CN109261221A - A method of for removing reductive organic matter in vanadium silver molybdophosphate catalyst - Google Patents
A method of for removing reductive organic matter in vanadium silver molybdophosphate catalyst Download PDFInfo
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- CN109261221A CN109261221A CN201811327154.6A CN201811327154A CN109261221A CN 109261221 A CN109261221 A CN 109261221A CN 201811327154 A CN201811327154 A CN 201811327154A CN 109261221 A CN109261221 A CN 109261221A
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- washing lotion
- organic matter
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- 239000003054 catalyst Substances 0.000 title claims abstract description 36
- 239000005416 organic matter Substances 0.000 title claims abstract description 14
- OTGZYHVWXQELCL-UHFFFAOYSA-N [V].[Ag] Chemical compound [V].[Ag] OTGZYHVWXQELCL-UHFFFAOYSA-N 0.000 title claims abstract description 9
- 238000000034 method Methods 0.000 title claims description 14
- 230000002829 reductive effect Effects 0.000 title abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 55
- 239000006210 lotion Substances 0.000 claims abstract description 30
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims abstract description 12
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 12
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 6
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims abstract description 5
- 230000004913 activation Effects 0.000 claims abstract description 5
- 238000006073 displacement reaction Methods 0.000 claims abstract description 5
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical class CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000009835 boiling Methods 0.000 claims abstract description 4
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims abstract description 3
- POLCUAVZOMRGSN-UHFFFAOYSA-N dipropyl ether Chemical compound CCCOCCC POLCUAVZOMRGSN-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000005516 engineering process Methods 0.000 claims abstract description 3
- 150000008282 halocarbons Chemical class 0.000 claims abstract description 3
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 3
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 3
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims abstract description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract 6
- 238000010926 purge Methods 0.000 claims description 7
- 238000003860 storage Methods 0.000 claims description 4
- 238000003825 pressing Methods 0.000 claims description 3
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 5
- 229910052720 vanadium Inorganic materials 0.000 abstract description 5
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 3
- HSJKGGMUJITCBW-UHFFFAOYSA-N 3-hydroxybutanal Chemical compound CC(O)CC=O HSJKGGMUJITCBW-UHFFFAOYSA-N 0.000 abstract 2
- 239000000126 substance Substances 0.000 abstract 2
- 150000001299 aldehydes Chemical class 0.000 abstract 1
- 238000001354 calcination Methods 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 10
- 239000000047 product Substances 0.000 description 10
- -1 3- methyl -3- cyclobutenyl Chemical group 0.000 description 8
- ASUAYTHWZCLXAN-UHFFFAOYSA-N prenol Chemical compound CC(C)=CCO ASUAYTHWZCLXAN-UHFFFAOYSA-N 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 5
- 239000012065 filter cake Substances 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 239000012190 activator Substances 0.000 description 4
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 4
- 125000001972 isopentyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])C([H])([H])* 0.000 description 4
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 4
- 238000010792 warming Methods 0.000 description 4
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 description 3
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 2
- 229940010552 ammonium molybdate Drugs 0.000 description 2
- 235000018660 ammonium molybdate Nutrition 0.000 description 2
- 239000011609 ammonium molybdate Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 125000001047 cyclobutenyl group Chemical group C1(=CCC1)* 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 229910001961 silver nitrate Inorganic materials 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- WTEVQBCEXWBHNA-UHFFFAOYSA-N Citral Natural products CC(C)=CCCC(C)=CC=O WTEVQBCEXWBHNA-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 235000019445 benzyl alcohol Nutrition 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229940043350 citral Drugs 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- WTEVQBCEXWBHNA-JXMROGBWSA-N geranial Chemical compound CC(C)=CCC\C(C)=C\C=O WTEVQBCEXWBHNA-JXMROGBWSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- LHTVMBMETNGEAN-UHFFFAOYSA-N pent-1-en-1-ol Chemical compound CCCC=CO LHTVMBMETNGEAN-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/06—Washing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J27/195—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with vanadium, niobium or tantalum
- B01J27/198—Vanadium
- B01J27/199—Vanadium with chromium, molybdenum, tungsten or polonium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of minimizing technologies of residual organic matter in vanadium silver molybdophosphate catalyst, using remaining organic matter in washing lotion removal catalyst;Warm air blowoff is carried out again;The washing lotion is selected from the halogenated hydrocarbons such as methylene chloride, chloroform, chloroform, dichloroethanes, the aromatic hydrocarbons such as benzene, toluene, the hydro carbons such as hexane, heptane, octane, the one or more of ether, propyl ether etc.;Washing lotion dosage is 1 to 5 times of catalyst volume;Washing displacement carries out below room temperature to boiling point.Remaining organic matter has alcohol, aldehyde and aldol(s) in organic synthesis vanadium silver molybdophosphate catalyst, the substance has reproducibility, due to there is the presence of the substance during calcination activation temperature raising, cause catalyst member vanadium to be reduced to trivalent, reduces activity, conversion ratio and the selectivity of catalyst.After the present invention is using low boiling point, the washing displacement of low reproducibility solvent, reject under vapor completely, to improve the activity of catalyst, conversion ratio and selectivity.
