Method of producing sulfate or sulfite organic compounds and reactor for effecting same

专利摘要:
The reactor 1 has vertical tubes 10 connected at the top to two common chambers 15 and 17 feeding an organic liquid and an SO3- containing gas respectively. At the bottom the tubes enter a common collecting chamber 40. The gas is fed into the tubes 10 at a pressure of 0.1 to 0.5 bar, which is substantially the same as the head loss over the length of the tubes 10. The liquid is fed into each tube 10 at an overpressure equivalent to 1 to 100 cm of liquid column with respect to the gas feeding pressure. The tubes 10 are externally cooled by water supplied at 20 and withdrawn at 21. <IMAGE>
公开号:SU1246892A3
申请号:SU802886103
申请日:1980-02-20
公开日:1986-07-23
发明作者:Моретти Джованни；Ное Серджо
申请人:Баллестра Кимика С.П.А. (Фирма)；
IPC主号:

专利说明:

The invention relates to an improved method for the preparation of sulphirovanes: or sulphthironamine organic compounds, which are used in the production of surfactants, and to an improved device for its implementation,
The aim of the invention is to improve the quality of the target product by using an improved device and maintaining in it the pressure of the supplied liquid and gaseous products supplied determined by the south.
FIG. 1 shows a longitudinal section reactor; FIG. 2 is a section A — A of FIG. 1; in fig. 3 is a section bb pa of fig. one; FIG. 4 is a schematic cross-section of three reactor tubes in an irregular operating position; on fpg, 5 and 6 th; in other working positions.
The reactor comprises a housing 1, a bundle of vertical and parallel pipes 2. Arranged side by side and connected at the top to the feed chamber 3 for said gas of a similar reagent entering through conduit 4 from the gas generating unit 80, preferably by catalytic conversion.
The pipes 2 are connected downwards with a chamber 3 for collecting reaction products, which are removed through conduit 6. A cooling station (water) is circulating-heated inside the sh-shindrichesky case but outside the pipes 2. Since the exothermic reaction is carried out to melodies 14 and products subject to sulphonation or sulphation and a gaseous reagent, represented by a1; by itself sulfuric anhydride, mainly 13 of the first or top part of the pipes 2 occurs, the cooling effect preferably flows in the same direction as the reactive mixture, i.e. way down. The upper pipeline 7 for the supply of coolant and the institute for the removal of the pipeline 8 are also foreseen.
The horizontal partitions 9 increase the turbulence of the cooling device that circulates inside the space between the external surfaces of the pipes 2, the internal surface of the housing 1 and the two pipe grids 10 and 11 passing through the pipe supports 2.
Third pipe grate 12, for- in: replenna vygge tube grate 10,
46892.2
pakhokhodkts below chamber 3 for distributing 1H :: gaseous reagent One or 6i: Jiee pipe 14 supplying liquid L: reagent to chamber 13, Yang; .. start-up of the liquid reagent from the distribution chamber 13 of the separation section. - 1 tubes 2 are provided with a threading device (Fig. 2). Each tube 2 in its own BepxHEHi part of 15 5g is supplied by dilindj, j is the same and has a:: slightly larger diameter; the upper end of the pipe is 2 connectors; 1} 1en - with the lowest condom - the upper part 15 cher bz the short cone - 5 times an hour 1 nd 16 "Upper,}; cylindrical
, part 15 of sn-abgene opredgch.genny; nu jto: M trench 17 for liquid reagent; ne outer surface is located with - :; the correct gap is E contact with jiivi peHHeH pg.1Be x: cylindrical cylindrical-3 | -, h (hubs gi 18, which gets iat: 1, en ;;; coarse lattices 10 d 2) 13 is equipped with windows 19 hr; ) shdky pearcHva j. a.Kor o the size and: the main distribution, which is not
;.; happened DIT of loss of pressure: - skidding. Inside the upper end of the cham; g 1 5 pipe 2 a second sleeve 20 is provided, the surface ko; oro: -1 is in contact with the inner | -) internal surface of part 15; for use- Kjir:; 4cni-ieM of its center, due to the presence of –ii; ij shi eokogo annular chute 21. The 1stc1-1-1 channels 22 allow liquid reagent to flow out of the annular (space defined by the same forehead 21, Sleeve 20 consists of the bottom - H-si o the conical end with the same open P) 1m angle 5, as well as the connecting part 16.
Between the lower conde of the sleeve 20 and the hour 16 there is an annular n-, e / s oriented oriented voice of the truncated cone, the width is determined / vertically twisted along the side of the sleeve 20, fitted with the overhang
