CN109336764A - A kind of ethyl alcohol, diphenyl carbonate, the separation method of dibutyl ester mixture and system - Google Patents
A kind of ethyl alcohol, diphenyl carbonate, the separation method of dibutyl ester mixture and system Download PDFInfo
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- CN109336764A CN109336764A CN201811430119.7A CN201811430119A CN109336764A CN 109336764 A CN109336764 A CN 109336764A CN 201811430119 A CN201811430119 A CN 201811430119A CN 109336764 A CN109336764 A CN 109336764A
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- ethyl alcohol
- temperature
- dbp
- diphenyl carbonate
- dibutyl ester
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C68/00—Preparation of esters of carbonic or haloformic acids
- C07C68/08—Purification; Separation; Stabilisation
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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
- 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
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/78—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by condensation or crystallisation
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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
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
Abstract
A kind of ethyl alcohol, diphenyl carbonate, dibutyl ester mixing organic matter separation method, it include: the hot solution that ethyl alcohol, DPC, DBP ternary are mixed to organic liquid waste, it is sent into crystallizer, circulating cooling, it is cooled to room temperature feed liquid temperature following, recycling centrifuge is separated, solid crystal, that is, DPC, liquid, that is, ethyl alcohol and DBP mixed solution；Ethyl alcohol and DBP mixed solution are sent into evaporator, using the size of temperature variable the control quantity of steam and material inlet of evaporator, evaporation separation, top escapes ethyl alcohol, cooling up to ethanol liquid by recirculated cooling water；Lower part outflow is DBP solution.A kind of ethyl alcohol, diphenyl carbonate, dibutyl ester mixing organic matter separation system, for realizing the above method.Simple operation, lower temperature are properly completed separation, and the main content of the DPC and ethyl alcohol that isolate meet Recycling requirement up to the main content of 98.5% or more, DBP also up to 97.0% or more, avoid waste of material, and save the cost protects environment.
Description
Technical field
The present invention relates to the separation of film waste liquid, especially with a kind of ethyl alcohol, diphenyl carbonate, dibutyl ester mixing organic matter
Separation method is related.
Background technique
Since in recent years, we are continuously improved living standard, and people increasingly pay attention to environmental protection, especially water resource
Protection and regeneration, thus result in the fast development of organic film producing industry.
In PVDF film producing industry, diphenyl carbonate (DPC) is widely used with dibutyl ester (DBP), is used as macromolecule crystal
Between filler, and the formation of polymeric membrane micropore needs to extract and clean using dehydrated alcohol, diphenyl carbonate (DPC) and two fourths
Ester (DBP) is dissolved in alcohol solvent, generates a large amount of ternary organic liquid waste, the method that these organic liquid wastes must use science
It is handled, otherwise, it will cause wastage of material, cost increases, and endangers the environment that we depend on for existence.
This ternary organic liquid waste separation is relatively difficult, and the past, common method was rectification under vacuum method, utilized each component
Boiling point difference is separated, and since the boiling point of ethyl alcohol is minimum (78.1 DEG C), rectifying first goes out ethyl alcohol, then rectifying goes out DPC, finally remains
Remaining DBP.Entire production process is intermittently operated, needs vacuum degree higher, is heated up higher, thus energy consumption is larger, and in rectifying
During will generate the substance containing phenol, be more toxic, pollute environment.
Summary of the invention
For above-mentioned prior art defect, a kind of separation of ethyl alcohol, diphenyl carbonate, dibutyl ester mixing organic matter of the present invention
Its ternary is mixed with machine waste liquid at lower temperature and is completely separated by method, simple operation, the DPC and second isolated
The main content of alcohol fully meets the requirement of product cycling and reutilization up to the main content of 98.5% or more, DBP also up to 97.0% or more,
Waste of material is avoided, save the cost protects environment.
The present invention uses following technology:
A kind of ethyl alcohol, diphenyl carbonate, dibutyl ester mixing organic matter separation method characterized by comprising
The hot solution that ethyl alcohol, DPC, DBP ternary are mixed to organic liquid waste, is sent into crystallizer, circulating cooling keeps feed liquid temperature cold
But to room temperature hereinafter, centrifuge is recycled to be separated, solid crystal, that is, DPC, liquid, that is, ethyl alcohol and DBP mixed solution；
It is sent into ethyl alcohol and DBP mixed solution in evaporator, is entered using the temperature variable control quantity of steam and material of evaporator
The size of amount, evaporation separation, top escape ethyl alcohol, cooling up to ethanol liquid by recirculated cooling water；Lower part outflow is that DBP is molten
Liquid.
