CN109503356A - A kind of method of heavy grey mother liquor preparation sodium acetate solution with high salt - Google Patents
A kind of method of heavy grey mother liquor preparation sodium acetate solution with high salt Download PDFInfo
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- CN109503356A CN109503356A CN201811567066.3A CN201811567066A CN109503356A CN 109503356 A CN109503356 A CN 109503356A CN 201811567066 A CN201811567066 A CN 201811567066A CN 109503356 A CN109503356 A CN 109503356A
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- mother liquor
- high salt
- sodium acetate
- acetate solution
- heavy grey
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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
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
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- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
The invention discloses a kind of methods of heavy grey mother liquor preparation sodium acetate solution with high salt.The sodium acetate solution of preparation meets the quality standard of sewage treatment plant's Dichlorodiphenyl Acetate sodium solution;First with tap water by heavy grey mother liquor dilution with high salt, then is mixed simultaneously by heavy grey mother liquor, acetic acid and the tap water with high salt after diluting and carry out reaction generation sodium acetate solution.The present invention prepares sodium acetate solution using the heavy grey mother liquor with high salt of combined soda method system outlet, not only provide the new method of preparation sodium acetate solution, also solve the expansion issues of heavy grey mother liquor with high salt in combined soda method industry, so that it is turned waste into wealth, is energy-saving, creating benefit, there is commercial introduction value.
Description
Technical field
The present invention relates to chemical field, specifically a kind of side of heavy grey mother liquor preparation sodium acetate solution with high salt
Method.
Background technique
Sodium acetate solution is the colorless and transparent homogeneous aqueous solution containing sodium acetate, is the one of sewage treatment plant's additional carbon
Kind.Carbon source is the major limitation of Biochemical method sewage technique as matter and energy source necessary to microorganism growth metabolism
Sexual factor.Due to the existing sewage treatment plant's denitrification process in China generally face it is low into water carbon-nitrogen ratio, be unable to satisfy normal micro- life
Object generally requires to add a certain amount of exogenous carbon to sewage disposal system to improve water outlet water to the needs of problems of carbon source
Matter.Sodium acetate solution has product qualification reliable, nontoxic, nonflammable explosive and sexual valence compared with other additional carbons such as methanol
Than it is high the advantages that, thus become the preferred carbon source of Most current sewage treatment plant.With wastewater treatment in China factory it is new (change,
Expand) build quantity and scale is more and more big, the demand of Dichlorodiphenyl Acetate sodium solution increasingly all increases, it is contemplated that has a extensive future.
Currently, the method system that domestic sodium acetate solution mainly uses acetic acid Yu sodium hydroxide (or sodium carbonate) solution reaction
It is standby, it is dissolved in obtained by water wherein reacting required sodium hydroxide (or sodium carbonate) solution by sodium hydroxide (or sodium carbonate) solid.By
There is strong impulse and corrosivity in sodium hydrate solid, and easily absorb water vapor in air and deliquesce, deliquesced
Journey releases a large amount of heat, therefore the packaging to sodium hydroxide, transport and to store range request very harsh.In addition, from thermal energy
Economy considers that sodium hydroxide (or sodium carbonate) solid is crystallized by its solution, dries gained, and in preparation sodium acetate solution
In application process, and sodium hydroxide (or sodium carbonate) solid is dissolved as solution, thermal energy is caused to waste.Therefore, using a kind of nothing
The harmless liquid sodium salt solution of poison and acetic acid reaction prepare sodium acetate solution, more meet the economy and the feature of environmental protection of chemical industry route.
During soda and sociation center production weight grey (sodium carbonate), when sodium chloride content reaches 80~90g/L in weight ash mother liquor
When, it with regard to required discharge unit mother liquor, and is added in systems into a certain amount of industrial sodium carbonate and water, to limit in mother liquor
Chlorinity guarantees that weight ash products are up-to-standard.Although part heavy grey mother liquor with high salt can be sent to sodium chloride refining step, system
In the heavy grey mother liquor with high salt that constantly accumulates seriously constrain the yield of weight ash, if its direct outlet is not only increased product
Unit consumption value does not only result in the wasting of resources, can also bring economic loss and environmental protection pressure.Therefore, the expansion of heavy grey mother liquor with high salt has been
As combined soda method Industry Demanding problem to be solved.