Description
Technical field
The present invention relates to a kind of methods for removing reductive organic matter in vanadium silver molybdophosphate catalyst, belong to catalysis
Agent synthesizes field.
Background technique
Prenol, isoamyl olefine aldehydr are the important source materials of artificial synthesized citral.Vanadium silver molybdophosphate is isoamyl olefine aldehydr, different
Pentenol synthesizes effective catalyst, which synthesized in isobutanol, benzyl alcohol mixed liquor, before roasting molding
In temperature-rise period, vanadium is very vivaciously easily reduced to trivalent state by the remaining isobutanol of catalyst, benzyl alcohol, to lose catalysis
Agent activity, removal catalyst residual organic matter becomes the key point of the activity for improving catalyst, conversion ratio and selectivity before roasting.
Summary of the invention
The purpose of the present invention is the displacement remaining organic matter of catalyst is washed in filter press with low reproducibility washing lotion.Make to urge
In agent heating drying or roasting process, the generation of trivalent state vanadium is reduced, guarantees the catalytic activity point of catalyst.
The present invention provides a kind of minimizing technology of residual organic matter in vanadium silver molybdophosphate catalyst, activation of catalyst
Before, using remaining organic matter in washing lotion removal catalyst;Warm air blowoff is carried out again;
The washing lotion is selected from the halogenated hydrocarbons such as methylene chloride, chloroform, chloroform, dichloroethanes, the aromatic hydrocarbons such as benzene, toluene, oneself
The hydro carbons such as alkane, heptane, octane, the one or more of ether, propyl ether etc.;Washing lotion dosage is 1 to 5 times of catalyst volume;Washing
Displacement carries out below room temperature to boiling point.
Further, in the above-mentioned technical solutions, it washs time swap 3~4 hours.
Further, in the above-mentioned technical solutions, filters pressing is carried out to catalyst before washing lotion cleaning and normal temperature air purges.
Further, in the above-mentioned technical solutions, warm air blowoff temperature is 120~150 DEG C, and purge time is 1~5 small
When;Hot-air speed is the volume of 0.5~5 times of catalyst per minute.
The present invention provides washing displacer used in a kind of above method: the washing displacer includes sequentially connected washes
Liquid storage tank, washing lotion delivery pump, washing press, washing lotion receiving tank;The washing displacer further includes warm air blowoff system, institute
The HAI Heated Air Intake piping connection in warm air blowoff system is stated on the pipeline between washing lotion delivery pump and washing press, institute
The air emptying pipeline stated in warm air blowoff system is connected on the pipeline between washing press and washing lotion receiving tank.
Further, in the above-mentioned technical solutions, washing lotion delivery pump can adjust flow and can guarantee lift 0.2~
Within the scope of 0.4 megapascal.
