CN102304026A - Method for removing residual catalyst in bisphenol A reaction liquid - Google Patents
Method for removing residual catalyst in bisphenol A reaction liquid Download PDFInfo
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- CN102304026A CN102304026A CN201110184292A CN201110184292A CN102304026A CN 102304026 A CN102304026 A CN 102304026A CN 201110184292 A CN201110184292 A CN 201110184292A CN 201110184292 A CN201110184292 A CN 201110184292A CN 102304026 A CN102304026 A CN 102304026A
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- bisphenol
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
Abstract
The invention relates to a method for removing residual catalyst in bisphenol A reaction liquid from the production of the chemical material. The method is capable of removing the residual acid catalyst in the bisphenol A reaction liquid and improving the quality of the bisphenol A. The technical scheme comprises the following steps of: inputting the bisphenol A reaction liquid or acid-removing assistant of the bisphenol A reaction liquid into a mixer through an inputting pipe; and then inputting the liquid into an adsorber, wherein the adsorber is a tube-type device and the tube-type device is filled with the fiber film coalescence material; inputting hot water into a shell layer of the tube, wherein the acidity of the bisphenol A reaction liquid is smaller than or equal to 0.001 mmol/L and meets the requirement after the liquid is adsorbed by the adsorber; then directly outputting the bisphenol A reaction liquid through an outputting pipe; inputting acetone solvent into the adsorber to wash the fiber film coalescence material when the acidity is more than 0.001 mmol/L; inputting the washed acetone into a solvent pot to be recycled or be recycled after the acetone is distilled. The method provided by the invention has the advantages of low investment and simple process flow; the method does not lead in other impurities and does not change the performance of the bisphenol A; the temperature for deacidifying is low, the solvent can be recycled and the method can be used for producing the bisphenol A.
Description
Technical field
The present invention relates to a kind of method that industrial chemicals production removes remainder catalyst in the bisphenol-a reaction liquid that is used for.
Technical background
Dihydroxyphenyl propane is an important chemical material; It is not only the monomer of making Resins, epoxy, polycarbonate, polysulfones, and is one of broad-spectrum raw material in the organic synthesis industry, the performance of its quality affects resin; Therefore, the purifying of dihydroxyphenyl propane is a major issue in the industry.In ion method bisphenol-a reaction building-up process; Resin catalyst can discharge free acid; Cause the corrosion damage of equipment, instrument; And because the existence of free acid; Cause dihydroxyphenyl propane in high temperature unit film evaporation treating process, to decompose, generate the polymer heavy constituent, influence the color and luster and the purity of dihydroxyphenyl propane; And increased the polymer reorganization tar residue amount of grading, influenced the unit consumption of raw material phenol.Therefore, must remove an acidic catalyst remaining in the bisphenol-a reaction liquid.
The method that removes residual catalyst in the at present relevant bisphenol-a reaction liquid mainly contains: (1) weakly alkaline ion method: on bisphenol A device, join a strainer that weak base anion-exchange resin is housed, be used for catching, collecting the free acid that reaction process discharges.This method exists the regeneration washing process of acid removal filter than very complicated, problems such as operation, investment cost height; (2) alkali-sour reprecipitation method: dihydroxyphenyl propane solubility property in alkali is good, can generate the corresponding metal derivative, and follow some by product of dihydroxyphenyl propane to be difficult to be dissolved in the alkali, can in solution, add acid then through removing by filter, and just separates out pure dihydroxyphenyl propane.But the existence of alkaline matter can cause the deterioration by oxidation of dihydroxyphenyl propane, makes in the reaction system material painted, and it is bad that the quality of dihydroxyphenyl propane becomes; Need set up the decolouring device for this reason; Add activated carbon to solution processings of decolouring, thereby make technical process complicated, the process cost increase.
Summary of the invention
The objective of the invention is to: in order to solve the problem that residual catalyst removes in the bisphenol-a reaction liquid, improve the quality of dihydroxyphenyl propane, the spy provides a kind of method that removes residual catalyst in the bisphenol-a reaction liquid.
