CN1298693C - Production of high purity ritalin from waste liquid or gas containing it - Google Patents
Production of high purity ritalin from waste liquid or gas containing it Download PDFInfo
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- CN1298693C CN1298693C CN 200510002905 CN200510002905A CN1298693C CN 1298693 C CN1298693 C CN 1298693C CN 200510002905 CN200510002905 CN 200510002905 CN 200510002905 A CN200510002905 A CN 200510002905A CN 1298693 C CN1298693 C CN 1298693C
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- 239000007788 liquid Substances 0.000 title claims abstract description 36
- 239000002699 waste material Substances 0.000 title claims abstract description 36
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- JUMYIBMBTDDLNG-OJERSXHUSA-N hydron;methyl (2r)-2-phenyl-2-[(2r)-piperidin-2-yl]acetate;chloride Chemical compound Cl.C([C@@H]1[C@H](C(=O)OC)C=2C=CC=CC=2)CCCN1 JUMYIBMBTDDLNG-OJERSXHUSA-N 0.000 title claims description 89
- 229940099204 ritalin Drugs 0.000 title claims description 89
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 189
- 238000000034 method Methods 0.000 claims abstract description 48
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000003795 desorption Methods 0.000 claims abstract description 32
- 230000008929 regeneration Effects 0.000 claims abstract description 28
- 238000011069 regeneration method Methods 0.000 claims abstract description 28
- 238000004821 distillation Methods 0.000 claims abstract description 15
- 238000010533 azeotropic distillation Methods 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims description 49
- 239000000463 material Substances 0.000 claims description 38
- 238000001179 sorption measurement Methods 0.000 claims description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 239000002808 molecular sieve Substances 0.000 claims description 17
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 17
- 230000000274 adsorptive effect Effects 0.000 claims description 15
- 239000002904 solvent Substances 0.000 claims description 7
- 241000282326 Felis catus Species 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 239000011148 porous material Substances 0.000 claims description 6
- 238000004088 simulation Methods 0.000 claims description 6
- 238000005194 fractionation Methods 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000006227 byproduct Substances 0.000 claims description 4
- 238000010926 purge Methods 0.000 claims description 4
- -1 Dichlorodiphenyl Acetate methyl esters Chemical class 0.000 claims description 3
- 229910021536 Zeolite Inorganic materials 0.000 claims description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 239000012046 mixed solvent Substances 0.000 claims description 3
- 238000011017 operating method Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 238000010992 reflux Methods 0.000 claims description 3
- 239000010457 zeolite Substances 0.000 claims description 3
- 239000003651 drinking water Substances 0.000 claims description 2
- 235000020188 drinking water Nutrition 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- 230000001172 regenerating effect Effects 0.000 claims description 2
- 230000009466 transformation Effects 0.000 claims description 2
- 239000002594 sorbent Substances 0.000 claims 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 abstract description 8
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 abstract description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 abstract description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 abstract description 5
- 239000011368 organic material Substances 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- 230000007547 defect Effects 0.000 abstract 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 18
- 238000009833 condensation Methods 0.000 description 5
- 230000005494 condensation Effects 0.000 description 5
- 229920006395 saturated elastomer Polymers 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 3
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 230000032050 esterification Effects 0.000 description 2
- 238000005886 esterification reaction Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000006315 carbonylation Effects 0.000 description 1
- 238000005810 carbonylation reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000010808 liquid waste Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The present invention belongs to a method for preparing high purity methyl acetate from waste liquid or gas containing the methyl acetate in the technical field of organic material preparation. The present invention is characterized in that the waste liquid (gas) containing a great quantity of methyl acetate in the industrial process of producing polyvinyl alcohol, terephthalic acid, etc. is processed through azeotropic distillation, adsorbing distillation, condensing back flow and desorption regeneration, and thus, the high purity methyl acetate can be conveniently obtained from the waste liquid (gas) containing the methyl acetate with high efficiency; besides, methyl alcohol which easily react with the methyl acetate to form azeotrope is independently obtained. The present invention overcomes the defect that the highly purify methyl acetate is difficult to prepare from the waste liquid (gas) by using an ordinary rectification method.
Description
Technical field
The invention belongs to organic materials preparation technique scope, particularly a kind ofly from the waste liquid that contains ritalin or gas, produce the method for preparing the high-purity acetic acid methyl esters.