Further, in the above-mentioned technical solutions, washing press is able to bear the pressure of 0.4 megapascal, 150 DEG C of temperature
Degree.
The present invention provides a kind of synthetic method of vanadium silver molybdophosphate catalyst, by vanadium source, Yin Yuan, molybdenum source, phosphorus source, benzene first
Alcohol, isobutanol, which are put into reactor, to react, filters, activation, it is characterised in that: before activation, removed and be catalyzed using the above method
Remaining organic matter in agent.
Detailed description of the invention
Fig. 1 is schematic structural diagram of the device of the invention;
In figure, 1, liquid storage tank;2, washing lotion delivery pump;3, washing press;4, washing lotion receiving tank;5, HAI Heated Air Intake pipe
Road;6, air empties pipeline.
Specific embodiment
Following nonlimiting examples can with a person of ordinary skill in the art will more fully understand the present invention, but not with
Any mode limits the present invention.Following embodiment can will elaborate to the present invention, raw materials used in the following embodiments
It is all to use analytical reagents.
Embodiment 1
As shown in Figure 1, in vanadium silver molybdophosphate catalyst residual organic matter washing displacer, including it is sequentially connected:
Washing lotion storage tank 1, washing lotion delivery pump 2, washing press 3, washing lotion receiving tank 4;The washing displacer further includes warm air blowoff
System, the HAI Heated Air Intake pipeline 5 in the warm air blowoff system are connected between washing lotion delivery pump 2 and washing press 3
Pipeline on, air in warm air blowoff system emptying pipeline 6 be connected to washing press 3 and washing lotion receiving tank 4 it
Between pipeline on.
148 kilograms of isobutanol, 216 kilograms of benzyl alcohol, 45 kilograms of vanadic anhydride, 0.75 kilogram of silver nitrate, ammonium molybdate 1,000
Gram, it puts into and opens stirring in four mouthfuls of glass reaction bottles, be slowly added to 49 kilograms of anhydrous phosphoric acid, it is small to be warming up to 115 DEG C of reactions 8
When.Filters pressing, normal temperature air purge 1 hour, with 500 liters of dichloroethanes, are uniformly pressed into filter cake with pump at 3.5 hours, with heat
Air 120 liters of speed per minute purges filter cake, and hot air temperature is 5 hours dry at 120~150 DEG C.Filter cake pulverizer
It crushes, 3 millimeters of pellet diameter, high 4 millimeters of cylindrical bodies.About 90 kilograms, 120 liters of heap volume.It is put into activator and is preheating to 200
DEG C or more, air 10%, vapor 90% (volume ratio) is passed into activator after being warming up to 400~450 DEG C, controls gas flow
2 cubic meters per minutes.Cool down after 10 hours time, obtains catalyst 1.
Comparative example 2
148 kilograms of isobutanol, 216 kilograms of benzyl alcohol, 45 kilograms of vanadic anhydride, 0.75 kilogram of silver nitrate, ammonium molybdate 1,000
Gram, it puts into and opens stirring in four mouthfuls of glass reaction bottles, be slowly added to 49 kilograms of anhydrous phosphoric acid, it is small to be warming up to 115 DEG C of reactions 8
When.Filtering, filter cake are 5 hours dry at~170 DEG C.Filter cake is crushed with pulverizer, 3 millimeters of pellet diameter, high 4 millimeters of cylindrical bodies.
About 90 kilograms, 120 liters of heap volume.It is put into activator and is preheating to 200 DEG C or more, air 10%, vapor 90% (volume ratio)
It is passed into activator after being warming up to 400~450 DEG C, controls 2,000 liters/min of gas flow.Cool down after 10 hours time, is urged
Agent 2.
