CN102229535A - Method for orderly rectifying and separating nitromethane-nitroethane-nitropropane by continuous three towers - Google Patents
Method for orderly rectifying and separating nitromethane-nitroethane-nitropropane by continuous three towers Download PDFInfo
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Abstract
The invention relates to a method for orderly rectifying and separating nitromethane-nitroethane-nitropropane by continuous three towers, the raw material (an mixed solution of nitromethane, nitroethane,2-nitropropane and 1-nitropropane) is separated through a first continuous rectifying tower at first(B1), the content of the separated nitromethane on the top of the tower can reach over 99.5%, a distillate from the bottom is separated through the second continuous rectifying tower (B2), the content of the separated 1-nitropropane at the bottom of the tower can reach over 99.5%, the once through yields are respectively reach to 89.7% and 91.2%; a distillate from top of a second continuous rectifying tower (B2) is entered into a third continuous rectifying tower (B3) for separating nitroethane and 2-nitropropane, the content of nitroethane can reach above 82.0%, the content of 2-nitropropane can reach above 87.0%. Compared with the multi-times distillation method in the prior art, the separated product content and yield rate of the method provided in the invention are higher than that of the multi-times distillation method.
Description
Technical field
The present invention relates to a kind of chemical separating technology, particularly relate to the method for a kind of continuous three towers order rectifying separation Nitromethane 99Min.-nitroethane-nitropropane.
Background technology
The low-carbon (LC) nitroparaffins are important solvent and intermediates, and Nitromethane 99Min. is mainly as solvent and gasoline dope; Nitroethane is used for organic synthesis, is used as the solvent of soluble cotton and other resins, wax, fat, dyestuff etc.; Nitropropane comprises 1-nitropropane and 2-nitropropane, and the 2-nitropropane also is used for organic synthesis as the additive of the special solvent of ethene and epoxypaint, rocket fuel, gasoline etc.; The 1-nitropropane mainly is used as solvent and intermediate, jet fuel, sprays etc., (1) as solvent, to alcohol, ketone, ether, ester, and dyestuff, grease, wax, resin, synthetic rubber all have very strong solvency power, with alcohol and with being the powerful solvent of acetate fiber; With alcohol, awns hydrocarbon and with replacing chlorinated hydrocarbons dissolution with solvents tri acetic acid fiber.As low-temperature solvent can the dissolved chlorine ethane-acetic acid ethyenyl multipolymer, also can be used for dissolving cellulose nitrate, (2) be the intermediate of Chemicals such as amine, azanol class, nitro oxy-compound, chlorination nitroparaffins, the hydrolysis in the presence of sulfuric acid as nitropropane and methane can get oxammonium sulfate and propionic acid; In medicine industry, be used to produce antitubercular agent ethylamine hydrochloride butyl ester.
The production method of Nitromethane 99Min. mainly contains vaporphase nitration method and nitrite substitution method; Nitroethane has low-carbon alkanes, monochloroethane and ethyl sulfate nitrofication process; The 1-nitropropane adopts propane and propylene nitrofication process; The 2-nitropropane is used nitric acid direct oxidation method and nitrogen oxide nitrofication process more.Nitromethane 99Min. only has the production equipment of half industrially scalable at home, and production method to be adopting the nitrite substitution method, and product price is difference to some extent with the difference of quality, and major part is used for outlet; Nitroethane is used for synthetic pesticide at home in a large number, the present domestic small-scale production of having only, and the content of product reaches 99%, because its production difficulty is bigger, dangerous higher, a part of manufacturer stops production successively, do not form scale production at home, basic dependence on import; And similar to nitroethane, nitropropane is not high owing to technology more complicated, the market requirement, the present domestic large-scale production that do not form substantially.
At present, the nitroparaffins mixture separation generally adopts repeatedly distillation method to obtain single cut, because boiling-point difference is little between the low-carbon (LC) nitroparaffins component, constitutive property is shown in Table 1, adopt distillation method to separate, not only complicated operating process, difficulty are controlled, product purity is low, and middle runnings simultaneously is too much, and yield can only reach 53%.
The character of table 1 low-carbon (LC) nitroparaffins
Summary of the invention
Above-mentioned deficiency at prior art, the invention provides the method for a kind of continuous three towers order rectifying separation Nitromethane 99Min.-nitroethane-nitropropane, to solve the difficulty that exists on the low-carbon (LC) nitroparaffins mixture separation, Nitromethane 99Min. and 1-nitropropane content after the inventive method is separated reach more than 99.5%, one time yield reaches 89.7% and 91.2% respectively, and 2-nitropropane and nitroethane content reach respectively more than 66% and 82%.