Background technology
In the production process of polyvinyl alcohol industry and terephthalic acid industry, all produce the waste liquid (gas) that contains ritalin in a large number.Owing to also contain methyl alcohol, water etc. easily form azeotrope with ritalin material in these waste liquids (gas), directly make highly purified ritalin by waste liquid (gas) with common rectificating method is very difficult.And contain the ritalin unstable properties of a large amount of methyl alcohol, water, limited it in industrial application.The pure liquid waste solution (gas) that produces in the polyvinyl alcohol Industrial processes, producer mainly passes through in recovery process its hydrolysis to be generated acetic acid and methyl alcohol at present, and reuse or sale aborning after being purified respectively.The energy consumption of this process is very big, and is also high to the requirement of equipment, and the acetic acid of generation is compared on price with methyl alcohol with the acetic acid of carbonylation method production with methyl alcohol and lacked competitiveness.And on the other hand, the high-purity acetic acid methyl esters of being badly in need of on the market is again to produce by the complicated technologies such as esterification extracting rectifying of methyl alcohol and acetic acid.Just as much as to say, present a part of manufacturer produces acetic acid and methyl alcohol with the methyl acetate hydrolysis of low concentration, and there is the waste of the huge energy and material therebetween in another part manufacturer with acetic acid and the methyl alcohol ritalin of the synthetic high density of esterification again.
In addition, also a considerable amount of ritalins of by-product in the Production of Terephthalic Acid process.This part ritalin is equally owing to purity is difficult to use inadequately.Other may produce the production process that contains ritalin waste liquid (gas) and no longer describe in detail.
Produce waste liquid (gas) for this class, a main difficult problem just is that material such as the methyl alcohol, water in ritalin and the waste liquid (gas) all can form azeotrope, and is very difficult with its separation with common rectificating method; And, be difficult to obtain at present high-purity ritalin again if adopt membrane separation technique.At the characteristics that contain ritalin waste liquid (gas), the present invention can will produce ritalin and the separating substances such as methyl alcohol, water in the waste liquid (gas) cheap, easily, when producing the high-purity acetic acid methyl esters, obtains other organic solvents in a large number, as methyl alcohol etc.
Summary of the invention
The purpose of this invention is to provide a kind of method of from the waste liquid that contains ritalin or gas, producing the high-purity acetic acid methyl esters, it is characterized in that, this method is the mode by adsorptive distillation and desorption and regeneration, from the waste liquid that contains ritalin or gas, make the high-purity acetic acid methyl esters, obtain byproduct methyl alcohol and other solvents simultaneously;
Its high-purity acetic acid methyl esters Production Flow Chart is:
1) azeotropic distillation, the production waste liquid or the gas that will contain ritalin are admitted to the ritalin azeotropy rectification column, producing temperature is 20-200 ℃, pressure is the steam that contains ritalin/methyl alcohol or ritalin/methanol of 0.1-10atm, cat head part steam small part condensing reflux, most of is 60-100 ℃ from the cat head extraction with the temperature, and pressure is that the azeotropic steam of 1-2atm is sent to the adsorptive distillation device;
2) fractionation by adsorption, the adsorptive distillation device is a fixed bed or simulation moving-bed, the azeotropic steam that will contain ritalin by adsorptive distillation device bottom not cause that sorbing material fluidizing superficial gas velocity is that 0.001m/s-100m/s sends into adsorber, gas is from bottom to top by being equipped with the adsorption bed of sorbing material, ritalin is not adsorbed by this bed, and methyl alcohol, water or other impurity are then constantly adsorbed by unsaturated bed in by the process of bed; Adjust the length of adsorption bed, be as the criterion by the ritalin of production different purity requirement; Or long adsorption bed should solve to adopt multistage series connection and simulation moving-bed operating method, and superficial gas velocity is 0.5m/s-10m/s;
3) regeneration of desorption and sorbing material, be trapped within little acetic acid methyl esters on the sorbing material, a large amount of first alcohol and waters or other solvents with known desorption mode desorption, mixed solvent under the desorption mixes as its charging with the fresh feed of azeotropic rectification working process, warm inert gas purge was clean during sorbing material behind the desorption was used, just finished the regeneration of sorbing material, to drop into the use of next round;
4) methanol rectifying tower, the discharging of azeotropic distillation operation are the thick methyl alcohol that does not contain ritalin, separate obtaining refined methanol in methanol rectifying system with known rectificating method.
