CN103483148A - Dehydration recovery method of non-acid oxygen-containing organic substances in Fischer-Tropsch synthesis water - Google Patents
Dehydration recovery method of non-acid oxygen-containing organic substances in Fischer-Tropsch synthesis water Download PDFInfo
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- 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
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- C07C45/81—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
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- 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
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Abstract
The invention discloses a dehydration recovery method of non-acid oxygen-containing organic substances in Fischer-Tropsch synthesis water. The method comprises the following steps: carrying out extractive distillation on non-acid oxygen-containing organic substances to obtain a light mixed alcohol product at the tower top and obtain a water solution containing heavy mixed alcohols and extractant at the tower bottom, wherein the non-acid oxygen-containing organic substances are oxygen-containing organic substances obtained by deacidifying and rectifying Fischer-Tropsch synthesis water; (2) rectifying the water solution containing heavy mixed alcohols and extractant to obtain a water solution containing heavy mixed alcohols at the tower top and obtain reclaimed extractant at the tower bottom; and (3) carrying out non-homogeneous phase stratification on the water solution containing heavy mixed alcohols to obtain an organic phase solution on the upper layer and obtain a water phase solution on the lower layer; and (4) rectifying the organic phase solution to obtain the heavy mixed alcohol product at the tower bottom. The mixed alcohol product is obtained through a plurality of rectifying operating units; and the product has the advantages of high purity and higher heat value, can be used as a fuel, and can also be subjected to deep processing to obtain different oxygen-containing compounds, thereby greatly increasing the product varieties of the solid fuel liquefying oil producer.
Description
Technical field
The present invention relates to the dewatering and recovery method of the non-sour oxygen-bearing organic matter in a kind of Fischer-Tropsch synthetic water.
Background technology
Fischer-Tropsch is synthetic be the synthetic gas (carbon monoxide and hydrogen) that will derive from Sweet natural gas, coal etc. by catalyzer be converted into chain length from C1 to C100 more than the reaction process of positive structure hydrocarbon (alkane and alpha-olefin), a small amount of isomeric hydrocarbon and low carbon number oxygen-bearing organic matter (acid, alcohol, aldehyde, ketone and ester) and water, and this reaction process is accompanied by strong heat release.
The detailed quantitative relation formula of Fischer-Tropsch synthesis can be expressed as:
Alkane nCO+ (2n+1) H
2=C
nh
2n+2+ nH
2o (1-1)
Alkene nCO+2nH
2=C
nh
2n+ nH
2o (1-2)
Acid nCO+ (2n-2) H
2=C
nh
2no
2+ (n-2) H
2o (1-3)
Alcohol nCO+2nH
2=C
nh
2n+2o+ (n-1) H
2o (1-4)
Aldehyde nCO+ (2n-1) H
2=C
nh
2no+ (n-1) H
2o (1-5)
Ketone nCO+ (2n-1) H
2=C
nh
2no+ (n-1) H
2o (1-6)
Ester nCO+ (2n-2) H
2=C
nh
2no
2+ (n-2) H
2o (1-7)
Water-gas shift (WGS) reaction:
CO+H
2O=CO
2+H
2 (1-8)。
From above-mentioned quantitative relation formula, in the Fischer-Tropsch synthesis process, water generates by approaching equimolar reaction of carbon monoxide.In the iron-base fischer-tropsch synthetic reaction process, the output of water is generally more than a times of synthetic oil output.
The product that Fischer-Tropsch synthesis generates can separate hydro carbons and aqueous phase by-product after initial gross separation.The initial gross separation process comprises by the cooling flash distillation from fischer-tropsch reactor, thereby gas-phase product out carries out gas-liquid separation and obtains liquid phase fluid, thereby then this liquid phase fluid is passed into to water-and-oil separator and obtain the water fluid that contains trace suspension and dissolved hydrocarbon and a small amount of oxygen-bearing organic matter at water, thereby this water fluid is passed into to the fluid that the synthetic water purolator obtains being rich in water, be the raw material that the present invention reclaims non-sour oxygen-bearing organic matter, be called in the present invention " Fischer-Tropsch synthetic water ".
