专利摘要:
A countercurrent washing tower including a slurry-charging nozzle provided in an upper part of the tower, a slurry-dispersing member disposed underneath the slurry-feeding nozzle and a plurality of washing liquid feeding nozzles provided in a lower part of the tower, thereby conducting the countercurrent washing of the slurry while maintaining each of the flows of the slurry and washing liquid in a stable and macroscopically-laminar state within the tower. A slurry of a synthetic resin can be washed countercurrently with good washing efficiency and percentage recovery of the synthetic resin by using the above washing tower and charging the slurry of the synthetic resin through the slurry-charging nozzle at a flow velocity of 0.5 m/sec. or slower as measured at the opening of the slurry-charging nozzle and, at the same time, feeding the washing liquid from the washing liquid feeding nozzles, preferably at a flow velocity of 0.2 m/sec. or slower as measured at the openings of the washing liquid feeding nozzles.
公开号:SU1251797A3
申请号:SU833633346
申请日:1983-08-02
公开日:1986-08-15
发明作者:Оока Татуо;Фунакоси Есиюки;Утикава Нобутака
申请人:Мицуи Тоацу Кемикалз Инкорпорейтед (Фирма);
IPC主号:
专利说明:

t
HgoPpeTcitiie from} Osita to the prototype purge, intended for washing the suspension, and can be used in the chemical industry.
The purpose of the invention is the higher productivity of the washing column and the effectiveness of the washing.
FIG. 1 shows schematically a counter flow wash column; in fig. 2 shows an arrangement for ensuring the supply of nozzle washing fluid; in fig. 3 - providing the flushing fluid nozzle section; in fig. 4 - jcxeMa annular arrangement of nozzles.
Iro tivotsi g1l prom 11yuchny pillar 1 el 1111 ien.ch:, 1kr | .1top behind Hciciiimi icini by inputs for the material that needs to be processed, and the liquid and B, Ghodor for the treated material and the used washing liquid (hermetic The flattening of the blade is especially necessary (handling of fuel B (1 spi
Column godeu) | G1p body 1, nozzle 2 for springs cycrioii-jini with an outlet, installed, for example, in the center of the upper part of body 1 Ko. ioiiiri I. Cnii.iiii 2 (vnqjbiBa-, for example, from the bottom. Nozzle 2 is intended for a smooth B1 suspension to the inside of the body 1 of the column with a small air to prevent the bucket post 1 (ka.Ll etog nozzle diameter 2 to Opportunities should be BOLY1 PM. O / T. PK-O -1RI
diameter of coirjin 2 n) oncxci; u (formation. y; 1 log. ivoryh flow OTpa6o r, 4 inriii; i; n ;; (. oc i k for npoMt: i vani, n pfiy ;; i, gc - what causes the turbo:; entn |,; (no-i-pc and does not form. steady-state-11-one-px-1-ti taken-up-eii -... suspension of n r-trlbotnp of protractive fluid.
Usually, the ripo i ibot (1 × 11, 1 pipette and the casing column contains G1 at the supply. Suspended flow of sus: 1ben1-: and sleep.pi 2, however, they may be bullish and only, if you prefer, gelt, by placing them in the form of a single block Hieptradt.N1.1y BepxneiV class Kojiiiyca Kojionntii.
1l) D conjTOM 2 pa. providing ai 4iuii i dist rgprotline conical suspension: disks surgery 3 image | 111) iepi: inHoii to nozzle 2. Koii cheskpy jincneprnp noiiuut element 3 pre517972
it keeps moving the suspension, which is injected into the colorp: s through the nozzle 2 and moves in the form of a free-falling current P1:), and provides it
5 uniform dispersion. The dispersing element 3 protrudes under the opening of the nozzle 2. and it should be larger than the opening of the nozzle 2 as compared with BhinycKHhiM.
10 The cross-sectional area of the top of the top of the dispersing element 3 is greater than the cross-sectional area of the nozzle outlet 2,
15 A dispersing element that provides dispersion of a suspension of 3 m (it can be made in the form of a simple paste design. For a smooth I o and a uniform dispersion of pa20 dan) | this suspension in horizontal and radial napranle11X1XXx should be in such a way that) 1 flow paths formed by a falling suspension 25, byp PLV1) 1 curves, the conical shape of dispersion element 3 from a nerve cone, pattern O1 to honeycomb 2 is preferable (an umbrella or hemisphere configuration) .