The sorbing material that is adopted is that Dichlorodiphenyl Acetate methyl esters, methyl alcohol or glassware for drinking water have the porous material of selecting adsorptivity, and described sorbing material is zeolite, molecular sieve or gac, the porous material of its aperture between 3 -13 ; The sorbing material that is adopted is the molecular sieve of 4 , 5 .
The described temperature of sending into the ritalin of adsorptive distillation device is 60-70 ℃, and pressure is 1atm.
The superficial gas velocity of described azeotropic steam is 0.5m/s-10m/s.
The method that adopts desorption and regeneration progressively is with the methyl alcohol in the abundant acquisition raw material; The used solvent of regenerating is a water, adopts the mode desorb of alternating temperature and/or transformation.
It is 1-10atm that the water vapor pressure of described usefulness requires, and it is 250-450 ℃ that the alternating temperature desorb requires used drying-air temperature, and it is 1-759mmHg that pressure-swing desorption requires used vacuum tightness.
The invention has the beneficial effects as follows the mode of the present invention by adsorptive distillation and desorption and regeneration, the sufficiently long bed absorption of process, condensation of gas just can conveniently make the high-purity acetic acid methyl esters of high value efficiently from the waste liquid that contains ritalin (gas) of low value, obtain methyl alcohol easy and ritalin formation azeotrope simultaneously separately.
Description of drawings
Fig. 1 is a high-purity acetic acid methyl esters reparation technology schematic flow sheet.
Embodiment
The invention provides a kind of method of from the waste liquid that contains ritalin or gas, producing the high-purity acetic acid methyl esters.This method is the mode by adsorptive distillation and desorption and regeneration, makes the high-purity acetic acid methyl esters from the waste liquid (gas) that contains ritalin, obtains byproduct methyl alcohol and other solvents simultaneously.
High-purity acetic acid methyl esters Production Flow Chart (as shown in Figure 1) is:
1. azeotropic distillation: the production waste liquid (gas) that will contain ritalin is admitted to ritalin azeotropy rectification column 1, producing temperature is 20-200 ℃, pressure is the steam that contains ritalin/methyl alcohol or ritalin/methanol of 0.1-10atm, cat head part steam small part condensing reflux, major part is extracted out from cat head; With the temperature is 60-100 ℃, and pressure is the adsorptive distillation device 3 that the azeotropic steam of 1-2atm directly is sent to the fractionation by adsorption operation.Optimum temps is 60-70 ℃, and pressure is 1atm.If there are other can produce ritalin azeotropic steam unit or the ready-made steam source that contains ritalin, this azeotropy rectification column 1 generally also can omit.
2. fractionation by adsorption: the adsorber of adsorptive distillation device 3 is a fixed bed or simulation moving-bed; The azeotropic steam that will contain ritalin by the adsorber bottom not cause that sorbing material fluidizing superficial gas velocity is that 0.001m/s-100m/s sends into adsorber, gas is from bottom to top by being equipped with the adsorption bed of sorbing material, ritalin is not adsorbed by this bed, and methyl alcohol, water or other impurity are then constantly adsorbed by unsaturated bed in by the process of bed; Adjust the length of adsorption bed, be as the criterion by the ritalin of production different purity requirement; Or long adsorption bed should solve (shown in Fig. 1 right-hand part frame of broken lines) to adopt multistage series connection and simulation moving-bed operating method; Best superficial gas velocity is 0.5m/s-10m/s.
3. the regeneration of desorption and sorbing material: be trapped within little acetic acid methyl esters on the sorbing material, a large amount of first alcohol and waters or other solvents with known desorption mode desorption, mixed solvent under the desorption mixes as its charging with the fresh feed of azeotropic rectification working process, warm inert gas purge was clean during sorbing material behind the desorption was used, just finished the regeneration of sorbing material, to drop into the use of next round.
4. methanol rectifying tower: the discharging of azeotropic distillation operation is the thick methyl alcohol that does not contain ritalin, separates obtaining refined methanol in methanol rectifying system 2 with known rectificating method.
The sorbing material that is adopted is that Dichlorodiphenyl Acetate methyl esters and methyl alcohol (or water) have the porous material of selecting adsorptivity, and described sorbing material is the porous material of aperture between 3 -13 : zeolite, molecular sieve or gac.More specifically, the optimal adsorption material that is adopted is 4 , 5 molecular sieves.