Further, the temperature of the hot solution is 60-65 DEG C, the ternary waste liquid obtained for filming technology.
Further, in the crystallizer, 30 ~ 60r.min of mixing speed is controlled-1, the temperature control of crystallisation by cooling material is 8
~ 20 DEG C, cooling time is 2.5 ~ 4.5hr.
Further, the separating factor 800 ~ 1300 of the seperator.
Further, the temperature of the evaporator is set as 80-82 DEG C, inlet amount 20-25Hz, steam pressure 0.2-
0.3MPa。
Further, the hot solution pump is squeezed into crystallizer.
Further, the ethyl alcohol and DBP mixed solution pump are squeezed into evaporator.
A kind of ethyl alcohol, diphenyl carbonate, dibutyl ester mixing organic matter separation system, for realizing the above method, feature
It is, comprising:
Crystallizer carries out circulating cooling for ethyl alcohol, DPC, DBP ternary the mixing organic liquid waste to feeding；
Seperator, for being separated to crystallizer waste liquid after cooling；
Evaporator is evaporated separation for the mixed solution after separating to seperator.
Further, further include cooler, cooled down for escaping isolated ethyl alcohol to evaporator top.
Further, further include pump I, be respectively used to ethyl alcohol, the organic waste drains pump of DPC, DBP ternary mixing entering crystallizer；
It further, further include pump II, the mixed solution after seperator is separated is pumped into evaporator.
Further, the separating factor 800 ~ 1300 of seperator.
Further, the temperature of evaporator is set as 80-82 DEG C, inlet amount 20-25Hz, steam pressure 0.2-
0.3MPa。
Further, in a crystallizer, at 8 ~ 20 DEG C, cooling time is 2.5 ~ 4.5hr, is stirred for the temperature control of crystallisation by cooling material
Mix 30 ~ 60r.min of speed-1。
Further, crystallizer is DT crystallizer, and the evaporator is GMB.
The beneficial effects of the present invention are:
1, operation of the present invention is simplified, and low energy consumption, its ternary is mixed with machine waste liquid at a lower temperature and is completely separated,
The main content of the DPC and ethyl alcohol that isolate fully meet product and follow up to the main content of 98.5% or more, DBP also up to 97.0% or more
The requirement that ring recycles, avoids waste of material, and save the cost protects environment；
2, when crystallizing, crystallization temperature is controlled at 20 DEG C hereinafter, 8 ~ 20 DEG C are specifically chosen, using DPC under this temperature environment
Low-res, dissolution is few, is conducive to the cerium sulphate crystal to DPC, conducive to the subsequent material purity for improving separation and obtaining；Meanwhile 20
DEG C temperature close to underground water, be easy to be controlled；Meanwhile temperature being controlled at lower 20 DEG C hereinafter, being conducive to magma
The conveying of liquid or mother liquor, temperature is low, and crystallization process has been completed, and is a stable state, and the process of feed liquid conveying will not be tied again
Crystalline substance avoids blocking pipeline or valve；
3, during crystallization is formed, control mixing speed is 30 ~ 60r.min-1, not only it is conducive to be separated by solid-liquid separation, but also impurity content is precipitated
It is low, it is conducive to subsequent centrifuge separation, improves the material purity that separation obtains；If mixing speed is excessively slow, the larger of formation is referred to
Acicular crystal, not only than more loose, but also product impurity content is higher, although be conducive to be separated by solid-liquid separation, be easy blocking valve and
Pipeline；If mixing speed is too fast, product impurity content is higher；
4, in centrifuge separation, using separating factor 800 ~ 1300, preferably 1000, under the premise of guaranteeing cleanliness of disengagement, effectively
Centrifuge energy consumption is reduced, the issuable security risk of heavy-duty service is avoided；If separating factor is too low, cause separation not thorough
Bottom influences the main content of crystal product；
5, the size of quantity of steam and material inlet is controlled using the temperature variable of evaporator, temperature is according to ethyl alcohol in evaporator
Boiling point determines that the practical temperature that controls is determining by temperature higher than 3 ~ 5 DEG C of its boiling point, inlet amount and steam pressure, when temperature changes
When, it is lasting, stable conducive to carrying out to keep the temperature in evaporator to keep constant by adjusting inlet amount or steam pressure
Evaporation separation, improve the main content of separation product.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
In order to keep the purpose, technical solution and specific implementation method of the application apparent, in conjunction with attached Example to this Shen
It please be further elaborated.
