CN1066648A - Purifying bisphenol a solvent by chemical extraction - Google Patents
Purifying bisphenol a solvent by chemical extraction Download PDFInfo
- Publication number
- CN1066648A CN1066648A CN 91103117 CN91103117A CN1066648A CN 1066648 A CN1066648 A CN 1066648A CN 91103117 CN91103117 CN 91103117 CN 91103117 A CN91103117 A CN 91103117A CN 1066648 A CN1066648 A CN 1066648A
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- Prior art keywords
- toluene
- bisphenol
- solvent
- aqueous solution
- extraction
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Abstract
The present invention is the solvent that synthesis of bisphenol A is used, and carries out Chemical Pretreatment, from bisphenol A solvent impurity is extracted then, reaches the purpose of solvent purification and energy reuse.Present method and original distillation method purifying bisphenol-A solvent phase ratio can reduce the bisphenol A solvent loss significantly.The 700 kilograms of bisphenol A solvent toluene of purifying, the toluene loss is less than 10 kilograms in the treating processes.Present method technology is simple, and processing cost is low.
Description
The present invention is the organic solvent with extracting process purification synthesis of bisphenol A.
Prior art is a distillation method.The solvent that China's synthesis of bisphenol A is used is a toluene.With the distillatory method toluene is steamed, reach the phenol that to remain in the toluene, dihydroxyphenyl propane, the various phenols of by product and sulfonic acid class, the isolating purpose of catalyzer Thiovanic acid.
I have consulted the patent of invention of China, find the Gazette of Patent for Invention of 8, first phases in 91 on May always, in CO7C, the 7/10(extraction process), 7/08(distillation extraction method), 15/06(toluene), 39/04(phenol), the 39/06(dihydroxyphenyl propane) in, all less than and the similar patent of the present invention, say nothing of the same (applying for, examine, authorize me all to look into).
In addition, I in the CA of the U.S., at benzene, methyl-(toluene) in,
Preparation (preparation)
Extn. (extraction)
Purifn. (purification)
Recovery (recovery)
Properties (character)
extn.
purifn.
Uses and miscellaneous (using and other)
extn.
Solvent (solvent)
purifn.
In these columns, consult relevant documents and materials and patent in detail, do not seen the report that a piece and the present invention have similarity.
In addition, at propane ,-2.2-bis(4-hydroxyphenyl) also consulted more corresponding columns in (dihydroxyphenyl propane) column, also find no report with similarity of the present invention.
With distillation method purification synthesis of bisphenol A solvent toluene, when condensator outlet was cooled to 30 ℃, nearly 5% toluene was run away in tail gas.Along with constantly steaming of toluene, the concentration that remains in the various phenols of main solute in the toluene improves gradually, and bubble point also raises gradually, and total some toluene can not steam in the vinasse (based on various phenols).The data that chemical industry four factories in Baoding provide are: bisphenol A solvent toluene of every distillation, 700 kilograms of toluene will lose 80 kilograms.And the distillation method energy consumption is also bigger, so can be without the distillating method of physics with the method purifying bisphenol-A solvent toluene of chemical extraction, and can reach the purpose that the toluene waste is few, save the energy? the present invention is based on above idea and designs, conceives.
Synthesis of bisphenol A solvent for use toluene, after the solvent toluene cooling, dihydroxyphenyl propane separates out, toluene is except that the dihydroxyphenyl propane that also is dissolved with part, also be dissolved with the raw material phenol of a certain amount of synthesis of bisphenol A, and by product creosote class, also remaining have a spot of by-product phenol sulfonic acid, toluenesulphonic acids and a catalyzer Thiovanic acid.
No matter be phenols, sulfonic acid class, carboxylic-acid all energy and NaOH reaction generation sodium salt.Phenol sodium, sodium sulfonate, carboxylic acid sodium are all soluble in water again and be insoluble to organic solvent toluene.We can water the sodium salt that forms, from toluene, extract.
Toluene is " insoluble " in water, and benzene is " slightly soluble " [1] in water, and in water, the solubleness of toluene is littler than benzene.Benzene is in the time of 22 ℃, and the solubleness in water is in per hundred parts of water of 0.07%() [2].Because of the dissolution data of toluene in water do not found, so calculate the volume that solvent toluene is 700 kilograms in the solubleness of water with benzene temporarily:
(700kg)/(0.866kg/l) ＝808.3l
In actual extraction, the NaOH aqueous solution: toluene=1: the 5(volume ratio), so, extraction 808.3l toluene, the volume of the NaOH aqueous solution is:
(808.3l)/5=161.7l(supposes that wherein the weight of water is 161.7kg)
In the time of 18 ℃, the solution loss of benzene in 161.7kg water:
161.7kg×0.07%＝0.113kg
The solution loss of toluene in water in the time of 22 ℃, is less than 0.113kg, also can not surpass 0.2kg in the time of 30 ℃.