The technical scheme of finishing the foregoing invention task is: adopt continuous three towers order rectifying separation technology, according to forming the boiling point difference in size, carry out Nitromethane 99Min.-nitroethane-nitropropane and separate, step is as follows:
(1), at first adopt the 1st continuous rectifying tower (B1) to separate Nitromethane 99Min., nitroethane, 2-nitropropane and 1-nitropropane mixing solutions, the control rectifying tower temperature when that refluxes, overhead distillate is a Nitromethane 99Min., and Nitromethane 99Min. content can reach more than 99.5% in the overhead distillate; Distillate is nitroethane, 2-nitropropane and 1-nitropropane mixed solution at the bottom of the tower;
(2), distillate is delivered to the 2nd continuous rectifying tower (B2) separation at the bottom of the 1st continuous rectifying tower (B1) tower, the control rectifying tower temperature when that refluxes, distillate obtains the 1-nitropropane more than 99.5% at the bottom of the tower, and overhead distillate is nitroethane, 2-nitropropane and a small amount of 1-nitropropane mixed solution;
(3), the 2nd continuous rectifying tower (B2) overhead distillate delivers to the 3rd continuous rectifying tower (B3), the reflux ratio and the temperature of control control rectifying tower, overhead distillate obtains the nitroethane more than 82.0%, distillate is the 2-nitropropane more than 87.0% at the bottom of the tower.
In the mixed solution of described raw material Nitromethane 99Min., nitroethane, 2-nitropropane and 1-nitropropane, the quality percentage composition of Nitromethane 99Min., nitroethane, 2-nitropropane and 1-nitropropane is respectively 5.0～15.0%, 10.0～20.0%, 35.0～45.0% and 30.0～40.0%.
In the described step (1), the 1st continuous rectifying tower (B1) top, low temperature are respectively 100.9 ~ 101.3 ℃ and 120.9 ~ 121.7 ℃, and reflux ratio (R1) is controlled at 9 ~ 11.
In the described step (2), the 2nd continuous rectifying tower (B2) top, low temperature are respectively 117.1 ~ 118.0 ℃ and 130.0 ~ 131.1 ℃, and reflux ratio (R2) is controlled at 8 ~ 10.
In the described step (3), the 3rd continuous rectifying tower (B3) top, low temperature are respectively 110.5 ~ 111.4 ℃ and 120.1 ~ 121.0 ℃, and reflux ratio (R3) is controlled at 11 ~ 12.
The technical process of continuous three towers order distillation and separation method of the present invention sepn process is seen shown in Figure 1, and separating apparatus adopts optimizes processing condition, separates back Nitromethane 99Min. and 1-nitropropane content and all reaches more than 99.5%, can reach the requirement of use.
Advantage of the present invention: adopt technology shown in Figure 1 and optimized parameters, raw material (Nitromethane 99Min., nitroethane, 2-nitropropane and 1-nitropropane mixing solutions) at first separates through the 1st continuous rectifying tower (B1), obtain content after the separation and can reach 99.6% above Nitromethane 99Min., distillate separates through the 1st continuous rectifying tower (B2) at the bottom of the tower, obtain content at the bottom of the B2 tower and reach 1-nitropropane more than 99.7%, the once through yield of Nitromethane 99Min. and 1-nitropropane reaches 89.7% and 91.2% respectively.Compare with repeatedly distillating method used in the prior art, content and yield all are higher than repeatedly distillation method, and in distillation method sepn process repeatedly, Nitromethane 99Min. and 1-nitropropane content all are lower than 99.1%, and yield is lower than 53.0%.
Description of drawings
The process flow sheet of the continuous three towers order of Fig. 1 rectifying separation Nitromethane 99Min.-nitroethane-nitropropane.
Embodiment
Describe the present invention below in conjunction with embodiment, described embodiment helps the understanding of the present invention and enforcement, be not to be construed as limiting the invention, implement the present invention, the related material and distillation operation condition, those skilled in the art can also be equal to or equivalent transformation it according to different separation purposes in specific embodiment.Protection scope of the present invention is not exceeded with embodiment, but is limited by claim.Except as otherwise noted, the per-cent among the present invention is mass percent.
The method of continuous three towers order rectifying separation Nitromethane 99Min.-nitroethane-nitropropane, with reference to parameter shown in technology shown in Figure 1 and the table 2, raw material (1) is the mixed solution of Nitromethane 99Min., nitroethane, 2-nitropropane and 1-nitropropane, wherein the quality percentage composition (X of Nitromethane 99Min., nitroethane, 2-nitropropane and 1-nitropropane
F1, X
F2, X
F3, X
F4) being respectively 10.0%, 15.0%, 40.0%, 35.0%, flow is 100Kg/h.