The diameter of the nozzle is 2 dollars / ken to be maximally, but in a possible way, and, consequently, (l. Shdie chyuyuyy d 1spergirovanie suspension dispersion element 3 dol-ks-k-n cross-section. However, when the surface area is dispersed1 And here of element 3 iipfu- ipaHci in between it and the wall s :-) 1 kpg 01P1y becomes narrow, and the appearance of the perturbing i: 1h; and ;: | stnyi each other suspension and G1p (1fluid fluid, which gp ohod) BTiejix and down respectively through this space, as a result of the chow arises T urbultent- ((: t. accepting in BHnMvinne as a move down soil suspension, and d, u1: q1dpys upward flow of flushing liquid, for which delivery is intended i, 4OHF: i means in the form of a row of nozzles 4,
 The area of this site rrpoc i - i.-iiiCTBa is larger than the area of horizon T, MjnjHoro of cetreiuin of support section 5 of housing 1 - washing column.
55 5i nozzle inlet port 2 through which slurry is injected, spread vb1p1zi of the top of the body 1 of the washing colo} 1n. If prom ot35
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3
If the nozzle 2 is positioned somewhat away from the top of the casing of the wash column in order to provide a small space between the outlet and the top, a stable interaction surface between the suspension and the used flushing liquid forms under the outlet of the nozzle 2. On said surface, the interactions of the suspension and the spent washing liquid are separated from each other. Thus, the part forming the interaction surface is used as a distribution zone for the suspension of the spent washing liquid.
Under the ensuring dispersion by dispersing element 3, there is an upward supporting section 5 of body I (washing zone L) of the column, above which a deposition (separation) zone B located in the upper part of the column housing 1 is placed, and the connecting zone B. A uniformly dispersed area is given in contact with an upstream countercurrent flow of washing liquid in these zones, resulting in a washing of the suspension.
In the lower part of the support section 5 of the casing 1 of the wash column, a series of nozzles are installed, each of which has a small opening — an exit slit for supplying the flushing liquid into the casing 1 of the wash column. The nozzles 4 provide a supply of washing liquid up through the wash column. In order to avoid turbulence in the wash column, the exit slits of the nozzles 4 are set obliquely to the horizontal plane and directed towards the bottom of the housing 1.
An outlet opening 6 for the washed slurry is made in the wall of the washing column 1 at its bottom. It passes through at a point located in the lower part of the column housing (i.e., in the cone-shaped part D) of the washing column. Through this opening 6, a naturally precipitated suspension is removed after washing it. To prevent turbulence in the fluid flow inside the industrial
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nozzle columns 4 are placed ni.inie HC1GO holes 6.
Each hundredth 4 contributes to the stabilization of the flow of liquid flow within the washing column. In addition to the exit |, p slots, guiding means such as a ceramic grid, a piece of cloth or a screen (not shown) could be provided in the nozzles 4. In the upper part of the c. -Pusp 1, the upper pyshodny opening 7 is made through its wall to remove the washing liquid. The nozzles 4 are connected to the line 8 supply of washing liquid.
Offer a flushing column OID Flush washing a significant volume of suspension with P) ic. gi | h; 1ost1) Yu, under conditions that correspond to macroscopic and arterial flow, for example, there is no use of a mixer in the nei, a mixer, a medium, a liter, 1, and f, which corresponds to the current flow program. However, the real values of the 1P1I flow rates of the suspension and G1p (1-part fluid can vary significantly depending on the physical properties of the solid material and the fluid.
The proposed wash column, for example, for washing a suspension of synthetic resin, works as follows.
The specific gravity of the CHHTCI resin is similar to the specific gravity of the phosphorus carbonate, bone, as which water or organic solvent can be used. , 1c particles of synthetic freedoms1 About pechuschuts in suspension, nonroNiy TpvV r.Ho ensure the penetration of the bol1, - I jiix (1b7 -.eme synthetic resin by the tm1 holiday method. As a suspension of nnthetic use a suspension of polyppronilon.