Firstly, summing up dissolution law of the DPC in ethyl alcohol and DBP mixed solution:
When temperature is lower than 15 DEG C, the solubility very little of DPC is not almost dissolved；
When temperature is higher than 50 DEG C, the solubility of DPC linearly rises；
When temperature is close to ethyl alcohol boiling point, almost in the solution to dissolve each other.
Specific method is:
Quantitative high-purity DPC is dissolved in the ethyl alcohol and DBP mixed solution of preparation, and the ratio of ethyl alcohol and DBP are according to filming technology
Ratio is prepared, and dissolves, such as 60 DEG C under assigned temperature, saturated solution is made, temperature filtration calculates in the saturated solution
The meltage of DPC, then its saturated solution is divided into several equal portions, different temperature spots is cooled to respectively and is sampled, in its phase
Temperature filtration at a temperature of answering, solid/crystal weight, that is, undissolved DPC are differed with primary quantity Ji Wei the molten of DPC at this temperature
Xie Du.
The solubility of table one, DPC in ethyl alcohol and DBP mixed solution:
| Temperature (DEG C) | 5 | 10 | 20 | 30 | 40 | 50 | 60 | 70 |
| Solubility (g/100g) | 0.030 | 0.034 | 0.090 | 0.195 | 0.480 | 1.256 | 5.732 | 13.831 |
Data find out 5 DEG C, 10 DEG C and 20 DEG C from table, solubility of the DPC in ethyl alcohol and DBP mixed solution at a temperature of these
Very low, especially lower in 10 DEG C or less solubility, nearly close to zero, and changes in solubility is little, is a stationary value,
That is the DPC dissolved in mixed solution is less, and at 5 DEG C, 10 DEG C, solubility is almost unchanged, is a stationary value；It is super
20 DEG C or more solubility are crossed then to increase at multiple.20 DEG C of temperature below of selection are implemented.
According to above-mentioned dissolution law, decomposed using process line figure as shown in Figure 1:
Separation method:
1, it is separated using the property that solubility with temperature of the DPC in ethyl alcohol and DBP mixed solution changes greatly.
Specific method:
By the ethyl alcohol generated in film producing industry, DPC, DBP ternary mix organic liquid waste hot solution, about 60-65 DEG C of temperature, with pump
It squeezes into DT crystallizer, using freezing liquid circulating cooling, is cooled to room temperature feed liquid temperature hereinafter, recycling separating factor 1000
Centrifuge separated, solid crystal, that is, DPC, liquid, that is, ethyl alcohol and DBP mixed solution will be delivered to next procedure and divided
From.
2,78.1 DEG C of the boiling point of ethyl alcohol, 340 DEG C of the boiling point of DBP, differed using ethyl alcohol with the boiling point of DBP biggish property into
Row separation.
Specific method:
It by the ethyl alcohol of previous process and DBP mixed solution, is squeezed into GMB evaporator with pump, using the temperature variable control of evaporator
The size of quantity of steam processed and material inlet；Temperature is determined according to the boiling point of ethyl alcohol in evaporator, and the practical temperature that controls is higher than it
3 ~ 5 DEG C of boiling point；The temperature of general evaporator is set as 80-82 DEG C, inlet amount 20-25Hz, steam pressure 0.2-0.3MPa.
When the temperature is low, steam pressure is constant, it is possible to reduce inlet amount, compensation temperature value make it maintain temperature constant；
When the temperature is low, inlet amount is constant, can increase steam pressure, and compensation temperature value makes it maintain temperature constant；
When the temperature is high, steam pressure is constant, can increase inlet amount, and reducing temperature value makes it maintain temperature constant；
When the temperature is high, inlet amount is constant, can reduce steam pressure, and reducing temperature value makes it maintain temperature constant.
The evolution of evaporator top is ethyl alcohol, cooling up to ethanol liquid by recirculated cooling water；Lower part outflow is that DBP is molten
Liquid.