, thief 23, screwed in the –3-thru part of part 15, By: em: niehert. down the sleeve 20 is regulated by the se-ChS ;; -: not the annular passage;
and and ;;;; - ;. OK to the END of the sleeves 20 and cone-50., „„ ,,
ooch - p; oi connecting part i6.
Ko, ;;;; П, passage, oriented, -; according to cone-forming, the benefits are determined by the distribution of the liquid reagent in the form of a film 24, the whole is around the inner wall of the pipe 2. 1: .1: morning dia; the sleeve is 20 m-is the same as the inner A duster-to-1 dp 2, so that the gas, the outlet from the distribution chamber 3, can be supplied to contact the free surface of the film 24 without noticeable pressure loss.
Due to the constructive simplicity of the liquid reagent distributor, it is very difficult to obtain accurate adjustment of the flow rate through the neg. Indeed, during tests without gaseous reactant supply, deviations of up to 20% were noted between the nominal flow rate and the flow rate in a separate pipe 2 of the indicated reactor.
Despite this, with the proposed method, the deviations of the ratio between the flow rate of the gaseous reactant and the flow rate of the liquid reactant within a certain limit can be maintained.
According to the invention, the pressure of the gaseous reactant gas is significantly lower (about 0.1-0.4 bar) than the pressure of the gaseous reactant,
35
therefore, the position of the levels of P depending on the used initial REO RE is unchanged, the Vlavli pressure of the supplied liquid reagent is higher than the pressure of the gaseous reagent supplied for a quantity equal in weight to the liquid level distribution chamber for it.
In spite of the low pressure of the supply of both reagents and the change in the flow rate of the liquid reagent to more than 20% for different tubes, the molar ratio between the liquid and gaseous agent gases remains very high.
close to the established average value with very low differences by about
 pipe length
In the interval of time (up to t) in each of the three pipes 25, 26 and 27, having the same diameter and length, the same ideal situation occurs, namely, the three speeds of the liquid reagent L, Lj, L are equal, the three flow rates of the gaseous reagent G, Gj and G, are equal and, therefore, three
molar ratios R,, R ,, R equal i
if the diameters of these three pipes are exactly equal, the degree of passage of the reaction of pipes at equal levels is equal
50
a lower flow rate in pipe 26 increases in levels, PJIJ and Pgg, whereas the opposite result is obtained for pipe 27 due to a higher rate of flow of liquid
The difference in pressure between chambers 3 and 5 is equal to the pressure loss for each of these three, in which the indicated pressure losses are therefore equal.
Along with the change in the degree of reaction, the viscosity and, consequently, the thickness of the specified film, consisting of a mixture of a liquid reagent and a liquid reaction product, vary significantly. In particular, with an increase in the degree of reaction, an increase in viscosity and polarity of electrons is observed. ,
Fig. 5 shows that the height h of the part of the pipe 27, where the degree of reaction passing is above 98, is less than the corresponding height b of the pipe 25, which in turn is less than
Because of the difference in lengths 11 h, h, h-j, these three pipes, therefore.
Because of the difference in lengths 11 h, h, h-j, these three pipes, therefore.
n x (Fig, 4, where the numbers P, RD
and ro | respectively, the levels, 55 have different average prone sections, the degree of passage of the reactors for the gaseous reaction stream is 60, 90 and 98% of the corresponding, as the average thickness is captive, the fluids along the pipes are different.
The lily of the tubes is chosen so that the contact time between the two reagents can be quite long under optimal supply conditions, to ensure almost complete conversion of the liquid reagent (the degree of progress is close to 100%). In this way, the completeness of the reaction is always ensured in each pipe, even if it differs from the optimum, when such a situation arises due to faults or m, p.
Assuming that for any reason, in the time interval t, -t, j, the three flow rates of the gaseous reagent G, C, G, G, remain non-expression l. J
As a result, there are changes in the flow rates of the liquid reagent 1, Lj, L, 5 so that, for example,,, 9 Lt / 3, L, t, 1 Lt / 3, where Lt means a decrease in the flow rate of the liquid reagent in three pipes, which remains constant. In pipe 25, the situation does not change (Fig. 4) and.