With uch: penzp polyprojable, P Eluchenn pn according to the method of bulk noyn f-U-rising NIN, has advantage; in terms of suspension with suspension, it is obtained by C (ii ii; iCHo in the way nnmormor1;: ii111 1h 1lt-tl L body , at about, which has been carried out using a saturated liquid carbon of hydrogen, the amount of carbon in a coral is 5 or more, preferably 5-7, but the solvent is solvent, and the resulting polymer can be solvent. nyTPNf 11-ni; -p-nn danny polymerizayanone suspension due to the fact that Enriched hydrocarbon monomers (in particular, propylene), used as a solvent for polymerization, have high vapor pressure and, therefore, are volatile to evaporation. However, the polymer obtained according to the bulk polymerization method contains boiling n-heptane soluble polymers and catalyst residue in high concentrations.
The physical properties of a polymer containing a solvent in boiling n-heptane polymers in high concentrations are degraded, especially with respect to stiffness, stress, etc. Accordingly, the characteristic properties of polypropylene are degraded; it is virtually impossible to use ultrasound in cases where relatively high physical properties are required.
The method of volume polymerization of 7C {Isiol-Esotsia allows reducing the amount of catalyst remaining in the substance, since the rate of polymerization is higher than the full-scale method in a solvent and polymerization can be carried out under conditions that are effective for the use of the catalyst. However, taco also cannot be used in cases when it is required; - it is of low quality, but it can not be matched; the breechiness and color do not correspond to the standard of tsrsiuomi--. For these reasons, in practice, soluble n boiling c-heptane polymers and catalyst residues are removed from each propylene polymer or copolymer obtained by polymerization.
The polypropylene slurry is introduced into the wash column through the nozzle 2. Dispersant element 3 is arranged; : En1c, 1st under nozzle 2, evenly disperses the slurry through the column and reduces the slurry flow rate, resulting in a stable interaction surface between the slurry and the developed washing liquid, which prevents the occurrence of a turbulent slurry flow into the supports

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Pom plot 5 Corps I wash wash. The flow rate of the suspension is clearly correlated with the state of the interface and the turbulence of the suspension in the support section 5 of the MIJ production column. Since the flushing efficiency for polypropylene decreases significantly with increasing flow scopes, the latter is limited to 0.5 m / s or less, preferably 0.1 m / s or even less. The efficiency of the flush increases with decreasing rate of suspension introduction.
The diameter of the dispersing element 3 influences the likelihood of excluding dynamic pressures in the slurry. With a diameter of the diameter, the growth of the dispersing element 3 becomes large. However, the diameter of the dispersing element 3 should not significantly increase, since the average speed of the two flush top of the flushing fluid in the annular section of the cross section between the dispersing element 3 and the inner wall of the casing 1 of the countercurrent washing column increases and begins to transform from 1-1П1 to the average value of the flow velocity. inoA fluids in the horizontal cross-sectional plane in the washing zone A, which worsens the conditions for the deposition of polypropylene particles and sposs) arises from the occurrence of i in tuberculosis. The diameter of the dispersion-iiiCi of the e.1-element 3 is 0.1-1.5. n; approximately 0.5 - 1.0, the diameter oiioiiHuro of section 5 of the hull 1 of the TO4Hoji promt, 1 in the column.
The industrial fluid containing the propylene in the mainstream is introduced into the lower part via the supply line 8 through the nozzles 4 in order to facilitate its dispersion. It is desirable to have in each of the exit slits a ceramic grid, a piece of cloth or a screen, for example a weeding grid. The flow rate during the washing of propylene fed through the nozzles 4 is clearly correlated with the stability of the boundary section formed between the suspension and the used washing liquid in the upper part of the housing 1) in the column and the degree of turbulence of the suspension in the washing zone L. Since efficiency
Reducing the flow rate of the flushing fluid to a value of 0.2 m / s or less, preferably to 0.05 m / s or less, In addition, the o67jeM suspension, from which no solids are removed, increases in case when the velocity of the upward flushing fluid stream forms the boundaries of the interaction between the slurry and the flushing fluid in the wash column.
A synthetic resin slurry, e.g., a polypropylene slurry, can be npoMi.iTa countercurrent-i in large volumes with good quality of washing and a high percentage of synthetic resin recovery by using the proposed industrial burner column and ensuring such a mode of operation that allows for better conditions described above.
Example (control), Suspension preparation: AI polypropylene.