The applicant adopts Fischer-Tropsch synthesis process technology and the Fischer-Tropsch synthetic iron-based catalyst technology of Zhongke Synthetic Oil Technology Co., Ltd., built respectively 160,000 tons of ICL for Indirect Coal Liquefaction synthetic oil demonstration plants of two cover annual outputs in the safe coal liquefaction company of Inner Mongol gouy and Shanxi the Lushui River peace coal liquefaction company, and the successfully operation in 2009.According to the data of demonstration plant, in the above-mentioned Fischer-Tropsch synthetic water gone out through initial gross separation, still contain micro-C
5-C
20hydrocarbon, its content is generally lower than 100ppm, specifically lower than 20ppm.Contain oxygen-bearing organic matter, its carbon number is less than 8 substantially simultaneously, and content is generally less than 10wt%.In this Fischer-Tropsch synthetic water, the content of hydrocarbon and oxygen-bearing organic matter is relevant with type, fischer-tropsch reaction condition (composition of air inlet and flow, temperature, pressure etc.) and the initial gross separation technique of fischer-tropsch catalysts.Usually, the oxygen-bearing organic matter in described Fischer-Tropsch synthetic water is mainly light alcohol, for example methyl alcohol and ethanol, and content is about 0.1wt%-5wt%.Heavy alcohol (such as propyl alcohol, butanols, amylalcohol, hexanol, enanthol, 2-butanols, 2-amylalcohol, 3-methyl-1-butanol, 2-hexanol etc.), aldehyde (such as acetaldehyde, propionic aldehyde, butyraldehyde etc.), ketone (such as acetone, pentanone, hexanone etc.), ester (such as methyl acetate, ethyl acetate, butyrolactone etc.) also exist with relative lower content with acid (such as acetic acid, propionic acid, butyric acid, valeric acid, caproic acid, isopropylformic acid etc.), and concentration is about 2.5wt%.
In addition, in the Fischer-Tropsch synthetic water, also have tens kinds of oxygen-bearing organic matters to exist with extremely low concentration, their content is usually less than 50ppm.Because content is extremely low, the technogenic influence that these oxygen-bearing organic matters are processed the Fischer-Tropsch synthetic water is less, does not generally do quantitatively.
Due to the existence of hydrocarbon and oxygen-bearing organic matter, above-mentioned Fischer-Tropsch synthetic water can not directly discharge, otherwise can cause environmental pollution; Above-mentioned Fischer-Tropsch synthetic water can not directly utilize, because the existence of oxygen-bearing organic matter makes the Fischer-Tropsch synthetic water far not reach discharge or the standard of cyclically utilizing, and wherein containedly such as acidic species such as carboxylic acids, can cause corrosion to equipment.Synthetic some technological process (as circulating cooling, gasification Quench, gasified coal water slurry preparation, water-gas shift etc.) of industry Fischer-Tropsch needs to consume a large amount of water, therefore the Fischer-Tropsch synthetic water should effectively reuse after rational treatment process purifying, the recycle of water in the Fischer-Tropsch building-up process can be realized on the one hand, the oxygen-bearing organic matter that added value is very high can be reclaimed as much as possible on the other hand.Therefore the Fischer-Tropsch synthetic water is carried out to purification process and just seem particularly necessary.
Chinese patent ZL 200810032926.3, ZL 200810032927.8, ZL 200810043252.7 and ZL 200810043253.1 disclose the separation and recovery method of oxygen-bearing organic matter in the Fischer-Tropsch synthetic water, main art route is: first adopt the method for conventional distillation to remove a small amount of boiling point and be less than the heavy component that the light constituent of 40 ℃ and boiling point are greater than 120 ℃, a large amount of cuts of side line extraction (50 ℃～120 ℃) enter the separation tower again; According to the component characteristics, adopt afterwards the methods such as azeotropic distillation, extracting rectifying to be separated successively all the other components.Whole technical process is comparatively simple, to oxygen-bearing organic matter, also can realize initial gross separation.But the separated portion related in patent is only acetone, methyl alcohol, ethanol, n-propyl alcohol and acetic acid, and in actual Fischer-Tropsch synthetic water, the composition of oxygen-bearing organic matter wants complicated a lot.Therefore these patents be not suitable for real Fischer-Tropsch synthetic water treating processes.