In order to achieve the above object; The present invention adopts following technical scheme: a kind of method that removes residual catalyst in the bisphenol-a reaction liquid; It is characterized in that: earlier with bisphenol-a reaction liquid or with the depickling auxiliary agent mixed solution of bisphenol-a reaction liquid and 1-2%; It is even to be conveyed into mixer mixing through the reaction solution input tube; The depickling auxiliary agent is a kind of of water or methyl alcohol, or is the mixed solution of water and methyl alcohol; Secondly the mixed solution in the mixing tank is conveyed into adsorber A and adsorber B; Adsorber A and adsorber B are the shell and tube device; Filling fiber film coalescence material in the tubulation; The outer shell of tubulation feeds 80-90 ℃ hot water; Play the effect of insulation and dry adsorption bed; The bisphenol-a reaction flow is after the adsorber adsorption treatment, and its acidity≤0.001mmol/L meets processing requirements, and bisphenol-a reaction liquid is defeated outside the reaction solution output tube is direct; When the acidity of after treatment bisphenol-a reaction liquid＞0.001mmol/L; Adsorption stuffing in the adsorber needs regeneration after treatment; With the acetone soln in the solvent tank with pump delivery to adsorber A and adsorber B washing the fibre film coalescence material; Clean with recycling in the acetone soln input solvent tank later; Or through the distillation of interchanger input distillation tower; Acetone soln after the recovery is stored in Recycling in the solvent tank through interchanger; Distillation back resultant product is main with an acidic catalyst water, does further processing by the output of waste liquid output tube; Import the adsorber shell with 80-90 ℃ hot water through the hot water input tube at last, tunica fibrosa coalescence material in oven dry adsorber A and the adsorber B tubulation, the solvent acetone that steams is stored in and supplies in the solvent tank to recycle.
Produce channel for avoiding handling bisphenol-a reaction liquid exit, back on adsorber top, establishing tunica fibrosa coalescence material layer top is h apart from the height at adsorber top, and tunica fibrosa coalescence material layer bottom is H apart from the height at adsorber top, and the relation of H and h is:
h=(1/2～2/3)H
The tunica fibrosa that the present invention adopts the sorbing material of strongly hydrophilic to process, as filler, the adsorber volume space velocity is 25-35m
3/ h, temperature is 55-75 ℃; The regeneration of adsorber filler; Regenerated solvent is to use acetone soln, and the acetone consumption is that bed is handled the long-pending 1/3-2/3 of bisphenol-a reaction liquid, and the volume ratio of fresh acetone and acetone recycle is 1: 1 or 3: 7; Regeneration temperature is 45-55 ℃, and the regenerated volume space velocity is 80-90m
3/ h; The oven dry of adsorber is to use in the adsorber shell 80-90 ℃ hot water.
The invention has the beneficial effects as follows: the tunica fibrosa that the sorbing material of (1) this process using strongly hydrophilic is processed; As filler; It can select the minor amount of water in the adsorbing and removing bisphenol-a reaction liquid, and free an acidic catalyst soluble in water is along with minor amount of water is removed together; (2) this technological equipment investment is low, and technical process is simple, and is easy to operate, and process cost is low, do not see domestic and international report; (3) this process using physisorphtion removes the micro free an acidic catalyst in the bisphenol-a reaction liquid, does not use any strong acid and strong base, in bisphenol-a reaction liquid, does not introduce new impurity, can not change the character of dihydroxyphenyl propane, can not make the quality of dihydroxyphenyl propane become bad; (4) the depickling temperature of this technology is low, and adsorption temp is 55-75 ℃, has remarkable energy saving effect; (5) regenerative operation of this process unit is easy, and expense is low, and energy consumption is low, the regenerated solvent reusable edible.
Description of drawings
Fig. 1 removes the residual catalyst schematic representation of apparatus in the bisphenol-a reaction liquid of the present invention.
Fig. 2 is for removing the structural representation of adsorber in the residual catalyst device in the bisphenol-a reaction liquid of the present invention.
Among the figure: 1. reaction solution input tube; 2. mixing tank; 3. adsorber A; 4. adsorber B; 5. hot water input tube; 6. reaction solution output tube; 7. solvent tank; 8. pump; 9. distillation tower; 10. interchanger; 11. waste liquid output tube; 12. tunica fibrosa coalescence material.