Because the adsorption process of first alcohol and water is accompanied by strong exothermic phenomenon, when ritalin passes through the sorbing material bed, bed temperature will sharply rise.The present invention directly utilizes this part heat of adsorption to keep bed to be in comparatively high temps, thereby reduces the adsorptive capacity of ritalin, and the maintenance ritalin can condensation in the process process of bed.Begin before logical ritalin adsorbs, sorbing material all passes through desorb and regeneration, and the temperature that keeps beginning to adsorb is more concrete at 20-200 ℃, and keeping the initial adsorption temperature of adsorption bed is 60-70 ℃.
Utilize the strong heat release of adsorption process, the control of adsorber is temperature sensing control with the switching employing.Utilization is installed in the temperature sensing controller on adsorption bed top, controls the switching between the input and output material of adsorber automatically, and begins material in the saturated adsorber is carried out desorb and regeneration.Concrete, the design temperature of temperature sensing controller is 70-150 ℃.Specifically under above-mentioned special conditions of contract, promptly adopt 60 ℃ of ritalin steam, the charging of 1atm pressure, sorbing material is 5 molecular sieves, 65 ℃ of regeneration back bed initial adsorption temperature, the design temperature of temperature sensing controller is 107 ℃.
The desorb of saturated bed can be adopted following method with regeneration, as rare gas element (N
2, CO
2) purge pressure-swing desorption, water vapor desorption, the combination of method such as alternating temperature desorb and these methods.Combination regeneration by above-mentioned arbitrary method or method sorbing material completely all can be used for the production of high-purity acetic acid methyl esters once more.Concrete, the desorb that contains the saturated bed of methyl alcohol can be adopted first water vapor desorption with regeneration, and the mode of alternating temperature or pressure-swing desorption is with abundant recovery methyl alcohol again; To not containing the extremely low saturated bed of methyl alcohol and ritalin content, also can consider direct alternating temperature or pressure-swing desorption and regeneration sorbing material.More concrete, water vapour desorb methyl alcohol can adopt the water vapor 4 of pressure 1-10atm, is fed by adsorber top, and is top-down by saturated adsorption bed, methyl alcohol is desorbed the formation mixing steam discharge adsorber, be sent to azeotropy rectification column 2 again and serve as direct heat source.Treat that methyl alcohol is fully desorbed, stop logical steam, the dry air of using 250-450 ℃ instead passes through adsorption bed from top to bottom, or adopts 1-759mmHg vacuum tightness to come dry regeneration sorbing material, and the adjustment sorbing material returns to the initial adsorption temperature.Water vapour desorb methyl alcohol also is a strong exothermic process, and the controlled temperature of temperature sensing controller that can be by being set in the adsorption bed bottom determines when and stops to feed water vapor and switch to alternating temperature desorb (or pressure-swing desorption).Concrete, the displays temperature that is arranged on the temperature sensor of adsorption bed bottom rises to the highest and is the best moment that stops water flowing steam when beginning to descend.
If no special instructions, above-mentioned ritalin then refers in particular to the steam that contains ritalin, and the concentration of the ritalin of being mentioned all is mass percent concentration.
Following for embodiment be the laboratory scale result of experiment, but it is conspicuous, the embodiment that it adopted is claims of the present invention and specification sheets open request and the concrete method of introducing, and be equally applicable to production, the especially large-scale industrial production of high-purity acetic acid methyl esters of various other high-purity acetic acid methyl esters of unit scale level.
Example 1: get the fully also good 5 molecular sieve 273.12g that preserve of 400 ℃ of regeneration and fill in the glass column, with mass percent concentration 99.4% 144.7g ritalin steam with the superficial gas velocity of 1.5m/s from bottom to top by behind the adsorber bed, collect the high-purity acetic acid methyl esters that 135.53g contains any impurity hardly with spherical condenser, molecular sieve adsorption 4.45g ritalin and methyl alcohol, other has 4.72g high-purity acetic acid methyl esters and condensation and the mistake of escaping.The molecular sieve that present embodiment uses is directly used in example 2 after 400 ℃ of regeneration.