Chinese patent ZL 200810034600.4, ZL 200810034601.9 and ZL 201010512405.5 disclose the Separation & Purification method of the single oxygen-bearing organic matter that content is higher.The unit process related in patent comprises: conventional distillation, azeotropic distillation, extracting rectifying, batch fractionating, stripping, extraction, drying and distilling, hydrogenation reaction etc., the existing sepn process process that responds again, technical process complexity.Because the oxygen-bearing organic matter kind in actual Fischer-Tropsch synthesized water phase is numerous, its content unavoidably has fluctuation in process of production, and the stability that the technique of introducing in these patents forms raw material, process integrated has very high requirement, therefore be difficult to realize that industry amplifies.
Summary of the invention
The dewatering and recovery method that the purpose of this invention is to provide the non-sour oxygen-bearing organic matter in a kind of Fischer-Tropsch synthetic water.
The dewatering and recovery method of the non-sour oxygen-bearing organic matter in a kind of Fischer-Tropsch synthetic water provided by the present invention, comprise the steps:
(1) non-sour oxygen-bearing organic matter is inputed in extractive distillation column and carries out extracting rectifying, obtain gently mixing pure product in described extracting rectifying column overhead, obtain the aqueous solution with extraction agent containing heavily mixed alcohol at the bottom of tower;
Described non-sour oxygen-bearing organic matter is the oxygen-bearing organic matter that the Fischer-Tropsch synthetic water obtains after depickling and rectifying;
(2) the described aqueous solution containing heavily mixed alcohol and extraction agent is inputed in the extraction agent recovery tower and carries out rectifying, obtain, containing the heavily mixed pure aqueous solution, obtaining the extraction agent of reuse at the bottom of tower at described extraction agent recovery tower tower top;
(3) input in quantizer and carry out heterogeneous layering containing the heavily mixed pure aqueous solution described, on described quantizer upper strata, obtain organic phase solution, lower floor obtains aqueous phase solution;
(4) described organic phase solution is delivered in heavily mixed pure knockout tower and carries out rectifying, at the bottom of described heavy mixed pure knockout tower tower, obtain heavily mixing pure product.
In above-mentioned dewatering and recovery method, in step (1), described non-sour oxygen-bearing organic matter can be pure organic compound, aldehyde organic compound, ketone organic compound or the ester organic compound of C1～C8;
Described pure organic compound is light alcohol or heavy alcohol, and described light alcohol can be methyl alcohol and ethanol, and described heavy alcohol can be propyl alcohol, butanols, amylalcohol, hexanol, enanthol, 2-butanols, 2-amylalcohol, 3-methyl-1-butanol or 2-hexanol;
Described aldehyde organic compound can be acetaldehyde, propionic aldehyde or butyraldehyde;
Described ketone organic compound can be acetone, pentanone or hexanone;
Described ester organic compound can be methyl acetate, ethyl acetate or butyrolactone.
In above-mentioned dewatering and recovery method, in step (1), the temperature of described extracting rectifying column overhead can be 40～70 ℃, and the temperature at the bottom of tower can be 70～200 ℃, and reflux ratio can be 0.1～8:1;
Described extracting rectifying extraction agent used can be polar organic solvent, ionic liquid and/or solid salt;
Described polar organic solvent can be in ethylene glycol and glycerol any;
Described ionic liquid can be in 1,3-methylimidazole acetate, 1-ethyl-3-methylimidazole acetate and 1-butyl-3-methyl imidazolium tetrafluoroborate any;
Described solid salt can be CaCl
2, in NaCl, KCl, NaAc and KAc any.
In above-mentioned dewatering and recovery method, in step (1), in described extracting rectifying, the add-on of extraction agent can be 0.1～10 times of quality of described non-sour oxygen-bearing organic matter.
In above-mentioned dewatering and recovery method, in step (2), described rectifying can be atmospheric distillation, compression rectification or rectification under vacuum.
In above-mentioned dewatering and recovery method, in step (2), the temperature of described extraction agent recovery tower tower top can be 80～100 ℃, and the temperature at the bottom of tower can be 100～220 ℃, and reflux ratio can be 1～10:1.
In above-mentioned dewatering and recovery method, in step (2), the extraction agent of described reuse inputs to recycle in described extractive distillation column.
In above-mentioned dewatering and recovery method, in step (3), in described organic phase solution, the quality percentage composition of water can be 1%～30%;
In described aqueous phase solution, the quality percentage composition of water can be 70%～99%.
In above-mentioned dewatering and recovery method, in step (4), the temperature of described heavy mixed pure knockout tower tower top can be 70～100 ℃, and the temperature at the bottom of tower can be 80～200 ℃, and reflux ratio can be 1～10:1.
