CN110372496A - A kind of method of electrodialysis purification neopentyl glycol sodium formate mixed liquor - Google Patents
A kind of method of electrodialysis purification neopentyl glycol sodium formate mixed liquor Download PDFInfo
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- CN110372496A CN110372496A CN201910811062.3A CN201910811062A CN110372496A CN 110372496 A CN110372496 A CN 110372496A CN 201910811062 A CN201910811062 A CN 201910811062A CN 110372496 A CN110372496 A CN 110372496A
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- neopentyl glycol
- sodium formate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/42—Electrodialysis; Electro-osmosis ; Electro-ultrafiltration; Membrane capacitive deionization
- B01D61/44—Ion-selective electrodialysis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/42—Electrodialysis; Electro-osmosis ; Electro-ultrafiltration; Membrane capacitive deionization
- B01D61/44—Ion-selective electrodialysis
- B01D61/46—Apparatus therefor
- B01D61/48—Apparatus therefor having one or more compartments filled with ion-exchange material, e.g. electrodeionisation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
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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
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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- Urology & Nephrology (AREA)
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Abstract
The invention discloses a kind of methods of electrodialysis purification neopentyl glycol sodium formate mixed liquor, the isolation and purification method technical field of the neopentyl glycol sodium formate mixed liquor generated when belonging to discrimination method production neopentyl glycol, thick solution is carried out processing separating formic sodium solution and neopentyl glycol solution by the electrodialysis plant with center liquid chamber by this method, is finally concentrated by evaporation the purity of the sodium formate and neopentyl glycol product that obtain up to 99% or more.Without additionally using extractant in subtractive process of the present invention, take a short time, removal of impurity is high, and neopentyl glycol almost recycles, and three waste discharge is few, environmental pollution is small, realizes the effective recycling of high-quality sodium formate, has good practical value.
Description
Technical field
The side of isolating and purifying the invention belongs to the neopentyl glycol sodium formate mixed liquor generated when discrimination method produces neopentyl glycol
Law technology field, and in particular to a kind of method of electrodialysis purification neopentyl glycol sodium formate mixed liquor, this method be both able to achieve pair
Sodium formate is purified, and can sufficiently recycle neopentyl glycol.
Background technique
Neopentyl glycol, the entitled 2,2-dimethyl-1,3-propanediol of chemistry, has good chemical reactivity, can be rapid
Participate in a variety of chemical reactions such as esterification, condensation and oxidation.Neopentyl glycol is mainly used for synthesizing unsaturated-resin, the painting of polyester powder
Material, oil-free alkyd resin, polyurethane foam plastic, insulating materials, polymerization inhibitor, synthesis aeroengine oil oil dope etc., together
When, neopentyl glycol or excellent solvent, the selection that can be used for aromatic hydrocarbons and naphthenic base hydrocarbon separate；Its regrowth is main
For automobile, weaving, medicine, pesticide, coating, petroleum and plastics etc..
Since u s company Texas Eastman realizes industrialized production first, neopentyl glycol is essentially all to pass through
Two-step method preparation: formaldehyde and isobutylaldehyde are condensed to yield hydroxyl valeral under basic catalyst effect；Hydroxy pivalin aldehyde is by restoring
Neopentyl glycol, reduction process can mainly use discrimination method or catalytic hydrogenation method.Discrimination method be exactly hydroxyl valeral and formaldehyde highly basic (such as
Sodium hydroxide) in the presence of be reduced to neopentyl glycol, formaldehyde is oxidized to formic acid, then with alkali formed formates (sodium formate
Deng), the mixed liquor of neopentyl glycol and sodium formate is ultimately formed, then by being refining to obtain neopentyl glycol.Catalytic hydrogenation method is hydroxyl
Neopentyl glycol is prepared under the effect of the catalyst, by hydrogenation reaction in base neovaleraldehyde.
Up to the present, domestic most of manufacturer is still using discrimination method production technology.But production method needs
A large amount of first bronsted lowry acids and bases bronsted lowry is consumed, and the purposes of the byproduct formic acid sodium generated is very limited, economic value is lower.First simultaneously
Sour sodium can largely be present in reaction product, not only influence product quality, and can make to the neopentyl glycol of high-purity
At very big difficulty.
The neopentyl glycol of discrimination method production at present mostly uses vaporizing extract process separation neopentyl glycol and sodium formate, i.e. neopentyl glycol, first
Acid sodium aqueous solution enters steam stripping at reduced pressure tower at high temperature, and steam distillation occurs for neopentyl glycol and superheated vapour, and gas phase is cooling
Neopentyl glycol aqueous solution is obtained, obtains product using dehydration, rectification under vacuum.Knot is precipitated in stripper tower bottom sodium formate supersaturation
Crystalline substance, centrifugal filtration, since vapor stripping temperature is about 120-140 DEG C, polymerization liquid meeting blackening occurs for impurity in reaction solution,
Therefore the sodium formate appearance obtained is brownish black crystallization, and sodium formate effective content is 85wt%-88wt%, separately has 3wt%-5wt% new
Pentanediol, other organic impurities 1wt%-3wt%, there are also the water of 5wt%-8wt% or so.