Summary of the invention
In order to solve the problems in the existing technology, the present invention provides a kind of heavy grey mother liquor preparation sodium acetate solution with high salt
Method, solve the problems, such as in combined soda method system weight ash mother liquor expansion.
Technical scheme is as follows:
A kind of sodium acetate solution of heavy grey mother liquor preparation with high salt;Meet the quality mark of sewage treatment plant's Dichlorodiphenyl Acetate sodium solution
It is quasi-;Quality standard is as follows:
Title | Excellent pure grade |
Content (sodium acetate), W/% | ≥18 |
pH | ≥6.0 |
Specific gravity | 1.10~1.13 |
COD | ≥140000 |
Appearance | It is transparent, without precipitating |
The method of one kind of the invention heavy grey mother liquor preparation sodium acetate solution with high salt, its step are as follows:
1) in dilution device, heavy grey mother liquor with high salt is added, tap water is added, stirs under room temperature to solution clear,
Deposit-free, the heavy grey mother liquor with high salt after being diluted;
2) in reaction unit, heavy grey mother liquor with high salt after tap water, acetic acid and dilution is added simultaneously, reaction temperature control
At 20~80 DEG C, stirring obtains sodium acetate solution after reaction.
Weight ash content is 300g/L in step 1) the heavy grey mother liquor with high salt, and heavy grey mother liquor temperature with high salt is 78~85 DEG C.
The volume ratio of the step 1) heavy grey mother liquor with high salt and tap water is 2:1~1:2.
Heavy grey mother liquor volume ratio 1:1:2~1:2:10 with high salt after the step 2) tap water, acetic acid and dilution.
The time is stirred at room temperature as 5-30min in the step 1);It is preferred that dilution mixing time is 10-15min, further preferably
Dilution stirring be 15min.
Step 2) the reaction time is 5-30min;Preferred reaction time is 10-15min, when further preferred reaction
Between be 15min.
Step 2) the preferable reaction temperature is 25-50 DEG C, and further preferred reaction temperature is 30 DEG C.
Dilution intermittently operated in dilution device.
The reaction process is operated batch-wise or continuously in reaction unit.
The beneficial effects of the present invention are:
Sodium acetate solution is the product that heavy grey mother liquor and acetic acid reaction with high salt generate, which can turn completely
Turn to sodium acetate solution.Compared to the method for sodium hydroxide (or sodium carbonate) solid preparation sodium acetate solution, the present invention utilizes connection
The heavy grey mother liquor with high salt for closing alkaline system outlet prepares sodium acetate solution, not only provides the new method of preparation sodium acetate solution,
The expansion issues of heavy grey mother liquor with high salt in combined soda method industry are also solved, so that it is turned waste into wealth, is energy-saving, creating benefit,
It is worth with commercial introduction.
Specific embodiment
Method provided by the invention is described in detail below with reference to embodiment, but the invention is not limited in any way.
Embodiment 1:
It is 300g/L that 100mL weight ash content is added in round-bottomed flask, and the heavy grey mother liquor with high salt that temperature is 78 DEG C is added
50mL tap water, is vigorously mixed at room temperature for, and is diluted to heavy grey mother liquor with high salt, mixing time is 5min, obtains 140mL
Heavy grey mother liquor with high salt after dilution.Reaction uses intermittently operated, will be with high salt heavy after 70mL tap water, 70mL acetic acid and dilution
(three's volume ratio is 1:1:2) is added into beaker in grey mother liquor, controls reaction temperature at 20 DEG C, stirs, reaction time 5min.
After reaction, solution appearance is transparent in achromaticity and clarification, and part still generates a small amount of bubble, and bottom is without precipitating;Through testing and analyzing,
Sodium acetate content is 23%, pH 6.42 in solution, and specific gravity 1.12, COD 220700mg/L reaches quality standards.