In above-mentioned dewatering and recovery method, in step (4), at described heavy mixed pure knockout tower tower top, obtain the solution containing heavily mixed alcohol and water, the described solution containing heavily mixed alcohol and water enters in described quantizer and carries out heterogeneous layering.
In method of the present invention, resulting light mixed pure product has higher calorific value, can be used as fuel, with the Fischer-Tropsch oil product is mixed, converts; Resulting heavy mixed pure product can further be isolated single component (as propyl carbinol) and sell as industrial goods.
In method of the present invention, resulting waste water (aqueous phase solution) can loop back in pure acid separation column, further extracts non-sour oxygenatedchemicals wherein, or reaches the standard of industrial circulating water after other are processed.
The dewatering and recovery method of non-sour organic oxygen-containing compound in Fischer-Tropsch synthesized water phase provided by the invention, adopt a plurality of distillation operations unit, obtained mixed pure product, and the purity of described product is high, higher calorific value is arranged, can serve as fuel, also further deep processing is processed, obtain different oxygenatedchemicalss, greatly increased the range of product of solid fuel liquefaction liquefaction device.Meanwhile, method of the present invention provides a kind of method of economical and practical processing Fischer-Tropsch synthesized water phase product for relevant enterprise, the method can obviously improve synthetic oil factory Technical Economy, increase the Fischer-Tropsch synthetic kind, solve the problem that Fischer-Tropsch synthesis oil factory water processes, the target that realizes cleaner production, can meet the scale requirement that the water of synthetic oil Industrial demonstration factory and megaton synthetic oil business factory is processed.
The accompanying drawing explanation
The dewatering and recovery process flow sheet that Fig. 1 is non-sour oxygen-bearing organic matter in Fischer-Tropsch synthetic water of the present invention.
Wherein the meaning of Reference numeral is as follows:
The 6 non-sour oxygen-bearing organic matter aqueous solution, 7 supplementary extraction agents, 8 extractive distillation columns, 9 light mixed pure products, 10 mixing solutionss containing extraction agent and heavy alcohol, 11 extraction agent recovery towers, 12 are containing heavily mixing the heavily mixed pure knockout tower of the pure aqueous solution, 13 logistics 12 and the mixed solution of logistics 19,14 quantizers, 15 aqueous phase solutions, 16 organic phase solutions, 17 cycling extraction agent, 18,19 containing the heavily mixed pure product of the heavily mixed pure aqueous solution, 20.
Embodiment
The experimental technique used in following embodiment if no special instructions, is ordinary method.
In following embodiment, material used, reagent etc., if no special instructions, all can obtain from commercial channels.
Embodiment 1,
Press the flow process shown in Fig. 1, raw material is the non-sour oxygen-bearing organic matter aqueous solution 6 of 12600kg/h, extraction agent is selected ethylene glycol, adopt rectifying tower to carry out lock out operation to this raw water, by the operational condition (reflux ratio, feed plate position and overhead extraction rate) of control tower and the consumption of extraction agent, obtain mixed pure product.Idiographic flow:
(1) non-sour oxygen-bearing organic matter solution 6 is inputed in extractive distillation column 8 and carries out extracting rectifying, obtain gently mixing pure product 9 at extractive distillation column 8 tower tops, obtain the mixing solutions 10 containing extraction agent and heavy alcohol at the bottom of tower;
(2) will input to containing the mixing solutions 10 of extraction agent and heavy alcohol in extraction agent recovery tower 11 and carry out rectifying, and obtain, containing the heavily mixed pure aqueous solution 12, obtaining the extraction agent 17 of reuse at the bottom of tower at extraction agent recovery tower 11 tower tops;
(3) will input in quantizer 14 and carry out heterogeneous layering containing the heavily mixed pure aqueous solution 12, and on quantizer 14 upper stratas, obtain organic phase solution 16, lower floor obtains aqueous phase solution 15;
(4) organic phase solution 16 is delivered in heavily mixed pure knockout tower 18 and carries out rectifying, at the bottom of heavily mixed pure knockout tower tower, obtain heavily mixing pure product 20.
In above-mentioned treating processes, from the organic phase solution that the upper strata of quantizer obtains, the quality percentage composition of water is 10.8%, and in the aqueous phase solution obtained in lower floor, the quality percentage composition of water is 88.6%.