Example 2: with mass percent concentration be 217.21g ritalin/methanol solution of 74% all vaporize the back with the superficial gas velocity of 4.4m/s from bottom to top by behind the adsorber bed, collecting mass percent concentration with spherical condenser is that 97% ritalin solution 58.33g, mass percent concentration are 77.9% ritalin solution 127.65g, 5 molecular sieve adsorption 24.74g ritalin and methyl alcohol, other has 6.29g ritalin and condensation and the mistake of escaping.The molecular sieve that present embodiment uses is directly used in example 3 after 400 ℃ of regeneration.
Example 3: with mass percent concentration be 129.82g ritalin/methanol solution of 76% all vaporize the back with the superficial gas velocity of 4m/s from bottom to top by behind the adsorber bed, collecting high-purity acetic acid methyl esters, mass percent concentration that 52.69g contains any impurity hardly with spherical condenser is that 95.2% ritalin methanol solution 28.59g and mass percent concentration are 92.2% ritalin methanol solution 23.38g, molecular sieve adsorption 21.26g ritalin and methyl alcohol, other has 3.9g ritalin and condensation and the mistake of escaping.Wait that the temperature sensor that is arranged at adsorption bed top shows that bed temperature reaches 107 ℃, then stop logical ritalin steam, use instead 100 ℃ water vapor with the superficial gas velocity of 1m/s by behind the bed, collect with spherical condenser that to contain mass percent concentration be that 10% ritalin, mass percent concentration are that 83% methyl alcohol and mass percent concentration are the solution 17.58g of 7% water.The 5 molecular sieves that present embodiment uses are directly used in example 4 after 400 ℃ of regeneration.
Example 4: will contain mass percent concentration and be 46.9% ritalin, mass percent concentration is that 6.2% methyl alcohol and mass percent concentration are that the solution 318.31g of 46.7% water sends into and produces azeotropic steam in the azeotropy rectification column, control this azeotropic steam with the superficial gas velocity of 5.3m/s from bottom to top by behind the adsorber bed, collecting mass percent concentration successively with spherical condenser is 99.9% ritalin solution 119.18g, mass percent concentration is ritalin/methanol solution 39.41g of 75% and to contain mass percent concentration be 5% ritalin, mass percent concentration is that 73% methyl alcohol and mass percent concentration are the solution 6.85g of 22% water, and mass percent concentration is 5% methanol/water solution 22.9g, residual still liquid 106.32g in the last azeotropy rectification column still almost all is a water.The molecular sieve that present embodiment uses is directly used in example 5 after 400 ℃ of regeneration.
Example 5: will contain mass percent concentration and be 77.84% ritalin, mass percent concentration is that 22% methyl alcohol and mass percent concentration are that the solution 96.77g of 0.16% acetaldehyde sends into azeotropy rectification column and all produces azeotropic steam, control this azeotropic steam with the superficial gas velocity of 3.8m/s from bottom to top by behind the adsorber bed, collect the high-purity acetic acid methyl esters that 65.8g contains any impurity hardly successively with spherical condenser; Absorption is finished, and feeds water vapor desorb under normal pressure of 100 ℃, and collecting 28.23g with spherical condenser, to contain mass percent concentration be 18% ritalin, and mass percent concentration is the solution of 50% methyl alcohol.The molecular sieve that present embodiment uses can recycle after 400 ℃ of regeneration once more.Component ratio in the raw material that present embodiment adopted is exactly the azeotropic composition that the industrial typical ritalin of polyvinyl alcohol is produced waste liquid.
Can be seen significantly by the foregoing description: the inventive method can make things convenient for and obtain the high-purity acetic acid methyl esters efficiently from the various ritalin waste liquids of forming (gas).More particularly, can make things convenient for and produce the waste liquid (gas) and obtain the high-purity acetic acid methyl esters from the ritalin that contains of industry such as polyvinyl alcohol, terephthalic acid efficiently.