Method disclosed in Chinese patent CN 103483179B is decolourized by decolorising agent and flocculant, by evaporative crystallization energy
Access the sodium formate product of high-purity.It is de- using ultrafiltration, nanofiltration device in method disclosed in Chinese patent CN 103483178A
Color removal of impurities, the available white sodium formate of condensing crystallizing.But still have a certain amount of new penta 2 in the waste residue that both methods obtains
Alcohol cannot recycle use, increase cost.
Summary of the invention
In view of the deficienciess of the prior art, the object of the present invention is to provide a kind of electrodialysis to refine neopentyl glycol formic acid
The method of sodium mixed liquor, this method is easy to operate, and the three wastes are less, can sufficiently recycle the neopentyl glycol in crude product, while can
The high-quality sodium formate of white is obtained, and electrodialysis plant can recycle again, greatly reduce the life of neopentyl glycol
Produce overall cost.
The present invention adopts the following technical scheme that solve above-mentioned technical problem, and a kind of electrodialysis refines neopentyl glycol sodium formate
The method of mixed liquor, it is characterised in that detailed process are as follows: the neopentyl glycol sodium formate generated when discrimination method is produced neopentyl glycol
Mixed liquor carries out electrodialysis process by the five compartment electrodialysis plants with center liquid chamber, and the five compartments electrodialysis plant is by sun
Amberplex, anion-exchange membrane, anion-exchange membrane, cation-exchange membrane, cation-exchange membrane and anion-exchange membrane
It is arranged successively mixing liquid chamber, center liquid chamber I, sodium formate concentration liquid chamber, center liquid chamber II and the mixing five compartment list of liquid chamber of composition
Tuple rearranges, and neopentyl glycol sodium formate mixed liquor is added in the mixed liquor room of five compartment electrodialysis plants, center liquid chamber I
With in center liquid chamber II be filled with formic acid solution, sodium hydroxide solution or sodium formate solution, sodium formate concentration liquid chamber obtain first
Sour sodium concentrated solution, the sodium formate solution are concentrated by evaporation, crystallize to obtain the white sodium formate product that purity is higher than 99wt%, mixing
Liquid chamber obtains the neopentyl glycol solution of desalination, which obtains purity through vacuum evaporation and be higher than the white of 99wt%
Color solid neopentyl glycol.
Preferably, the mass concentration of neopentyl glycol is 1%-30% in the neopentyl glycol sodium formate mixed solution；It is described new
The mass concentration of sodium formate is 15%-90% in pentanediol sodium formate mixed solution.
Preferably, the cation-exchange membrane is the cation-exchange membrane for having selective penetrated property to sodium ion, the yin
Amberplex is the anion-exchange membrane for having selective penetrated property to formate ion
Preferably, the method for electrodialysis purification neopentyl glycol sodium formate mixed liquor, it is characterised in that specific steps are as follows: will
Discrimination method produces the mixed liquor that the neopentyl glycol sodium formate mixed liquor generated when neopentyl glycol is added to five compartment electrodialysis plants
Room, 21wt% containing sodium formate in the neopentyl glycol sodium formate mixed liquor, neopentyl glycol 27wt%, moisture 40wt%, it is other be a small amount of first
Sour and other impurity, sodium formate concentration liquid chamber obtains sodium formate concentrated solution in five compartment electrodialysis plants, sodium formate solution warp
It is concentrated by evaporation, the white sodium formate product that crystallization obtains purity as 99.1wt%, mixing liquid chamber obtains in five compartment electrodialysis plants
The neopentyl glycol solution of desalination, the neopentyl glycol solution through vacuum evaporation obtain purity be 99.3wt% white solid it is new
Pentanediol.
Preferably, the method for electrodialysis purification neopentyl glycol sodium formate mixed liquor, it is characterised in that specific steps
Are as follows: the neopentyl glycol sodium formate mixed liquor generated when discrimination method is produced neopentyl glycol is added to the mixed of five compartment electrodialysis plants
Close liquid chamber, 22.3wt% containing sodium formate in the neopentyl glycol sodium formate mixed liquor, neopentyl glycol 25.5wt%, moisture 39.4wt%, its
It is a small amount of formic acid and other impurity, and sodium formate concentration liquid chamber obtains sodium formate concentrated solution in five compartment electrodialysis plants, the first
Acid sodium solution is concentrated by evaporation, crystallizes to obtain the white sodium formate product that purity is 99.4wt%, is mixed in five compartment electrodialysis plants
It closes liquid chamber and obtains the neopentyl glycol solution of desalination, it is 99.1wt%'s which, which obtains purity through vacuum evaporation,
White solid neopentyl glycol.