The boiling point of toluene is 110.8 ℃
[3], be the 40mmHg post 31.8 ℃ partial vapor pressures
[4]Extraction is at 3m
3Airtight carrying out in the reactor put into 800 liters of toluene, 800 liters of NaOH aqueous solution, also surplus above 1.4m
3The space, the concentration of toluene in the air above the benzene is calculated by following formula
G＝ (16·M·P)/(273+t) （g/m
3）[5]
In the formula: the M-molecular weight of material
The vapour pressure (mmHg post) of P-material when temperature t.
G＝ (16×92×40)/(273+31.8) ＝193g/m
3
193g/m
3×1.4m
3＝270g
Promptly when 32 ℃ (room temperature in summer) extracted, the volatilization loss of toluene was 270 grams, and when 32 ℃ of extraction 700kg toluene, in operating process, the total losses amount of toluene is
0.3kg+0.2kg＝0.5kg
(evaporation) (dissolving)
In sum, every extraction 700kg toluene, the loss of toluene should be less than 10 kilograms (factor of assurance of 20 times) in operating process, compares with distillation method, lose 60～70 kilograms of toluene (2.5 yuan of per kilogram toluene) less.Handle toluene and compare with distillation method processing toluene with the present invention, one ton of Resins, epoxy of every production can be saved 120～140 kilograms of toluene.The turnout of annual domestic Resins, epoxy is 20,000～40,000 tons now, and Yueyang chemical general factory has newly been gone up the ten thousand tons of equipment of producing per year again, and 10,000 tons of equipment are also prepared to produce per year by Shenyang Resin Factory.In producing Resins, epoxy, if having in 10,000 tons of Resins, epoxy productions, the whole nation handles solvent toluene with the present invention, can save 1200 tons～1400 tons of toluene every year, be worth 300～3,500,000 yuan.Promptly saved resource, reduced environmental pollution again, technology of the present invention is simple, and processing cost and distillation method purifying methylbenzene are similar.
Optimum implementation
1, after dihydroxyphenyl propane is separated out in the toluene cooling, with alkali-metal hydroxide aqueous solution extraction.
2, in 1, alkali-metal hydroxide aqueous solution is the NaOH aqueous solution.
3, in 2, the concentration expressed in percentage by weight of the NaOH aqueous solution is 10～15%.
When 4, extracting, 10-15%(weight) NaOH aqueous solution volume: volume of toluene=1: 1.
5, in 4, the NaOH aqueous solution extraction with volume toluene after, extract another for the second time part with volume toluene with it again; Reextraction is crossed the NaOH aqueous solution of toluene, removes to extract the toluene of another part with volume more for the third time, extracts the toluene of another part with volume the 4th time with this NaOH aqueous solution again; Extract the toluene of another part the 5th time with this NaOH aqueous solution again with volume.The 4th time, the 5th time stripped toluene, the available new NaOH aqueous solution carry out the extraction second time, to remove the yellow of toluene.Carry out the NaOH aqueous solution of extraction for the second time, still can be used for continuous five untreated toluene of extraction.
6, with above art breading bisphenol A solvent toluene, can reach following index:
1. remove sulfonic acid class, dihydroxyphenyl propane, creosote class, Thiovanic acid and most of phenol in the toluene.
2. extraction back toluene color and luster: colourless or band is yellow slightly.
3. toluene can reuse.
4. per 700 kilograms of toluene, the toluene loss is less than 10 kilograms in the treating processes.
5. handle 700 kilograms of toluene, with 80 kilograms of 30%NaOH liquid caustic soda.
7, extracted the cresylol sodium water solution 5 times, water was boiled off, with the form recovery phenol of phenol sodium.
8, sodium phenolate is joined in the dihydroxyphenyl propane building-up process and to wash in the water for the first time, wash water for the first time and contain about phenol 10000ppm sulfur acid 30-40%(weight).