Raw material (1) at first enters the 1st continuous rectifying tower B1 with the 100.0Kg/h flow and separates Nitromethane 99Min., nitroethane, 2-nitropropane and 1-nitropropane mixing solutions, the 1st continuous rectifying tower B1 stage number is 50, when cat head, low temperature are respectively 100.9 ~ 101.3 ℃ and 120.9 ~ 121.7 ℃, top, low flow are respectively 9.0Kg/h, 91.0Kg/h, trim the top of column is controlled at 9 ~ 11 than R1, and cat head, end distillate quality are formed (x
Di, x
Wi) x
D1=0.9967, x
D2=0.0032, x
D3=0.0001, x
D4=0.0000 and x
W1=0.0220, x
W2=0.1667, x
W3=0.4347, x
W4The=0.3766, the 1st continuous rectifying tower B1 overhead distillate (2) reaches 99.67% Nitromethane 99Min. for content.
Distillate (3) enters the 2nd continuous rectifying tower B2 separation at the bottom of the 1st continuous rectifying tower B1 tower, the 2nd continuous rectifying tower B2 stage number is 40, when cat head, low temperature are respectively 117.1 ~ 118.0 ℃ and 130.0 ~ 131.1 ℃, top, low flow are respectively 60.0Kg/h, 32.0Kg/h, trim the top of column is controlled at 8 ~ 10 than R2, and distillate (5) reaches 99.76% 1-nitropropane at the bottom of the 2nd continuous rectifying tower B2 tower for content.
The 2nd continuous rectifying tower B2 overhead distillate (4) enters the 3rd continuous rectifying tower B3 to be separated, the 3rd continuous rectifying tower B3 stage number is 50, when cat head, low temperature are respectively 110.5 ~ 111.4 ℃ and 120.1 ~ 121.0 ℃, top, low flow are respectively 16.5Kg/h, 43.5Kg/h, trim the top of column is controlled at 11 ~ 12 than R3, the 3rd continuous rectifying tower B3 overhead distillate (6) is the nitroethane of content 82.35%, and distillate at the bottom of the tower (7) is the 2-nitropropane of content 87.30%.
The processing condition of each continuous rectifying tower and separating resulting see Table 2 and table 3 respectively in the described method.
Table 2 technological parameter
In table 3 sepn process stream strand material flow and composition (%)
Claims (6)
1. the method for continuous three towers order rectifying separation Nitromethane 99Min.-nitroethane-nitropropane, Nitromethane 99Min. and 1-nitropropane quality percentage composition after this method is separated reach more than 99.5%, it is characterized in that described method comprises the steps:
(1), at first adopt the 1st continuous rectifying tower (B1) to separate Nitromethane 99Min., nitroethane, 2-nitropropane and 1-nitropropane mixing solutions, the control rectifying tower temperature when that refluxes, overhead distillate is a Nitromethane 99Min., and Nitromethane 99Min. content reaches more than 99.5% in the overhead distillate; Distillate is nitroethane, 2-nitropropane and 1-nitropropane mixed solution at the bottom of the tower;
(2), distillate is delivered to the 2nd continuous rectifying tower (B2) separation at the bottom of the 1st continuous rectifying tower (B1) tower, the control rectifying tower temperature when that refluxes, distillate obtains the 1-nitropropane more than 99.5% at the bottom of the tower, and overhead distillate is nitroethane, 2-nitropropane and 1-nitropropane mixed solution;
(3), the 2nd continuous rectifying tower (B2) overhead distillate delivers to the 3rd continuous rectifying tower (B3), the reflux ratio and the temperature of control control rectifying tower, overhead distillate obtains the nitroethane more than 82.0%, distillate is the 2-nitropropane more than 87.0% at the bottom of the tower.
2. the method for continuous three towers order rectifying separation Nitromethane 99Min.-nitroethane according to claim 1-nitropropane, it is characterized in that in the mixed solution of described Nitromethane 99Min., nitroethane, 2-nitropropane and 1-nitropropane, the quality percentage composition of Nitromethane 99Min., nitroethane, 2-nitropropane and 1-nitropropane is respectively 5.0～15.0%, 10.0～20.0%, 35.0～45.0% and 30.0～40.0%.