Embodiment 2:
It is 300g/L that 50mL weight ash content is added in round-bottomed flask, and the heavy grey mother liquor with high salt that temperature is 80 DEG C is added
50mL tap water, is vigorously mixed at room temperature for, and is diluted to heavy grey mother liquor with high salt, mixing time is 15min, obtains 92mL
Heavy grey mother liquor with high salt after dilution.Reaction uses intermittently operated, will be with high salt heavy after 23mL tap water, 28mL acetic acid and dilution
(three's volume ratio is 1:1.2:4) is added into beaker in grey mother liquor, controls reaction temperature at 25 DEG C, stirs, the reaction time
15min.After reaction, solution appearance is transparent in achromaticity and clarification, and bubble-free generates, and bottom is without precipitating;It is molten through testing and analyzing
Sodium acetate content is 23%, pH 7.57 in liquid, and specific gravity 1.12, COD 149200mg/L reaches quality standards.
Embodiment 3:
It is 300g/L that 50mL weight ash content is added in round-bottomed flask, and the heavy grey mother liquor with high salt that temperature is 82 DEG C is added
50mL tap water, is vigorously mixed at room temperature for, and is diluted to heavy grey mother liquor with high salt, mixing time is 10min, obtains 92mL
Heavy grey mother liquor with high salt after dilution.Reaction uses intermittently operated, will be with high salt heavy after 15mL tap water, 31mL acetic acid and dilution
(three's volume ratio is 1:2:6) is added into beaker in grey mother liquor, controls reaction temperature at 30 DEG C, stirs, reaction time 10min.
After reaction, solution appearance is transparent in achromaticity and clarification, and bubble-free generates, and bottom is without precipitating;Through testing and analyzing, vinegar in solution
Sour sodium content is 22%, pH 6.87, and specific gravity 1.12, COD 153000mg/L reaches quality standards.
Embodiment 4:
It is 300g/L that 50mL weight ash content is added in round-bottomed flask, and the heavy grey mother liquor with high salt that temperature is 85 DEG C is added
100mL tap water, is vigorously mixed at room temperature for, and is diluted to heavy grey mother liquor with high salt, mixing time is 20min, is obtained
Heavy grey mother liquor with high salt after 140mL dilution.Reaction uses intermittently operated, by the height after 14mL tap water, 28mL acetic acid and dilution
(three's volume ratio is 1:2:10) is added into beaker in the grey mother liquor of salt weight, controls reaction temperature at 50 DEG C, stirs, the reaction time
20min.After reaction, solution appearance is transparent in achromaticity and clarification, and bubble-free generates, and bottom is without precipitating;It is molten through testing and analyzing
Sodium acetate content is 21%, pH 8.21 in liquid, and specific gravity 1.12, COD 141300mg/L reaches quality standards.
Embodiment 5:
It is 300g/L that 50mL weight ash content is added in round-bottomed flask, and the heavy grey mother liquor with high salt that temperature is 80 DEG C is added
50mL tap water, is vigorously mixed at room temperature for, and is diluted to heavy grey mother liquor with high salt, mixing time is 30min, obtains 92mL
Heavy grey mother liquor with high salt after dilution.Reaction uses intermittently operated, will be with high salt heavy after 23mL tap water, 28mL acetic acid and dilution
(three's volume ratio is 1:1.2:4) is added into beaker in grey mother liquor, controls reaction temperature at 80 DEG C, stirs, the reaction time
30min.After reaction, solution appearance is transparent in achromaticity and clarification, and bubble-free generates, and bottom is without precipitating;It is molten through testing and analyzing
Sodium acetate content is 21%, pH 7.72 in liquid, and specific gravity 1.11, COD 144200mg/L reaches quality standards.
Embodiment 6:
It is 300g/L that 2.2L weight ash content is added in dilution device, and the heavy grey mother liquor with high salt that temperature is 80 DEG C is added
2.2L tap water, is vigorously mixed at room temperature for, and is diluted to heavy grey mother liquor with high salt, mixing time is 15min, and it is dilute to obtain 4L
Heavy grey mother liquor with high salt after releasing.Reaction is female by the heavy ash with high salt after 1L tap water, 1.2L acetic acid and dilution using continuous operation
Liquid is added simultaneously into reaction kettle (three's volume flow ratio be 1:1.2:4), and control reaction temperature is at 30 DEG C, the reaction time
15min.After reaction, solution appearance is transparent in achromaticity and clarification, and bubble-free generates, and bottom is without precipitating;It is molten through testing and analyzing
Sodium acetate content is 23%, pH 7.28 in liquid, and specific gravity 1.12, COD 153800mg/L reaches quality standards.