Sulfocarbolic acid, mercaptoethyl and Na
2SO
4Be dissolved in water, phenol, dihydroxyphenyl propane and other creosote are then separated out from water.Like this, can utilize the waste water of dihydroxyphenyl propane in synthetic, reclaim phenols.
Reference
[1]??CRC??Handbook??of??Chemistry??and??Physics??58th??edition??C-518，C-416。
[2]??Handbook??of??Chemistry??third??edition??219PP。
[3]??CnpaboiHllk??Xuuuka，mau??Bmepoǔ，765Cmp.
[4]??CRC.Handbook??of??Chemistry??and??Physics58th??edition??D-198。
[5] " the industry absorption of gas and steam " [Soviet Union] E.H. Xie Erpinuowa, 35 pages.
Claims (5)
- The invention belongs to after chemical reaction, with the method for purification by liquid extraction synthesis of bisphenol A organic solvent.Common extraction is to extract from the aqueous solution with organic solvent, complex compound as extracting metals, and the present invention is just in time opposite, be to use water as extraction agent, the water-soluble salt that solute reaction back generates in the extraction organic solvent, the method of present domestic purification synthesis of bisphenol A organic solvent toluene is all taked distillation method.1, technical characterictic of the present invention is: be the alkali metal hydroxide aqueous solution extraction, and the method for purification synthesis of bisphenol A solvent.
- 2,1 part of 10～15%(weight) the NaOH aqueous solution extracts isopyknic bisphenol A solvent toluene technology continuous five to ten times.
- 3, utilize in the dihydroxyphenyl propane production process and contain phenol, wash phenol that waste water and the present invention extract the acidiferous first time and receive reaction, reclaim phenols.
- 4, the alkali metal hydroxide aqueous solution in the claim I is the NaOH aqueous solution; The synthesis of bisphenol A solvent is a toluene.
- 5, the NaOH aqueous solution concentration expressed in percentage by weight in the claim 4 is 10～15%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91103117 CN1066648A (en) | 1991-05-16 | 1991-05-16 | Purifying bisphenol a solvent by chemical extraction |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91103117 CN1066648A (en) | 1991-05-16 | 1991-05-16 | Purifying bisphenol a solvent by chemical extraction |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1066648A true CN1066648A (en) | 1992-12-02 |
Family
ID=4905905
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 91103117 Pending CN1066648A (en) | 1991-05-16 | 1991-05-16 | Purifying bisphenol a solvent by chemical extraction |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1066648A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0796834A3 (en) * | 1996-03-21 | 1998-04-01 | Bayer Ag | Purification of p,p-bisphenolate solutions |
| CN102718732A (en) * | 2012-06-27 | 2012-10-10 | 四川东材科技集团股份有限公司 | Method for purifying bisphenol A diglycidyl ether |
| CN108611189A (en) * | 2016-12-09 | 2018-10-02 | 丰益(上海)生物技术研发中心有限公司 | The refinery practice of bisphenol-A and alkyl phenol in a kind of control grease |
| CN109324004A (en) * | 2018-10-06 | 2019-02-12 | 聊城鲁西聚碳酸酯有限公司 | The method of content of bisphenol A is remained in a kind of measurement polycarbonate |
-
1991
- 1991-05-16 CN CN 91103117 patent/CN1066648A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0796834A3 (en) * | 1996-03-21 | 1998-04-01 | Bayer Ag | Purification of p,p-bisphenolate solutions |
| CN1073071C (en) * | 1996-03-21 | 2001-10-17 | 拜尔公司 | Purification of P,P-biphenolate solutions |
| CN102718732A (en) * | 2012-06-27 | 2012-10-10 | 四川东材科技集团股份有限公司 | Method for purifying bisphenol A diglycidyl ether |
| CN102718732B (en) * | 2012-06-27 | 2014-07-16 | 四川东材科技集团股份有限公司 | Method for purifying bisphenol A diglycidyl ether |
| CN108611189A (en) * | 2016-12-09 | 2018-10-02 | 丰益(上海)生物技术研发中心有限公司 | The refinery practice of bisphenol-A and alkyl phenol in a kind of control grease |
| CN108611189B (en) * | 2016-12-09 | 2023-02-21 | 丰益(上海)生物技术研发中心有限公司 | Refining process for controlling bisphenol A and alkylphenol in grease |
| CN109324004A (en) * | 2018-10-06 | 2019-02-12 | 聊城鲁西聚碳酸酯有限公司 | The method of content of bisphenol A is remained in a kind of measurement polycarbonate |
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