Embodiment
Embodiment 1: it is in the adsorber device of filler that bisphenol-a reaction liquid is added with fiber mould coalescence material, and temperature is controlled at 75 ℃, and normal pressure, volume space velocity are 25m
3/ h; The amount that this device can be handled bisphenol-a reaction liquid continuously is 35 times of packing volume; When the dihydroxyphenyl propane of handling does not meet the acidity requirement; The filler of device needs regeneration; (consumption is got 2/3 by handling the bisphenol-a reaction liquid measure with hot acetone flushing arrangement filler; Wherein fresh acetone respectively accounts for 50% with recovery acetone consumption), the volume space velocity of acetone is 80m
3/ h, regeneration temperature is 55 ℃, the device filler after the regeneration can return to original processing power.
Embodiment 2: it is in the adsorber device of filler that bisphenol-a reaction liquid is added with fiber mould coalescence material, and temperature is controlled at 75 ℃, and normal pressure, volume space velocity are 25 m
3/ h; The amount that this device can be handled bisphenol-a reaction liquid continuously is 35 times of packing volume; When the dihydroxyphenyl propane of handling does not meet the acidity requirement; The filler of device needs regeneration; (consumption is got 1/3 by handling the bisphenol-a reaction liquid measure with hot acetone flushing arrangement filler; Wherein fresh acetone is 3: 7 with recovery acetone amount ratio), the volume space velocity of acetone is 85 m
3/ h, regeneration temperature is 50 ℃, the device filler after the regeneration can return to original processing power.
Embodiment 3: it is in the adsorption unit of filler that bisphenol-a reaction liquid is added with fiber mould coalescence material, and temperature is controlled at 75 ℃, and normal pressure, volume space velocity are 25 m
3/ h; The amount that this device can be handled bisphenol-a reaction liquid continuously is 35 times of packing volume; When the dihydroxyphenyl propane of handling does not meet the acidity requirement; The filler of device needs regeneration; (consumption is got 1/3 by handling the bisphenol-a reaction liquid measure with hot acetone flushing arrangement filler; Wherein fresh acetone is 1: 1 with recovery acetone amount ratio), the volume space velocity of acetone is 90 m
3/ h, regeneration temperature is 45 ℃, the device filler after the regeneration can return to original processing power.
Embodiment 4: it is in the adsorption unit of filler that bisphenol-a reaction liquid is added with fiber mould coalescence material, and temperature is controlled at 75 ℃, and normal pressure, volume space velocity are 35 m
3/ h; The amount that this device can be handled bisphenol-a reaction liquid continuously is 60 times of packing volume; When the dihydroxyphenyl propane of handling does not meet the acidity requirement; The filler of device needs regeneration; (consumption is got 1/3 by handling the bisphenol-a reaction liquid measure with hot acetone flushing arrangement filler; Wherein fresh acetone respectively accounts for 50% with recovery acetone consumption), the volume space velocity of acetone is 80 m
3/ h, regeneration temperature is 50 ℃, the device filler after the regeneration can return to original processing power.
Embodiment 5: it is in the adsorption unit of filler that bisphenol-a reaction liquid is mixed with 1% water that the back adds with fiber mould coalescence material, and temperature is controlled at 75 ℃, and normal pressure, volume space velocity are 35 m
3/ h; The amount that this device can be handled bisphenol-a reaction liquid continuously is 35 times of packing volume; When the dihydroxyphenyl propane of handling does not meet the acidity requirement; The filler of device needs regeneration; (consumption is got 1/3 by handling the bisphenol-a reaction liquid measure with hot acetone flushing arrangement filler; Wherein fresh acetone respectively accounts for 50% with recovery acetone consumption), the volume space velocity of acetone is 85 m
3/ h, regeneration temperature is 45 ℃, the device after the regeneration can return to original processing power.
Embodiment 6: it is in the adsorption unit of filler that bisphenol-a reaction liquid is mixed with 2% water that the back adds with the fiber mold materials, and temperature is 75 ℃, and normal pressure, volume space velocity are 35 m
3/ h; The amount that this device can be handled bisphenol-a reaction liquid continuously is 35 times of packing volume; When the dihydroxyphenyl propane of handling does not meet the acidity requirement; The filler of device needs regeneration; (consumption is got 2/3 by handling the bisphenol-a reaction liquid measure with hot acetone flushing arrangement filler; Wherein fresh acetone respectively accounts for 50% with recovery acetone consumption), the air speed of acetone is 90 m
3/ h, the volume regeneration temperature is 55 ℃, the device after the regeneration can return to original processing power.