A vibratory mill equipped with a tank (internal volume of 700 liters) was used, which contained 2300 kg of steel balls with a diameter of 12 mm. 60 kg of magnesium chloride was introduced into the container under a nitrogen atmosphere. 12 liters of tetraethoxysilane and 9 liters of 1,2-dichloroethane. The contents of the container were milled for 12 hours. Then, 36 kg of the ground mixture and 240 l of titanium tetrachloride were loaded into a thoroughly dried mixing bag (internal volume of 600 l) in a nitrogen gas atmosphere. The contents were stirred at 80 ° C. for 120 minutes and then kept. The resulting supernatant was removed. Then 420 l of n-heptane was added, the mixture was stirred at 80 ° C for 15 minutes and kept. Remove the vip-nip layer. This washing procedure was repeated 7 times, after which it was added 240 l of n-heptane to form a suspension of the solid catalyst. A suspension of the solid catalyst was sampled and n-petchan was distilled off from the suspension. The precipitate was analyzed. This analysis showed that the solid catalyst contained 1.62 7, by weight Ti. 4000 kg of propylene were loaded into a polytrimmerization device, equipped with a jacket and having a volume of 20 m, which was previously dried, dried, filled with nitrogen, and then propylene. In a small car. Internal jhim with a volume of 30 l was loaded with otdelt.nosti 22 l of n-heptane, 1056 ml of diethylamine chloride, 616 ml
methyl g-p-toluiata, and 220 g of the solid catalyst prepared as described above. The contents were mixed at room temperature for t minutes, after which 220 ml of aluminum triethyl was added. The resulting mixture was injected under pressure into a polymerization unit with a monitored volume of 20 m. After this, the device injected the device with 900 meters of hydrogen gas.
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and the temperature inside the device was raised to rm by passing heated water through the ruble. The polymerization was continued while maintaining the temperature in vcTpoficTBe at 75 ° C and with the supply of gaseous-GS.1 hydrogen inside the polymerization unit so that the concentration of hydrogen gas was at the same level. The autoclave was continuously fed under pressure and at a rate of 1 I O ml / min to a solution containing 660 ml of triethylaluminum, pacirated into 12540 ml of n-heptane, and also liquid propylene at a rate of 27.5 kg / min, with the result that it was provided. In the course of 2 h polymerization of propylene. After that, 16.5 kg of diethylngol of monoisopropyl ether was introduced into the system in order to | stop the reaction. Zaghem contents were mixed with suspension} 1y, contents Its 3300 kg polypropylene / 4000 kg propylene.
Example 1. Washing the propyl suspension was carried out in an anti-wash column, the dimensions followed with a leaching: the inside diameter of the washing zone is 80 cm; length of wash area A 500 cm; inner diameter of the zones, 1B sedimentation of the suspension 120 cm; the length of the precipitation zone B is from — where the suspension is 200 cm; the height of the part is 100 cm; the height of the junction ei oiu.i B between the Bepxiieii zonoGg B sedimentation-branch1 and, n zone A prom, that 1i-branch | 70 cm; the diameter of the bottom surface of the conical core of the first displacement of the suspension of the dispersing element 3, located under the nozzle supplying the suspension, 2, 60 cm; the diameter of the outlet of the nozzle 2 for the introduction of a suspension of polypropylene, which is subjected to washing, 1 inch (2.5 cm); nozzle diameter 2 6 inches (15.24 cm).
The washing propylene was introduced via line 8 into the countercurrent wash column through nine sintered cylindrical nozzles A, as shown in FIG. 2 in order to disperse the washing liquid. Each of the nozzles 4 has a structure corresponding to that shown in FIG. 3. The washed suspension was removed through the outlet opening 6, and the spent washing liquid — 1) without the outlet opening 7. When using the specified column, the suspension, floor 1-non 1 in the example used as a control, was introduced along the feed line of the nozzle 2 with a speed 1880 kg / h (like polypropylene) and with a flow rate of 0.06 m / s to the inside of the column through nozzle 2. At the same time, propylene used as washing liquid was fed through a line in the amount of 2900 kg / h at a flow rate of 0.01 m / s into the column through the nozzles 4. Washed Susp It was removed in an amount of 1880 kg / h through the outlet opening 6, while the spent propylene was removed in the amount of 2900 kg / h through the upper outlet opening 7 intended for the washing liquid. The washing was continued for 2 hours, during which it was carried out the regulation of the supply of the suspension and propylene, as well as the removal of the washed suspension and recovery of the multi propylene at the above levels. Then, to determine the efficiency of the powder, the powder obtained by drying the suspension prepared by F according to the example used as the control, the supernatant layer being removed when the stirring process in the autoclave, the same as the one being performed, and powder obtained by drying the slurry.