Although invention has been described above, but the invention is not limited in above-mentioned embodiment, on
The specific embodiment stated is only schematical, rather than restrictive, and those skilled in the art are of the invention
Under enlightenment, without deviating from the spirit of the invention, many variations can also be made, these belong to protection of the invention
Within.
Claims (10)
1. a kind of method of heavy grey mother liquor preparation sodium acetate solution with high salt, it is characterised in that steps are as follows:
1) in dilution device, heavy grey mother liquor with high salt is added, tap water is added, stirring is to solution clear under room temperature, without heavy
Starch, the heavy grey mother liquor with high salt after being diluted;
2) in reaction unit, heavy grey mother liquor with high salt after tap water, acetic acid and dilution is added simultaneously, reaction temperature is controlled 20
~80 DEG C, stirring obtains sodium acetate solution after reaction.
2. the method for heavy grey mother liquor preparation sodium acetate solution with high salt as described in claim 1, it is characterized in that the step 1) is high
Weight ash content is 300g/L in the grey mother liquor of salt weight, and heavy grey mother liquor temperature with high salt is 78~85 DEG C.
3. the method for heavy grey mother liquor preparation sodium acetate solution with high salt as described in claim 1, it is characterized in that the step 1) is high
The volume ratio of the grey mother liquor of salt weight and tap water is 2:1~1:2.
4. the method for heavy grey mother liquor preparation sodium acetate solution with high salt as described in claim 1, it is characterized in that the step 2) is certainly
The volume ratio of heavy grey mother liquor with high salt is 1:1:2~1:2:10 after water, acetic acid and dilution.
5. the method for heavy grey mother liquor preparation sodium acetate solution with high salt as described in claim 1, it is characterized in that the step 1) is stirred
Mixing the time is 5-30min.
6. the method for heavy grey mother liquor preparation sodium acetate solution with high salt as described in claim 1, it is characterized in that the step 2) is anti-
It is 5-30min between seasonable.
7. the method for heavy grey mother liquor preparation sodium acetate solution with high salt as described in claim 1, it is characterized in that the step 2) is anti-
It is 15min between seasonable.
8. the method for heavy grey mother liquor preparation sodium acetate solution with high salt as described in claim 1, it is characterized in that the step 2) is anti-
Answering temperature is 25-50 DEG C.
9. the method for heavy grey mother liquor preparation sodium acetate solution with high salt as described in claim 1, it is characterized in that the step 2) is anti-
Answering temperature is 30 DEG C.
10. the method for heavy grey mother liquor preparation sodium acetate solution with high salt as described in claim 1, it is characterized in that dilution is dilute
Intermittently operated in release device;Reaction process is operated batch-wise or continuously in reaction unit.
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EP0603548A1 (en) * | 1992-12-17 | 1994-06-29 | Hoechst Aktiengesellschaft | Acetate of sodium and alkaline earth metal, process of preparation and use |
CN101531582A (en) * | 2009-01-06 | 2009-09-16 | 云南省玉溪市溶剂厂有限公司 | Method for preparing sodium diacetate by industrial waste |
CN104445304A (en) * | 2014-12-09 | 2015-03-25 | 天津渤化永利化工股份有限公司 | Method for preparing basic magnesium carbonate by using combinative alkali system high-salt heavy-ash mother solution |
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EP0603548A1 (en) * | 1992-12-17 | 1994-06-29 | Hoechst Aktiengesellschaft | Acetate of sodium and alkaline earth metal, process of preparation and use |
CN101531582A (en) * | 2009-01-06 | 2009-09-16 | 云南省玉溪市溶剂厂有限公司 | Method for preparing sodium diacetate by industrial waste |
CN104445304A (en) * | 2014-12-09 | 2015-03-25 | 天津渤化永利化工股份有限公司 | Method for preparing basic magnesium carbonate by using combinative alkali system high-salt heavy-ash mother solution |
CN108892611A (en) * | 2018-06-27 | 2018-11-27 | 蓝保(厦门)水处理科技有限公司 | A kind of production technology of sodium acetate solution |
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