The non-sour oxygen-bearing organic matter aqueous solution of table 1 forms
The operational condition of each tower of table 2
Claims (9)
1. the dewatering and recovery method of the non-sour oxygen-bearing organic matter in a Fischer-Tropsch synthetic water, comprise the steps:
(1) non-sour oxygen-bearing organic matter is inputed in extractive distillation column and carries out extracting rectifying, obtain gently mixing pure product in described extracting rectifying column overhead, obtain the aqueous solution with extraction agent containing heavily mixed alcohol at the bottom of tower;
Described non-sour oxygen-bearing organic matter is the oxygen-bearing organic matter that the Fischer-Tropsch synthetic water obtains after depickling and rectifying;
(2) the described aqueous solution containing heavily mixed alcohol and extraction agent is inputed in the extraction agent recovery tower and carries out rectifying, obtain, containing the heavily mixed pure aqueous solution, obtaining the extraction agent of reuse at the bottom of tower at described extraction agent recovery tower tower top;
(3) input in quantizer and carry out heterogeneous layering containing the heavily mixed pure aqueous solution described, on described quantizer upper strata, obtain organic phase solution, lower floor obtains aqueous phase solution;
(4) described organic phase solution is delivered in heavily mixed pure knockout tower and carries out rectifying, at the bottom of described heavy mixed pure knockout tower tower, obtain heavily mixing pure product.
2. dewatering and recovery method according to claim 1 is characterized in that: in step (1), and pure organic compound, aldehyde organic compound, ketone organic compound or ester organic compound that described non-sour oxygen-bearing organic matter is C1～C8;
Described pure organic compound is light alcohol or heavy alcohol, and described light alcohol is methyl alcohol and ethanol, and described heavy alcohol is propyl alcohol, butanols, amylalcohol, hexanol, enanthol, 2-butanols, 2-amylalcohol, 3-methyl-1-butanol or 2-hexanol;
Described aldehyde organic compound is acetaldehyde, propionic aldehyde or butyraldehyde;
Described ketone organic compound is acetone, pentanone or hexanone;
Described ester organic compound is methyl acetate, ethyl acetate or butyrolactone.
3. dewatering and recovery method according to claim 1 and 2, it is characterized in that: in step (1), the temperature of described extracting rectifying column overhead is 40～70 ℃, and the temperature at the bottom of tower is 70～200 ℃, and reflux ratio is 0.1～8:1;
Described extracting rectifying extraction agent used is polar organic solvent, ionic liquid and/or solid salt;
Described polar organic solvent be in ethylene glycol and glycerol any;
Described ionic liquid be in 1,3-methylimidazole acetate, 1-ethyl-3-methylimidazole acetate and 1-butyl-3-methyl imidazolium tetrafluoroborate any;
Described solid salt is CaCl
2, in NaCl, KCl, NaAc and KAc any.
4. according to the described dewatering and recovery method of any one in claim 1-3, it is characterized in that: in step (1), 0.1～10 times of the quality that in described extracting rectifying, the add-on of extraction agent is described non-sour oxygen-bearing organic matter.
5. according to the described dewatering and recovery method of any one in claim 1-4, it is characterized in that: in step (2), the temperature of described extraction agent recovery tower tower top is 80～100 ℃, and the temperature at the bottom of tower is 100～220 ℃, and reflux ratio is 1～10:1.
6. according to the described dewatering and recovery method of any one in claim 1-5, it is characterized in that: in step (2), the extraction agent of described reuse inputs to recycle in described extractive distillation column.
7. according to the described dewatering and recovery method of any one in claim 1-6, it is characterized in that: in step (3), in described organic phase solution, the quality percentage composition of water is 1%～30%;
In described aqueous phase solution, the quality percentage composition of water is 70%～99%.
8. according to the described dewatering and recovery method of any one in claim 1-7, it is characterized in that: in step (4), the temperature of described heavy mixed pure knockout tower tower top is 70～100 ℃, and the temperature at the bottom of tower is 80～200 ℃, and reflux ratio is 1～10:1.
9. according to the described dewatering and recovery method of any one in claim 1-8, it is characterized in that: in step (4), obtain the solution containing heavily mixed alcohol and water at described heavy mixed pure knockout tower tower top, the described solution containing heavily mixed alcohol and water enters in described quantizer and carries out heterogeneous layering.
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