The parameters analyzed were the intrinsic viscosity (l) of the powder obtained by drying the suspension prepared in the control example, the residue (in percent) of the polymer after extracting it with boiling n-heptane, calculated as the ratio of half a polymer after extraction / polymer before extraction X 100% (denoted by T T)
A1, Mg and methyl-p-toluylate.
Mixing in the autoclave was stopped and the expanded layer was separated, removing it from the autoclave during the implementation of the test example.
The nonvolatile components (dissolved polymer + dissolved ash), A1, Mg, and methyl p-toluylate present in the surface layer were analyzed. In addition to 11, A1, Mg, and methyl p-toluylate were also analyzed in the powder obtained by drying the washed suspension. The results are presented in table. I.
Based on the analysis data A1 and Mg,
present in the powder, as well as non-volatile components present in the supernatant, calculate the percentage of A1 dissolved in propylene relative to the total amount of aluminum based on the data from table. G:, 3%.
Similarly, the percentage of Mg dissolved in propylene, in relation to the total amount of Mg,
amounted to 78.2%.
The supernatant was dried in order to determine the weight of the polypropylene dissolved therein. It was established that the amount of soluble propylene corresponded to 1.4% of the entire 1-1-meter pol. Assuming that methyl p-toluylate is fully attached to the dissolved polypro-, present in the device
for polymerization, the concentration of methyl-p-toluylate thus added was calculated by the equation
., 058, 0,, dh per million
Thus, the percentage of the remaining elements in the dissolved parts of the purified polymer was: AI 1.3%; Mg 2.0%; methyl p-toluylate 1.5% and a soluble polymer 2.0%.
Therefore, the cleaning efficiency is 98.7% for AI, 98.0% for Mg, 98.5% for methyl-p-toluylate and
100% of the soluble polypropylene In the mid-range, the cleaning efficiency is 98.8%.
The percent recovery of polypropylene for the amount of half-gravel and Kai-alizer residue that were removed by spent propylene with BNtecTe was determined by evaporating the spent polypropylene to obtain a dry substance. As a result, it was found that the percentage recovery of polypropylene was 98.4%.
PRI me R 1 (comparative). The experiment was carried out according to Example I, only the nozzle 2, intended for supplying the field of tropylene to the countercurrent washing column, had a smaller diameter with a change in the velocity of the flow of the slurry flow to 1.5 m / s. The washing efficiency values determined on the basis of the analysis of L1 and methyl p-toluylate, carried out in the same manner as in example 1, the amount of sludge removed in the same manner as in example 1, and the amount of sludge removed together with the spent Short proprietary {om, are presented in table. 2. Both the efficiency of the industry and the percentage of extraction of polyethylene had lower values compared with example 1.
Example 2 (comparative). The experiment was carried out according to Example 1, only the nozzles 4, intended to introduce the propylene used for washing into the countercurrent washing column, were stirred in the form of a hoop, as shown in
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FIG. 4, and the propylene used for washing was fed at an average flow rate of 1.5 m / s through eight openings into the countercurrent washing column. The results of the analysis, which was carried out in exactly the same way as in comparative example 1, are given in table. 2
Compared to Example 1, the washing efficiency and the percent recovery of lipropileans did not decrease.
Example 3 (comparative). The experiment was carried out according to Example I, only the dispersing element 3, which provided dispersion of the suspension, was removed from the countercurrent column. The results of the analysis, which were obtained in exactly the same way as in comparative example 1, are given in table. 2. Compared with example 1, the efficiency of the flushing and the percentage of extraction of polypropylene decreased significantly.