Preferably, the method for electrodialysis purification neopentyl glycol sodium formate mixed liquor, it is characterised in that specific steps
Are as follows: the neopentyl glycol sodium formate mixed liquor generated when discrimination method is produced neopentyl glycol is added to the mixed of five compartment electrodialysis plants
Close liquid chamber, 85wt% containing sodium formate in the neopentyl glycol sodium formate mixed liquor, neopentyl glycol 5wt%, moisture 7wt%, it is other be a small amount of
Formic acid and other impurity, sodium formate concentration liquid chamber obtains sodium formate concentrated solution in five compartment electrodialysis plants, the sodium formate solution
It is concentrated by evaporation, crystallizes to obtain the white sodium formate product that purity is 99.6wt%, mixing liquid chamber obtains in five compartment electrodialysis plants
To the neopentyl glycol solution of desalination, which obtains the white solid that purity is 99.1wt% through vacuum evaporation
Neopentyl glycol.
Preferably, the method for electrodialysis purification neopentyl glycol sodium formate mixed liquor, it is characterised in that specific steps
Are as follows: the neopentyl glycol sodium formate mixed liquor generated when discrimination method is produced neopentyl glycol is added to the mixed of five compartment electrodialysis plants
Close liquid chamber, 87wt% containing sodium formate, neopentyl glycol 4.5wt%, moisture 6.5wt%, Qi Tawei in the neopentyl glycol sodium formate mixed liquor
A small amount of formic acid and other impurity, sodium formate concentration liquid chamber obtains sodium formate concentrated solution in five compartment electrodialysis plants, the sodium formate
Solution is concentrated by evaporation, crystallizes to obtain the white sodium formate product that purity is 99.7wt%, mixed liquor in five compartment electrodialysis plants
Room obtains the neopentyl glycol solution of desalination, which obtains the white that purity is 99.3wt% through vacuum evaporation
Solid neopentyl glycol.
Neopentyl glycol of the invention and sodium formate crystallization can be crystallized using multiple-effect evaporation, and conventional purification work can also be used
Skill.The electrodialysis process technique that the present invention uses has the spy for improving the sodium formate rate of recovery and raising sodium formate quality in thick solution
Point, while the rate of recovery of neopentyl glycol is also improved, greatly reduce the synthesis production cost of neopentyl glycol.
The neopentyl glycol sodium formate mixed liquor generated when the present invention is to using discrimination method production neopentyl glycol provides one kind
Refining methd, this method can be applied not only to the reaction solution of production neopentyl glycol, after can also be applied to neopentyl glycol extracting
Raffinate.Then this method can be obtained height by being concentrated by evaporation for first by thick solution by electrodialysis plant separating formic sodium salt
The sodium formate and neopentyl glycol of quality.The present invention is separated using five compartment electroosmose process, without additionally using extractant, newly
It is simple that pentanediol is further processed process, takes a short time, and removal of impurity is high, and energy consumption is lower.After the method for the present invention purification
Sodium formate and neopentyl glycol purity can reach 99% or more, and neopentyl glycol almost recycles in subtractive process, three waste discharge
Less, environmental pollution is small, realizes the effective recycling of resource, has good practical value.
Detailed description of the invention
Fig. 1 is five compartment electrodialysis plant structural unit schematic diagram in the present invention.
Specific embodiment
Illustrate technical solution of the present invention combined with specific embodiments below, but protection scope is without being limited thereto.Used in the present invention
Electrodialysis plant is that Germany produces cation-exchange membrane and anion-exchange membrane composition.
Embodiment 1
21wt% containing sodium formate in certain neopentyl glycol production reaction solution after measured, neopentyl glycol 27wt%, moisture 40wt%, other are
A small amount of formic acid and other impurities.Reaction solution is handled by five compartment electrodialysis plants, sodium formate concentrate solution room obtains
Sodium formate solution be concentrated by evaporation, crystallize to obtain the white sodium formate product that purity is 99.1wt%；Mixing liquid chamber obtains new
Pentanediol solution obtains the white solid neopentyl glycol that purity is 99.3wt% by vacuum evaporation.
Embodiment 2
22.3wt% containing sodium formate, neopentyl glycol 25.5wt%, moisture 39.4wt% in certain neopentyl glycol production reaction solution after measured,
Other are a small amount of formic acid and other impurities.Reaction solution is handled by five compartment electrodialysis plants, sodium formate concentrate solution
The sodium formate solution that room obtains is concentrated by evaporation, crystallizes to obtain the white sodium formate product that purity is 99.4wt%；Mixing liquid chamber obtains
To neopentyl glycol solution by vacuum evaporation obtain purity be 99.1wt% white solid neopentyl glycol.