A kind of ethyl alcohol, diphenyl carbonate, dibutyl ester mixing organic matter separation system, for realizing the above method, comprising:
Crystallizer carries out circulating cooling for ethyl alcohol, DPC, DBP ternary the mixing organic liquid waste to feeding；
Seperator, for being separated to crystallizer waste liquid after cooling；
Evaporator is evaporated separation for the mixed solution after separating to seperator；
Cooler is cooled down for escaping isolated ethyl alcohol to evaporator top；
I is pumped, is respectively used to ethyl alcohol, the organic waste drains pump of DPC, DBP ternary mixing entering crystallizer；
II is pumped, the mixed solution after seperator is separated is pumped into evaporator；
Wherein, the separating factor 1000 of seperator；Using evaporator temperature variable control quantity of steam and material inlet it is big
Small, the temperature of evaporator is set as 80-82 DEG C, inlet amount 20-25Hz, steam pressure 0.2-0.3MPa；Crystallizer is DT
Crystallizer, evaporator GMB.
Example 1:
By 1.5m3The ethyl alcohol of film producing industry generation, DPC, DBP ternary mix organic liquid waste, and temperature 60 C is used by Constant-temp. pipeline
Pump is squeezed into DT crystallizer, and mixing speed 45r.min is controlled-1, open coolant liquid circulating cooling, the temperature of general crystallisation by cooling material
Control is at 8 DEG C, and 4hr, was then squeezed into the centrifuge of separating factor 1000 with pump and separated cooling time, obtains DPC weight
Amount is 65kg, and the content that DPC is detected after dry is 99.5%, can return to use；
Liquid after separation is squeezed into GMB evaporator again and is evaporated, and the frequency that the temperature in GMB evaporator is 80 DEG C of feed pumps is controlled
Rate is 20Hz, and steam pressure 0.3MPa, continuous evaporation 3hr is up to 1.3m3Ethanol solution, through inspection the main content of ethyl alcohol
98.5%, it can equally return to use；
The remaining DBP in GBM evaporator lower part is 85kg, and detecting main content is 97.5%, or returns and use.
Example 2:
By 1.5m3The ethyl alcohol of film producing industry generation, DPC, DBP ternary mix organic liquid waste, 65 DEG C of temperature, are used by Constant-temp. pipeline
Pump is squeezed into DT crystallizer, and mixing speed 30r.min is controlled-1, open coolant liquid circulating cooling, the temperature of general crystallisation by cooling material
Control is at 15 DEG C, and 2.5hr, was then squeezed into the centrifuge of separating factor 1300 with pump and separated, obtain DPC cooling time
Weight is 64.5kg, and the content that DPC is detected after dry is 99.4%, can return to use；
Liquid after separation is squeezed into GMB evaporator again and is evaporated, and the frequency that the temperature in GMB evaporator is 82 DEG C of feed pumps is controlled
Rate is 25Hz, and steam pressure 0.2MPa, continuous evaporation 3hr is up to 1.35m3Ethanol solution, through inspection the main content of ethyl alcohol
98.6%, it can equally return to use；
The remaining DBP in GBM evaporator lower part is 84.5kg, and detecting main content is 97.8%, or returns and use.
Example 3:
By 1.5m3The ethyl alcohol of film producing industry generation, DPC, DBP ternary mix organic liquid waste, and temperature is 62 DEG C, pass through Constant-temp. pipeline
It is squeezed into DT crystallizer with pump, controls mixing speed 60r.min-1, open coolant liquid circulating cooling, the temperature of general crystallisation by cooling material
Degree control is at 20 DEG C, and 4.5hr, was then squeezed into the centrifuge of high separating factor with pump and separated, obtain DPC cooling time
Weight is 63.8kg, and the content that DPC is detected after dry is 99.3%, can return to use；
Liquid after separation is squeezed into GMB evaporator again and is evaporated, and the frequency that the temperature in GMB evaporator is 81 DEG C of feed pumps is controlled
Rate is 22Hz, and steam pressure 0.25MPa, continuous evaporation 3hr are up to 1.28 m3Ethanol solution, through inspection the main content of ethyl alcohol
98.9%, it can equally return to use；
The remaining DBP in GBM evaporator lower part is 86.2kg, and detecting main content is 97.2%, or returns and use.