Claims (8)
1. method of from the waste liquid that contains ritalin or gas, producing the high-purity acetic acid methyl esters, it is characterized in that: this method is the mode by adsorptive distillation and desorption and regeneration, from the waste liquid that contains ritalin or gas, make the high-purity acetic acid methyl esters, obtain byproduct methyl alcohol and other solvents simultaneously;
Its high-purity acetic acid methyl esters Production Flow Chart is:
1) azeotropic distillation: the production waste liquid or the gas that will contain ritalin are admitted to the ritalin azeotropy rectification column, producing temperature is 20-200 ℃, pressure is the steam that contains ritalin/methyl alcohol or ritalin/methanol of 0.1-10atm, cat head part steam small part condensing reflux, major part is extracted out from cat head, with the temperature is 60-100 ℃, and pressure is the adsorptive distillation device that the azeotropic steam of 1-2atm is sent to the fractionation by adsorption operation;
2) fractionation by adsorption: the adsorptive distillation device is a fixed bed or simulation moving-bed; The azeotropic steam that will contain ritalin by adsorptive distillation device bottom not cause that sorbing material fluidizing superficial gas velocity is that 0.001m/s-100m/s sends into adsorber, gas is from bottom to top by being equipped with the adsorption bed of sorbing material, ritalin is not adsorbed by this bed, and methyl alcohol, water or other impurity are then constantly adsorbed by unsaturated bed in by the process of bed; Adjust the length of adsorption bed, be as the criterion by the ritalin of production different purity requirement; Or long adsorption bed should solve to adopt multistage series connection and simulation moving-bed operating method; Superficial gas velocity is 0.5m/s-10m/s;
3) regeneration of desorption and sorbing material: be trapped within little acetic acid methyl esters on the sorbing material, a large amount of first alcohol and water with known desorption mode desorption, mixed solvent under the desorption mixes as charging with the fresh feed of azeotropic rectification working process, warm inert gas purge was clean during sorbing material behind the desorption was used, just finished the regeneration of sorbing material, to drop into the use of next round;
4) methanol rectifying tower: the discharging of azeotropic distillation operation is the thick methyl alcohol that does not contain ritalin, separates obtaining refined methanol in methanol rectifying system with known rectificating method.
2. according to the described method of producing the high-purity acetic acid methyl esters from the waste liquid that contains ritalin or gas of claim 1, it is characterized in that: the sorbing material that is adopted is that Dichlorodiphenyl Acetate methyl esters and methyl alcohol or glassware for drinking water have the porous material of selecting adsorptivity.
3. according to the described method of producing the high-purity acetic acid methyl esters from the waste liquid that contains ritalin or gas of claim 2, it is characterized in that: described porous material is zeolite, molecular sieve or the gac of aperture between 3 -13 .
4. according to the described method of producing the high-purity acetic acid methyl esters from the waste liquid that contains ritalin or gas of claim 3, it is characterized in that: described molecular sieve is 4 , 5 molecular sieves.
5. according to the described method of producing the high-purity acetic acid methyl esters from the waste liquid that contains ritalin or gas of claim 1, it is characterized in that: the described temperature of sending into the ritalin of adsorptive distillation device is 60-70 ℃, and pressure is 1atm.
6. according to the described method of producing the high-purity acetic acid methyl esters from the waste liquid that contains ritalin or gas of claim 1, it is characterized in that: the superficial gas velocity of described azeotropic steam is 0.5m/s-10m/s.
7. according to the described method of from the waste liquid that contains ritalin or gas, producing the high-purity acetic acid methyl esters of claim 1, it is characterized in that: the progressively method of desorption and regeneration that is regenerated as of described desorption and sorbing material, to comprise other organic solvents of methyl alcohol in the abundant acquisition raw material; The used solvent of regenerating is a water, adopts the mode desorb of alternating temperature and/or transformation.
8. according to claim 1 or the 5 described methods of from the waste liquid that contains ritalin or gas, producing the high-purity acetic acid methyl esters, it is characterized in that: the described sorbent material progressively used water vapor pressure of method of desorption and regeneration is 1-10atm, the used drying-air temperature of alternating temperature desorb is 250-450 ℃, and the used vacuum tightness of pressure-swing desorption is 1-759mmHg.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200510002905 CN1298693C (en) | 2005-01-26 | 2005-01-26 | Production of high purity ritalin from waste liquid or gas containing it |
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| CN 200510002905 CN1298693C (en) | 2005-01-26 | 2005-01-26 | Production of high purity ritalin from waste liquid or gas containing it |
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| CN103102265B (en) * | 2013-03-06 | 2015-03-04 | 福州大学 | Method and production equipment for variable-pressure distillation and purification of methyl acetate |
| CN104710306A (en) * | 2015-01-12 | 2015-06-17 | 吉林化工学院 | Method for preparing acetate through ester interchange-adsorption ethanol removal combined technology |
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|---|---|
| CN1680267A (en) | 2005-10-12 |
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