Embodiment 3
No. 1 50 grams of catalyst are added in reactor, heats up when reactor is at 250 DEG C, is uniformly beaten per hour with metering pump
Enter 25 grams of 3- methyl -3- cyclobutenyl -1- alcohol (content 98.9%, content used in following embodiment are consistent), in receiving tank per hour
25 grams of product are obtained, through analyzing product prenol content 99.0%, 3- methyl -3- cyclobutenyl -1- alcohol content 0.1%.When anti-
More No. 2 50 grams of catalyst changeout are answered in device, heats up when reactor is at 250 DEG C, uniformly squeezes into 3- methyl -3- per hour with metering pump
25 grams of cyclobutenyl -1- alcohol (content 98.9%) obtains 25 grams of product in receiving tank per hour, through analyzing product prenol content
13.5%, 3- methyl -3- cyclobutenyl -1- alcohol content 85.3%.When temperature rises to 400 DEG C, prenol content is mentioned
98.7%, 3- methyl -3- cyclobutenyl -1- alcohol content 0.1%.
Embodiment 4
No. 1 50 grams of catalyst are added in reactor, heats up when reactor is at~230 DEG C, it is uniform per hour with metering pump
40 grams of alcohol of -3- cyclobutenyl -1- of 3- methyl are squeezed into, 53 liters per hour of air, obtains 40 grams of product in receiving tank per hour, through dividing
Division product prenol content 49.2%, isoamyl olefine aldehydr 48.9%, 3- methyl -3- cyclobutenyl -1- alcohol content 0.0%.Work as reaction
More No. 2 50 grams of catalyst changeout in device, heats up when reactor is at~230 DEG C, uniformly squeeze into 3- methyl -3- per hour with metering pump
40 grams of cyclobutenyl -1- alcohol, obtains 40 grams of product per hour by 53 liters per hour of air in receiving tank, through analyzing product prenol
Content 9.2%, isoamyl olefine aldehydr 8.5%, 3- methyl -3- cyclobutenyl -1- alcohol content 81.0%.When temperature is mentioned to 370 DEG C, per small
When obtain 50 grams of product, product analysis prenol content 51.1%, iso-amylene aldehyde 47.3%, 3- methyl -3- cyclobutenyl -
1- alcohol content 0.0%.
It can be seen that catalyst activity improves much from embodiment, reaction temperature can be made to be greatly reduced, conversion ratio and choosing
Less, the improvement of technique can substantially reduce production cost to the variation of selecting property.
Claims (7)
1. the minimizing technology of residual organic matter in a kind of vanadium silver molybdophosphate catalyst, it is characterised in that: before activation of catalyst, adopt
With remaining organic matter in washing lotion removal catalyst;Warm air blowoff is carried out again;
The washing lotion is selected from the halogenated hydrocarbons such as methylene chloride, chloroform, chloroform, dichloroethanes, the aromatic hydrocarbons such as benzene, toluene, hexane, heptan
The hydro carbons such as alkane, octane, the one or more of ether, propyl ether etc.;Washing lotion dosage is 1 to 5 times of catalyst volume;Washing displacement exists
It is carried out below room temperature to boiling point.
2. according to the method described in claim 1, it is characterized by: washing time swap 3~4 hours.
3. according to the method described in claim 1, it is characterized by: carrying out filters pressing and normal temperature air to catalyst before washing lotion cleaning
Purging.
4. according to the method described in claim 1, it is characterized by: warm air blowoff temperature be 120~150 DEG C, purge time
It is 1~5 hour;Hot-air speed is the volume of 0.5~5 times of catalyst per minute.
5. according to the method described in claim 1, it is characterized in that using following washing displacers: the washing displacer includes
It is sequentially connected: washing lotion storage tank, washing lotion delivery pump, washing press, washing lotion receiving tank;The washing displacer further includes hot empty
Gas purge system, HAI Heated Air Intake piping connection in the warm air blowoff system washing lotion delivery pump and washing press it
Between pipeline on, air in warm air blowoff system emptying pipeline is connected between washing press and washing lotion receiving tank
Pipeline on.
6. according to the method described in claim 5, it is characterized by: washing lotion delivery pump can adjust flow and can guarantee that lift exists
Within the scope of 0.2~0.4 megapascal.
7. according to the method described in claim 5, it is characterized by: washing press is able to bear the pressure of 0.4 megapascal, 150
DEG C temperature.
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