Embodiment 7: it is in the adsorption unit of filler that bisphenol-a reaction liquid is added with fiber mould coalescence material, and temperature is controlled at 65 ℃, and normal pressure, volume space velocity are 35 m
3/ h; The amount that this device can be handled bisphenol-a reaction liquid continuously is 10 times of packing volume; When the dihydroxyphenyl propane of handling does not meet the acidity requirement; The filler of device needs regeneration; (consumption is got 1/3 by handling the bisphenol-a reaction liquid measure with hot acetone flushing arrangement filler; Wherein fresh acetone is 3: 7 with recovery acetone amount ratio), the volume space velocity of acetone is 85 m
3/ h, regeneration temperature is 50 ℃, the device filler after the regeneration can return to original processing power.
Embodiment 8: it is in the adsorption unit of filler that bisphenol-a reaction liquid is added with fiber mould coalescence material, and temperature is 55 ℃, and normal pressure, volume space velocity are 35 m
3/ h; The amount that this device can be handled bisphenol-a reaction liquid continuously is 24 times of packing volume; When the dihydroxyphenyl propane of handling does not meet the acidity requirement; The filler of device needs regeneration; (consumption is got 1/3 by handling the bisphenol-a reaction liquid measure with hot acetone flushing arrangement filler; Wherein fresh acetone respectively accounted for 3: 7 with recovery acetone consumption), the volume space velocity of acetone is 80 m
3/ h, regeneration temperature is 45 ℃, the device filler after the regeneration can return to original processing power.
Embodiment 9: it is in the adsorption unit of filler that bisphenol-a reaction liquid is mixed with 1% water that the back adds with fiber mould coalescence material, and temperature is 55 ℃, and normal pressure, volume space velocity are 35 m
3/ h; The amount that this device can be handled the dihydroxyphenyl propane reaction solution continuously is 24 times of packing volume; When the dihydroxyphenyl propane of handling does not meet the acidity requirement; The filler of device needs regeneration; (consumption is got 2/3 by handling the bisphenol-a reaction liquid measure with hot acetone flushing arrangement filler; Wherein fresh acetone respectively accounts for 50% with recovery acetone consumption), the volume space velocity of acetone is 85 m
3/ h, regeneration temperature is 55 ℃, the device filler after the regeneration can return to original processing power.
Embodiment 10: it is in the adsorption unit of filler that bisphenol-a reaction liquid is mixed with 2% water that the back adds with fiber mould coalescence material, and temperature is 55 ℃, and normal pressure, volume space velocity are 35 m
3/ h; The amount that this device can be handled the dihydroxyphenyl propane reaction solution continuously is 24 times of packing volume; When the dihydroxyphenyl propane of handling does not meet the acidity requirement; The filler of device needs regeneration; (consumption is got 1/3 by handling the bisphenol-a reaction liquid measure with hot acetone flushing arrangement filler; Wherein fresh acetone respectively accounts for 50% with recovery acetone consumption), the air speed of acetone is 90 m
3/ h, the volume regeneration temperature is 50 ℃, the device filler after the regeneration can return to original processing power.