Example 4 (comparative). The experiment was carried out as in example 1, only the diameter of the dispersing element 3 that provided dispersion of the suspension was reduced to one third of the diameter of the bottom, of the element 3 used in gidrimer I. The results of the analysis, which would be carried out in exactly the same way as in Example I, are presented in Table. 2. In comparison with example 1, the efficiency of proshgany and the percentage of extraction of polypropylene is lower.:;
Table 1
1.32
197
 Methyl p-toluylate has been assumed to be fully bound to undissolved polypropylene.
table 2
98.7 98.5 Comparative
The flow rate of the suspension flow, determined at the nozzle 1.5 m / s
The flow rate used for flushing propylene 1.5 m / s
Without conical dispersing element
The diameter of the bottom of the conical element: 1/3 of the element used in the application
Continued table. I
98.4
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97.7
31.2
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94.8
97.3
eight
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fig 2
(re.e.
i
cpuff
Editor A. Lezhnia
Compiled by L. Koltsova
Tehred L. Serdyukova Proofreader M. Samborska
Order 4428/60
Circulation 640 Subscription
VNIISH State Committee of the USSR
for inventions and discoveries 113035, Moscow, Zh-35, Raushsk nab., 4/5
Production and printing company, Uzhgorod, st. Design, d
权利要求:
Claims (1)
[1]
A counterflow flushing column containing a housing, a nozzle for introducing a suspension with an outlet located in the upper part of the housing having a supporting portion, a lower outlet for removing the washed suspension, made in the wall of the housing at its bottom, an upper outlet for removing the washing liquid, in the case wall, and flushing fluid supply means located in the lower part of the supporting section above the outlet. To remove the washed suspension, so that In order to increase the productivity of the washing column and the washing efficiency, the column is equipped with a conical dispersing element located under the nozzle for introducing the suspension and facing the apex, the cross-sectional area of the protruding upper part of which is selected with a larger cross-sectional area of the nozzle outlet to create a downward macroscopic laminar flow of the suspension, moreover, the cross-sectional area of the support section, vertically placed under the dispersing element, A smaller area of the annular channel between the casing and the dispersing element was selected, and the flushing fluid supply means are made in the form of a series of nozzles with outlet slots, the axes of which are arranged obliquely to the horizontal plane and directed toward the bottom of the casing to create an upward macroscopic laminar flow of flushing fluid and form a boundary section between the suspension and the spent washing liquid in the upper part of the housing.
SU, „> 1251797>
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同族专利:
公开号 | 公开日
CA1217599A|1987-02-03|
AU1720883A|1984-02-09|
JPH032162B2|1991-01-14|
BR8304149A|1984-03-13|
KR860001912B1|1986-10-24|
PT77116B|1986-01-27|
EP0101907A3|1985-05-15|
MX162891B|1991-07-05|
PT77116A|1983-08-01|
NZ205078A|1986-08-08|
JPS5925803A|1984-02-09|
AU548326B2|1985-12-05|
IN158401B|1986-11-08|
EP0101907B1|1987-07-15|
KR840006133A|1984-11-22|
DE3372440D1|1987-08-20|
EP0101907A2|1984-03-07|
引用文献:
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US3454545A|1964-10-30|1969-07-08|Phillips Petroleum Co|Polymerization of mono-1-olefins|
US3998739A|1973-08-02|1976-12-21|Kurita Water Industries Ltd.|Apparatus for filtration|US4836302A|1986-12-03|1989-06-06|Heilhecker Joe K|Apparatus and method for removing and recovering oil and/or other oil-based drilling mud additives from drill cuttings|
JP2639484B2|1991-12-24|1997-08-13|松下電工株式会社|Lobby intercom with integrated control unit|
GB2353735B|1999-09-06|2003-06-11|Ici Plc|Apparatus and method for extracting biomass|
CN1294182C|2001-12-03|2007-01-10|株式会社吴羽|Method of continuously cleansing polyarylene sulfide|
DE10163163A1|2001-12-20|2003-07-03|Basf Ag|Process for the production of highly functional, hyperbranched polyester by enzymatic esterification|
ITMI20050705A1|2005-04-20|2006-10-21|Solvay Solexis Spa|PROCESS FOR THE PREPARATION OF FLUOROPOLYMER DISPERSERS|
EP2727637B1|2012-11-06|2019-08-28|Uhde Inventa-Fischer GmbH|Extraction reactor and method for extraction of granular material|
法律状态:
优先权:
申请号 | 申请日 | 专利标题
JP57134708A|JPH032162B2|1982-08-03|1982-08-03|
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