Embodiment 3
85wt% containing sodium formate, neopentyl glycol 5wt%, moisture 7wt% in certain neopentyl glycol production reaction solution after measured, other are few
Measure formic acid and other impurities.Reaction solution is handled by five compartment electrodialysis plants, sodium formate concentrate solution room obtains
Sodium formate solution is concentrated by evaporation, crystallizes to obtain the white sodium formate product that purity is 99.6wt%；Mix liquid chamber obtains new penta
Glycol solution obtains the white solid neopentyl glycol that purity is 99.1wt% by vacuum evaporation.
Embodiment 4
87wt% containing sodium formate, neopentyl glycol 4.5wt%, moisture 6.5wt% in certain neopentyl glycol production reaction solution after measured, other
For a small amount of formic acid and other impurities.Reaction solution is handled by five compartment electrodialysis plants, sodium formate concentrate solution room obtains
To sodium formate solution be concentrated by evaporation, crystallize to obtain the white sodium formate product that purity is 99.7wt%；Mixing liquid chamber obtains
Neopentyl glycol solution obtains the white solid neopentyl glycol that purity is 99.3wt% by vacuum evaporation.
Basic principle of the invention, main feature and advantage has been shown and described above, do not depart from spirit of that invention and
Under the premise of range, there are also various changes and modifications, these changes and improvements to both fall within claimed invention by the present invention
Range.
Claims (4)
1. a kind of method of electrodialysis purification neopentyl glycol sodium formate mixed liquor, it is characterised in that detailed process are as follows: by discrimination method
When producing neopentyl glycol the neopentyl glycol sodium formate mixed liquor that generates by the five compartment electrodialysis plants with center liquid chamber into
Row electrodialysis process, the five compartments electrodialysis plant by cation-exchange membrane, anion-exchange membrane, anion-exchange membrane, sun from
It is dense that proton exchange, cation-exchange membrane and anion-exchange membrane are arranged successively the mixing liquid chamber of composition, center liquid chamber I, sodium formate
Contracting liquid chamber, center liquid chamber II and mixing five compartment unit group of liquid chamber rearrange, and neopentyl glycol sodium formate mixed liquor is added to five
It is molten filled with formic acid solution, sodium hydroxide in center liquid chamber I and center liquid chamber II in the mixed liquor room of compartment electrodialysis plant
Liquid or sodium formate solution, sodium formate concentration liquid chamber obtain sodium formate concentrated solution, which is concentrated by evaporation, crystallizes to obtain
Purity is higher than the white sodium formate product of 99wt%, and mixing liquid chamber obtains the neopentyl glycol solution of desalination, neopentyl glycol solution warp
Vacuum evaporation obtains the white solid neopentyl glycol that purity is higher than 99wt%.
2. the method for electrodialysis purification neopentyl glycol sodium formate mixed liquor according to claim 1, it is characterised in that: described
The mass concentration of neopentyl glycol is 1%-30% in neopentyl glycol sodium formate mixed solution.
3. the method for electrodialysis purification neopentyl glycol sodium formate mixed liquor according to claim 1, it is characterised in that: described
The mass concentration of sodium formate is 15%-90% in neopentyl glycol sodium formate mixed solution.
4. the method for electrodialysis purification neopentyl glycol sodium formate mixed liquor according to claim 1, it is characterised in that: described
Cation-exchange membrane be to sodium ion have selective penetrated property cation-exchange membrane, the anion-exchange membrane be to formic acid from
Son has the anion-exchange membrane of selective penetrated property.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113603565A (en) * | 2021-07-15 | 2021-11-05 | 浙江蓝波新材料科技有限公司 | Novel process for separating pentaerythritol and byproduct sodium formate by membrane method |
| CN114230441A (en) * | 2021-11-26 | 2022-03-25 | 南通百川新材料有限公司 | Electrodialysis membrane separation method for sodium formate in trimethylolpropane |
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| CN109809964A (en) * | 2019-03-04 | 2019-05-28 | 中国科学技术大学 | A method of neopentyl glycol is purified using bipolar membrane electrodialysis system |
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| CN1560023A (en) * | 2004-02-16 | 2005-01-05 | 浙江大学 | Process of separating DL-alpha lactamic acid by ion membrane electric dialysis method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113603565A (en) * | 2021-07-15 | 2021-11-05 | 浙江蓝波新材料科技有限公司 | Novel process for separating pentaerythritol and byproduct sodium formate by membrane method |
| CN114230441A (en) * | 2021-11-26 | 2022-03-25 | 南通百川新材料有限公司 | Electrodialysis membrane separation method for sodium formate in trimethylolpropane |
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