3. the method for continuous three towers order rectifying separation Nitromethane 99Min.-nitroethane according to claim 1 and 2-nitropropane, it is characterized in that in the described step (1), the 1st continuous rectifying tower (B1) top, low temperature are respectively 100.9 ~ 101.3 ℃ and 120.9 ~ 121.7 ℃, and reflux ratio R1 is controlled at 9 ~ 11.
4. the method for continuous three towers order rectifying separation Nitromethane 99Min.-nitroethane according to claim 1 and 2-nitropropane, it is characterized in that in the described step (2), the 2nd continuous rectifying tower (B2) top, low temperature are respectively 117.1 ~ 118.0 ℃ and 130.0 ~ 131.1 ℃, and reflux ratio R2 is controlled at 8 ~ 10.
5. the method for continuous three towers order rectifying separation Nitromethane 99Min.-nitroethane according to claim 1 and 2-nitropropane, it is characterized in that in the described step (3), the 3rd continuous rectifying tower (B3) top, low temperature are respectively 110.5 ~ 111.4 ℃ and 120.1 ~ 121.0 ℃, and reflux ratio R3 is controlled at 11 ~ 12.
6. the method for continuous three towers order rectifying separation Nitromethane 99Min.-nitroethane according to claim 1-nitropropane is characterized in that the concrete operations step is:
(1) raw material (1) Nitromethane 99Min., nitroethane, the mixed solution of 2-nitropropane and 1-nitropropane, Nitromethane 99Min. wherein, nitroethane, the quality percentage composition of 2-nitropropane and 1-nitropropane is respectively 10.0%, 15.0%, 40.0%, 35.0%, flow is 100Kg/h, entering stage number and be 50 the 1st continuous rectifying tower B1 separates, the 1st continuous rectifying tower (B1) top, when low temperature is respectively 100.9 ~ 101.3 ℃ and 120.9 ~ 121.7 ℃, the top, low flow is respectively 9.0Kg/h, 91.0Kg/h, trim the top of column is controlled at 9 ~ 11 than R1, and overhead distillate (2) reaches 99.67% Nitromethane 99Min. for content;
To enter stage number be that 40 the 2nd continuous rectifying tower B2 separates to distillate (3) at the bottom of (2) the 1st continuous rectifying tower B1 towers, when the 2nd continuous rectifying tower B2 cat head, low temperature are respectively 117.1 ~ 118.0 ℃ and 130.0 ~ 131.1 ℃, top, low flow are respectively 60.0Kg/h, 32.0Kg/h, trim the top of column is controlled at 8 ~ 10 than R2, and distillate (5) reaches 99.76% 1-nitropropane at the bottom of the 2nd continuous rectifying tower B2 tower for content;
It is that 50 the 3rd continuous rectifying tower B3 separates that (3) the 2nd continuous rectifying tower B2 overhead distillates (4) enter stage number, when the 3rd continuous rectifying tower B3 cat head, low temperature are respectively 110.5 ~ 111.4 ℃ and 120.1 ~ 121.0 ℃, top, low flow are respectively 16.5Kg/h, 43.5Kg/h, trim the top of column is controlled at 11 ~ 12 than R3, the 3rd continuous rectifying tower B3 overhead distillate (6) is the nitroethane of content 82.35%, and distillate at the bottom of the tower (7) is the 2-nitropropane of content 87.30%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102617627A (en) * | 2012-02-23 | 2012-08-01 | 淄博市临淄齐泉工贸有限公司 | Device and method for continuously separating silicon tetrachloride, propyl trichlorosilane and 3-chloropropyltrichlorosilane |
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| US20110092749A1 (en) * | 2009-10-20 | 2011-04-21 | Dow Global Technologies Inc. | Process For Downstream Recovery Of Nitroalkane Using Dividing Wall Column |
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2011
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3869253A (en) * | 1972-10-19 | 1975-03-04 | Azote & Prod Chim | Apparatus for producing nitroparaffins |
| US20110092749A1 (en) * | 2009-10-20 | 2011-04-21 | Dow Global Technologies Inc. | Process For Downstream Recovery Of Nitroalkane Using Dividing Wall Column |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102617627A (en) * | 2012-02-23 | 2012-08-01 | 淄博市临淄齐泉工贸有限公司 | Device and method for continuously separating silicon tetrachloride, propyl trichlorosilane and 3-chloropropyltrichlorosilane |
| CN102617627B (en) * | 2012-02-23 | 2015-02-18 | 淄博市临淄齐泉工贸有限公司 | Method for continuously separating silicon tetrachloride, propyl trichlorosilane and 3-chloropropyltrichlorosilane |
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Application publication date: 20111102 |