five
5 therefore, the position of the levels Р РЭО РЭ remains unchanged,
about
five
0
a lower flow rate in pipe 26 increases in levels, PJIJ and Pgg, while the opposite is true for pipe 27 due to a higher liquid flow rate.
The difference in pressure between chambers 3 and 5 is equal to the pressure loss for each of these three, in which the indicated pressure losses are therefore equal.
Along with the change in the degree of reaction, the viscosity and, consequently, the thickness of the specified film, consisting of a mixture of a liquid reagent and a liquid reaction product, vary significantly. In particular, with an increase in the degree of reaction, an increase in viscosity and polarity of electrons is observed. ,
Fig. 5 shows that the height h of the part of the pipe 27, where the degree of reaction passing is higher than 98, is less than the corresponding height b of the pipe 25, which in turn is smaller than
Because of the difference in lengths 11 h, h, h-j, these three pipes, therefore.
Since the three flow rates of the gaseous reagent in pipes 2e 27 depend only on the relative cross sections of the passageways, there is a pressure difference at the edges of three corpses.
3 a pipe 26 with an average cross section of the passage smaller than the initial one (Fig. 4) decreases the rate of flow of the gaseous reactant, driving the molar ratio to an expectation of two reagents to the value of 5% and initially optimal; quantities.
In pipe 26 with an average passage cross section larger than the initial one (Fig. 4) 5, an increase in the flow rate of the specified gaseous reagent is observed, which in the case also leads to a shift of the molar coo, v of the initial optimum value . po: i-- can be, starting from the moment t ,,,. when although remain constant and equal to 1-w the three flow rates L ,. , V, ..., L, liquid reagent, flow rates: gaseous reagent is changed in a manner to have (Fig. 6), for example, G 0., 9 Gt / 3 5 Gj 1, 1 Gt / where Gt - a decrease in the flow rate of the indicated gaseous peai eHj a in three pipes, which remains ncv stationary.
In pipe 25, the situation of the remaining 1 (Fig. 4) and, therefore, the levels of Pg ,, $ Г, and Рдр, remain unchanged: -. Due to lower gas flow rates. G Tr be 26 levels. ,,,, Р
 50
 AND
whereas nz - for more free ir; The gas flow in the pipe 27 ei ypoBiii-i increases.
For the same reasons, there is a decrease in the gas flow rate in the pipe 27 and an increase in the flow rate of the same gaseous reactant in the pipe 26, since this corresponds to; the middle sections of the passage reduce ..: in pipe 27 and increase in pipe 26. In this section. - also molar
the ratios R and R. deviate; t
The optimal initial magnitudes, along with the influence of the balance of modification of the conversion profiles in the pipes, have a Taiuce-balancing effect which leads to an advantage from the observed viscosity deviation with temperature. Indeed, if the average temperature in the liquid film,
 ; 6892S
.; -;; cd mace uiiy-ypii / rub, chalk exchange, cooi ;. The mean also varies averaging from 3 s; about with t ъ Ж1-1 д кост и. S l (; d about 13 atelln ,, jjDi of the same flow rate and rij; riju increase in the average of those: —sheets of 1, Eredl) 1 I then Shchina films decreased, 1, therefore, Wed, r, 1h; esech passage for gas increases, 11p 1iBo positive iris; - ;: single to the case: j ijiHJKOHijii srp; 1 time center of plspkch. C: ice gel 3 for pipe Z6 effect-l
g.NILKhNII CKOVJOCTH HCTO-CJi. LSI::
the reagent cpta leads to the ump;;: .-.:.; - :: ::: about the number of mater: -: ag1aJ rea 1pu -1h; ::: -. ;; Е ed:; .- iS ..its u c)., Cc, ged (g ;;;: yy :: lko J: itts I (1b; le2 ko .- ::.. EaTTj pe; -K .11 11.
Chystyol as served; al; &., i; ; e ;. a-f yp;: - l ps TijKc: oxj; aAv a. : Tv-i. ::: / -p1us op: odi, i; aK:; iii ,,;; s Juii with :; -z ;; Shch: G with; -. 1ln
-. :::, -. ja.;., og tea; -: n; dzhe, che.- first, uji: -i 4ecTEa T - ;: ruia ;; c - Uv uj and, kgigorea c) bq (;; iyivayatsya oy: .1 pushed; by her environment, i fi Pel; ultimately, this leads to more -; and; cc; which mean viscosity, higher - :: oi-: average tol1g; not the film and trace aTeJObHO-j to the gas passage
1i) how much is the pressure at the end of the TRU-,: Cl 2d; remain -: unshifted speed j: c:; a l ;; - a f; ,,, decrease c and trace. -2 - -. - - -, - ,,,