Claims (3)
1. method that removes residual catalyst in the bisphenol-a reaction liquid; It is characterized in that: earlier with bisphenol-a reaction liquid or with the depickling auxiliary agent mixed solution of bisphenol-a reaction liquid and 1-2%; Being conveyed into mixing tank (2) through reaction solution input tube (1) mixes; De-acidying agent is a kind of of water or methyl alcohol, perhaps is the mixed solution of water and methyl alcohol; Secondly the mixed solution in the mixing tank (2) is conveyed into adsorber A (3) and adsorber B (4); Adsorber A (3) and adsorber B (4) are the shell and tube device; Filling fiber film coalescence material (12) in the tubulation; The outer shell of tubulation feeds 80-90 ℃ hot water; The bisphenol-a reaction flow is after adsorber (3,4) adsorption treatment; Its acidity≤0.001mmol/L meets processing requirements, and bisphenol-a reaction liquid is defeated outside reaction solution output tube (6) is direct; When the acidity of after treatment bisphenol-a reaction liquid＞0.001mmol/L; Adsorber (3; 4) adsorption stuffing in needs treated regeneration; Acetone solvent in the solvent tank (7) is delivered to adsorber (3 with pump (8); 4) washing the fibre film coalescence mould material (12); Clean with recycling in the acetone solvent input solvent tank (7) later; Or through interchanger (10) input distillation tower (9) distillation; Acetone soln after the recovery is stored in Recycling in the solvent tank (7) through interchanger (10); Distillation back resultant product is main with an acidic catalyst water, does further processing by waste liquid output tube (11) output; The hot water of using 80-90 ℃ is at last dried tunica fibrosa coalescence material (12) in the interior tubulation of adsorber (3,4) through hot water input tube (5) input adsorber (3,4) shell, and the solvent acetone that steams is stored in and supplies in the solvent tank (7) to recycle.
2. the method that removes residual catalyst in the bisphenol-a reaction liquid according to claim 1 is characterized in that: the volume space velocity of adsorber (3,4) is 25-35m
3/ h, temperature 55-75 ℃, normal pressure.
3. the method that removes residual catalyst in the bisphenol-a reaction liquid according to claim 1 is characterized in that: the regenerated solvent of filler is to use acetone soln in the adsorber (3,4), and the acetone consumption is that bed is handled the long-pending 1/3-2/3 of bisphenol-a reaction liquid; The volume ratio of fresh acetone and acetone recycle is 1: 1 or 3: 7; Regeneration temperature is 45-55 ℃, and the regenerated volume space velocity is 80-90m
3/ h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101842925A CN102304026B (en) | 2011-07-04 | 2011-07-04 | Method for removing residual catalyst in bisphenol A reaction liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101842925A CN102304026B (en) | 2011-07-04 | 2011-07-04 | Method for removing residual catalyst in bisphenol A reaction liquid |
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| Publication Number | Publication Date |
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| CN102304026A true CN102304026A (en) | 2012-01-04 |
| CN102304026B CN102304026B (en) | 2013-06-19 |
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| CN2011101842925A Expired - Fee Related CN102304026B (en) | 2011-07-04 | 2011-07-04 | Method for removing residual catalyst in bisphenol A reaction liquid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20210188750A1 (en) * | 2018-09-05 | 2021-06-24 | Badger Licensing Llc | Process for producing bisphenol-a |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1457334A (en) * | 2001-03-05 | 2003-11-19 | 出光石油化学株式会社 | Process for producing bisphenol A |
| JP3903644B2 (en) * | 1999-05-20 | 2007-04-11 | 三菱化学株式会社 | Method for producing bisphenol A |
| JP3981334B2 (en) * | 2002-09-04 | 2007-09-26 | 出光興産株式会社 | Method for producing bisphenol A |
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2011
- 2011-07-04 CN CN2011101842925A patent/CN102304026B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3903644B2 (en) * | 1999-05-20 | 2007-04-11 | 三菱化学株式会社 | Method for producing bisphenol A |
| CN1457334A (en) * | 2001-03-05 | 2003-11-19 | 出光石油化学株式会社 | Process for producing bisphenol A |
| JP3981334B2 (en) * | 2002-09-04 | 2007-09-26 | 出光興産株式会社 | Method for producing bisphenol A |
Non-Patent Citations (1)
| Title |
|---|
| 范洪明: "酸吸收工艺在离子法双酚A生产中的运用", 《热固性树脂》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20210188750A1 (en) * | 2018-09-05 | 2021-06-24 | Badger Licensing Llc | Process for producing bisphenol-a |
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| CN102304026B (en) | 2013-06-19 |
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Application publication date: 20120104 Assignee: CHENGDU CAIXING TECHNOLOGIES CO., LTD. Assignor: Southwest Petroleum University Contract record no.: 2014510000085 Denomination of invention: Method for removing residual catalyst in bisphenol A reaction liquid Granted publication date: 20130619 License type: Exclusive License Record date: 20140722 |
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