: 4 ~ 6h.
The method that a kind of diene alcohol ketone acetic ester waste acid water described in 1 recycles the most as requested, it is characterised in that: described step
Rapid 2) sodium carbonate described in described in: hydrazine hydrate: mass ratio=0.002 of waste acid water ~ 0.005:0.0005 ~ 0.0008:1.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5808117A (en) * | 1996-01-22 | 1998-09-15 | Chowdhury; Pritish Kumar | Process for the production of 16-Dehydropregenolone acetate form diosgenin |
| CN101508640A (en) * | 2009-04-02 | 2009-08-19 | 湖北民生工贸有限公司 | Method for recycling dilute acetic acid with azeotropic abstraction distillation |
| CN103274923A (en) * | 2013-05-28 | 2013-09-04 | 三峡大学 | Method for recycling dehydropregnenolone acetate waste liquor |
| CN103408175A (en) * | 2013-07-22 | 2013-11-27 | 沈阳理工大学 | Treatment and reclamation method of (methyl) acrylic acid production wastewater |
| CN104445132A (en) * | 2014-11-27 | 2015-03-25 | 三峡大学 | Method for preparing chromium phosphate by utilizing diene chrome waste liquid |
-
2015
- 2015-08-18 CN CN201510504637.9A patent/CN105061191B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5808117A (en) * | 1996-01-22 | 1998-09-15 | Chowdhury; Pritish Kumar | Process for the production of 16-Dehydropregenolone acetate form diosgenin |
| CN101508640A (en) * | 2009-04-02 | 2009-08-19 | 湖北民生工贸有限公司 | Method for recycling dilute acetic acid with azeotropic abstraction distillation |
| CN103274923A (en) * | 2013-05-28 | 2013-09-04 | 三峡大学 | Method for recycling dehydropregnenolone acetate waste liquor |
| CN103408175A (en) * | 2013-07-22 | 2013-11-27 | 沈阳理工大学 | Treatment and reclamation method of (methyl) acrylic acid production wastewater |
| CN104445132A (en) * | 2014-11-27 | 2015-03-25 | 三峡大学 | Method for preparing chromium phosphate by utilizing diene chrome waste liquid |
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