li - O;: reduction of the ratio to the outcome-- i ::: rt , -.; -1 rubles 27 (f; g, 5). flow R4n: CKOpocTJi flow at; sod; 1 t to y: ie-. ICS:; ICT: OLC:; ala r agk-- .v (iro: as time goes on, and, with /: r; ds- -potolno, to Zlcpkmu: o,; 1,1 -; - :; heyou; - -1, g 1d ; 1el c: C; mus; - :: pii h; - 1,: -: c ;.
 SG: Tuatsi; . -. . ,
 1ro P BopsloL: 11сy taccju i - - L.:;-ee; d, C1; edova :: e., IU; 6ji: r. . . - -were-- ic: --i :. Temper /; ut.-s -; -1 ::: i-, ii: i I - iijrc iri a of average wk. ; -.;:,: kn th, -; -.) -: if di; to belypenu sech -;):;:;,, at :. ;;: ,, -: og
 :; tp; . case of swiftness:; s .-,: ..:.: gaz gas:;: ceases with uveapeshche-; relations:: relationship;: laziness; about to perlopachal. : a.ly size
1-J situation fr; g. 6 р.н post: :) Ley rate of fluid flow average w-jn -; -: U a temperature of the film is pactic; vr; subjected to action and work;) 5 this balggsiruyayy; u; f; 1: t manifests itself 1 thanks to: -gz -v; Iercl profile -; , spzersr; g;
 7
These two oajiancHpyroiuiix effects are so powerful to compensate for the unbalancing effect due to the application of the flow rate of the reagents and do not restore the first channel optimum value for the flow rates in each pipe but only the initial value of the molar ratio between the two reagents.
Indeed, based on the ideal situation (Fig. 4), k; when the unstable period ends and the balancing effects give their results, the single situation compatible with the material balance of the entire reactor is:
R R p. / - J.
Therefore, despite the fact that the flow rates in each pipe are different from the ideal GT / 3 and LT / 3, the molar ratio in each pipe corresponds to the setting of BH and the control devices of the reactor.
Example 1. As the original product using linear dodecylbenzene with a wide range of composition-Cd.
Sulfur content in the feedstock,
Average molecular weight of feedstock 267
Feed flow rate, kg / h180 Concentration 50 in gas carrier, vol.% 5 TeNfflepaTypa SO fed to the reactor, C 36-40 Pressure at the inlet of the gas reagent to the reactor, bar 0,180 Overpressure of the liquid reagent, bar, 0.05 Proposed reactor has the following characteristics: number of pipes 7, internal diameter of pipes 25 mm, length of pipes 6000 mm,
Water with a temperature of 25 ° C is used as a coolant.
the exit of the reactor 45 C.
Analysis of the composition and characteristics of the product obtained after aging and stabilization:
468Ч2
/ 40
thirty
34
0
The availability of peprosulfurized material in the reaction,% 1.35
Amount of free 3H S0,,% Below 1
Product Color, Kletta25
Example 2. Performance characteristics used for the sulfonation of synthetic lauryl alcohol - fO and (c.) G
The average molecular weight of the feedstock 207 The flow rate of the feedstock, kg / h150 f5 Concentration 30 in the carrier gas, vol.% 5 Te fflepypa 30 fed to the reactor, ° C 38 Pressure when the EO gaseous reactant is supplied,
bar0,179
Overpressure of liquid reagent, bar0.008
The reactor used has the same 25 characteristics as the reactor of Example 1.
As cooled, giving liquid - water with a temperature of 20 ° C was used. Sulfated product at the exit of the reactor has a temperature, Analysis of the neutralized product: Amount of non-sulphated material,% 1.9
Content,% 0.88
Color, iCrieTTa 7
Neutralization is carried out in an aqueous solution of caustic soda. The indicated amounts of non-sulphurized material and sodium sulphate are 100% of the active substance.
Example 3 Performance characteristics used for the sulfonation of synthetic lauryl alcohol (C) ethoxylated with three molecules of ethylene oxide:
Average molecular weight339
The flow rate of the raw material, kg / h 130
0Concentration SO, in carrier gas, vol.% 2.5
Te merapypa SO-, supplied B reactor, C 36 Pressure at flow
5 gas reagent, bar 0,303
Excess pressure of liquid reagent, bar0,015
The reactor used has the same characteristics as the reactor. Example K The product that is removed from the reactor has a temperature that is cooled ;; schA water -.
Aaaliz Paytraral Product Quantity Amount of non-sulfonic E1 material; % 3
The content of Na.j 80, I e Color S Kletta15
Neutralization is carried out immediately after the water in water solution,
6892 O
According to pvsprosulfurised prol, yktu and sulphate, patches are classified as 100% active (
; Color co1; ecch) hc: the product is determined on a Rltett-Sommers-o colorimeter with boiling water (filter 42 in 5%;; solution, Nslo: 1 cozier cell 40 mm.
Aa
f --- H chcha
t :.
r / -.
-.-,
. - -.- -, /
about
oo
{oI
 oo /
 -...
 h / /
. /
 J
15
G,
five..
Sj
  i