Operation of the present invention is simplified, its ternary is mixed with machine waste liquid at lower temperature and is completely separated, is isolated
DPC and ethyl alcohol main content up to the main content of 98.5% or more, DBP also up to 97.0% or more, it is sharp again to fully meet product circulation
It is required that avoiding waste of material, save the cost protects environment.
Claims (10)
1. a kind of ethyl alcohol, diphenyl carbonate, dibutyl ester mixing organic matter separation method characterized by comprising
The hot solution that ethyl alcohol, DPC, DBP ternary are mixed to organic liquid waste, is sent into crystallizer, circulating cooling keeps feed liquid temperature cold
But to room temperature hereinafter, centrifuge is recycled to be separated, solid crystal, that is, DPC, liquid, that is, ethyl alcohol and DBP mixed solution；
It is sent into ethyl alcohol and DBP mixed solution in evaporator, is entered using the temperature variable control quantity of steam and material of evaporator
The size of amount, evaporation separation, top escape ethyl alcohol, cooling up to ethanol liquid by recirculated cooling water；Lower part outflow is that DBP is molten
Liquid.
2. the separation method of ethyl alcohol according to claim 1, diphenyl carbonate, dibutyl ester mixing organic matter, feature exist
In the temperature of the hot solution is 60-65 DEG C.
3. the separation method of ethyl alcohol according to claim 1, diphenyl carbonate, dibutyl ester mixing organic matter, feature exist
In, in the crystallizer, control 30 ~ 60r.min of mixing speed-1, the temperature of crystallisation by cooling material is controlled at 8 ~ 20 DEG C, when cooling
Between be 2.5 ~ 4.5hr.
4. the separation method of ethyl alcohol according to claim 1, diphenyl carbonate, dibutyl ester mixing organic matter, feature exist
In the separating factor 800 ~ 1300 of the seperator.
5. the separation method of ethyl alcohol according to claim 1, diphenyl carbonate, dibutyl ester mixing organic matter, feature exist
In the temperature of the evaporator is set as 80-82 DEG C, inlet amount 20-25Hz, steam pressure 0.2-0.3MPa.
6. the separation method of ethyl alcohol according to claim 1, diphenyl carbonate, dibutyl ester mixing organic matter, feature exist
In the hot solution is squeezed into crystallizer by Constant-temp. pipeline pump, and the ethyl alcohol and DBP mixed solution pump squeeze into evaporator
In.
7. a kind of ethyl alcohol, diphenyl carbonate, dibutyl ester mixing organic matter separation system are appointed for realizing in such as claim 1 ~ 5
Ethyl alcohol, diphenyl carbonate, dibutyl ester mixing organic matter separation method described in meaning one characterized by comprising
Crystallizer carries out circulating cooling for ethyl alcohol, DPC, DBP ternary the mixing organic liquid waste to feeding；
Seperator, for being separated to crystallizer waste liquid after cooling；
Evaporator is evaporated separation for the mixed solution after separating to seperator.
8. ethyl alcohol according to claim 7, diphenyl carbonate, dibutyl ester mixing organic matter separation system, the seperator
Separating factor 800 ~ 1300.
9. ethyl alcohol according to claim 7, diphenyl carbonate, dibutyl ester mixing organic matter separation system, the evaporator
Temperature be set as 80-82 DEG C, inlet amount 20-25Hz, steam pressure 0.2-0.3MPa.
10. ethyl alcohol according to claim 7, diphenyl carbonate, dibutyl ester mixing organic matter separation system, the crystallization
Device, at 8 ~ 20 DEG C, cooling time is 2.5 ~ 4.5hr, 30 ~ 60r.min of mixing speed for the temperature control of crystallisation by cooling material-1。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112387226A (en) * | 2020-11-11 | 2021-02-23 | 润泰化学（泰兴）有限公司 | Dealcoholization tower for producing isobutyl 2,2, 4-trimethyl-3-hydroxypentanoate |
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| EP0687666A1 (en) * | 1994-06-15 | 1995-12-20 | Bayer Ag | Process for purifying diphenyle carbonate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112387226A (en) * | 2020-11-11 | 2021-02-23 | 润泰化学（泰兴）有限公司 | Dealcoholization tower for producing isobutyl 2,2, 4-trimethyl-3-hydroxypentanoate |
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