Jif
G:

l
Re | T
iocr
EiL PSS
Pos
C
-c:
 -2 3
 bO
., j ..,
F (g. 5
 I
40
Pgc
P98
.6
Compiled by T.Vlasova Editor I.Nikolaychuk Tehred I.Popovit- Proofreader V.But ha
Order 4027/59 Circulation 379Subscription
VNIIPI State Committee of the USSR
for inventions and discoveries 113035, Moscow, Zh-35, Rauigska nab., 4/5
Production and printing company, Uzhgo15od5 Proektna st., 4

权利要求:
Claims (2)
[1]
1. A method for producing sulfonated or sulfated organic compounds such as dodecylbenzene, lauryl syirt or ethoxylated lauryl alcohol, combined by treating the 'liquid feed reagent with gaseous sulfuric anhydride diluted with an inert gas to 3.5-
7 vol.% At 35-45 ° C in a variety of parallel vertical pipes cooled externally with a downward flow of reagents, followed by neutralization with caustic soda, characterized in that, in order to improve the quality of the target product, the filing of the liquid source reagent in the form of a film into many identical parallel pipes, each 5-7 m long and an inner diameter of 2030 mm, are carried out through annular grooves with a clearance of less than G mm and the process is carried out while maintaining the supply pressure of the gaseous reagent 0.179-0.3003 bar, and the supply pressure of the liquid ex one reagent - 0.005-0.015 bar above the supply pressure of the gaseous reagent.
[2]
2. A sulfonation or sulfation reactor for organic compounds such as dodecylbenzene, lauryl alcohol or ethoxylated lauryl alcohol, gaseous sulfuric anhydride containing a vertical cylindrical body, horizontal tube sheets fixed in the body and dividing it into gas inlet chambers, liquid reagent inlet, heat exchange and the output of the reaction products, vertical reaction tubes fixed in tube sheets and made with holes for supplying a liquid reagent, which are located in the chamber in liquid reagent water, and reagent inlet and outlet fittings, characterized in that, in order to improve the quality of the target product by improving the distribution of the liquid reagent, it is equipped with a cylindrical sleeve with a conical lower part and an annular groove mounted coaxially inside each reaction pipe, the annular groove of the sleeve is located opposite the hole in the pipe for introducing the liquid reagent and forms an annular distribution channel for supplying the liquid reagent to the inner surface of the reaction tube.

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引用文献:

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DE2107968C2|1970-02-23|1982-05-19|Costruzioni Meccaniche G. Mazzoni S.p.A., Busto Arsizio, Varese|Process for the sulfonation and sulfation of organic compounds with sulfur trioxide and device for carrying out this process|

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JPS5218682B2|1972-04-15|1977-05-24|

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IT1255737B|1992-05-19|1995-11-15|MULTITUBULAR FALLING FILM REACTOR|

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DE102005060816B3|2005-12-21|2007-03-29|Rudolf Aigner|Sulfonation and/or sulfation of liquid organic raw materials with sulfite/air-mixture comprises splitting the mixture feed into two feed points with in reaction tubes and/or annular gap region of annular gas-falling film reactor|

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DE102008000785A1|2008-03-20|2009-09-24|Evonik Röhm Gmbh|Process for the preparation of methacrylic acid|

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EP3094615A4|2014-01-13|2017-11-08|P2 Science, Inc.|Terpene-derived acids and esters and methods for preparing and using same|

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WO2015196019A1|2014-06-20|2015-12-23|P2 Science, Inc.|Film ozonolysis in a tubular or multitubular reactor|

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ITUA20162647A1|2016-04-15|2017-10-15|Iit S R L|PROCESS AND DISTRIBUTION SYSTEM OF ORGANIC SUBSTANCE IN FALLEN FILM REACTOR, AND REACTOR SO CONSTITUTED|

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US10668446B2|2016-06-21|2020-06-02|P2 Science, Inc.|Flow-through reactors for the continuous quenching of peroxide mixtures and methods comprising the same|

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EP3512631A4|2016-09-16|2020-05-13|P2 Science, Inc.|Uses of vanadium to oxidize aldehydes and ozonides|

法律状态:

优先权:

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申请号 | 申请日 | 专利标题

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IT7912480A|IT1166068B|1979-02-23|1979-02-23|PROCESS PERFECTED FOR FILM SULPHONATION IN A MULTITUBULAR REACTOR WITH A MULTITUBULAR REACTOR SUITABLE FOR CARRYING OUT THAT PROCEDURE|

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