CN103157429A - Device and method for activating adsorbents for vacuum multilayer heat insulation - Google Patents
Device and method for activating adsorbents for vacuum multilayer heat insulation Download PDFInfo
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- CN103157429A CN103157429A CN2013100925332A CN201310092533A CN103157429A CN 103157429 A CN103157429 A CN 103157429A CN 2013100925332 A CN2013100925332 A CN 2013100925332A CN 201310092533 A CN201310092533 A CN 201310092533A CN 103157429 A CN103157429 A CN 103157429A
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Abstract
The invention discloses a device and a method for activating adsorbents for vacuum multilayer heat insulation, and belongs to the field of lower-temperature heat insulation containers. The device comprises a cold trap (1), a vacuum fine-adjustment valve (2), a first ionization gauge (3), a first thermocouple gauge (4), a calibration container (5), a first shut off valve (6), a second shut off valve (7), a second ionization gauge (8), a second thermocouple gauge (9), an activating box (10), a third shut off valve (11), a vacuum pump (12), a fourth shut off valve (13) and a safety valve (14). The device and the method are characterized in that as the activating by using the device and the mature strengthening technology are utilized, the adsorptive properties of the adsorbents such as activated carbon and molecular sieves of interlayers of the heat insulation containers can be improved, and further the service life of the vacuum heat insulation containers can be prolonged.
Description
Technical field
The present invention relates to a kind of high vacuum multiple layer heat insulation with the apparatus and method of adsorbent activation, belong to the low temperature insulation container made field.
Background technology
Low temperature insulation container made will obtain excellent heat-insulating property, need to be reduced to various forms of heat transmission minimum.High vacuum multiple layer heat insulation not only can be eliminated gaseous exchange heat exchange and most of gas conduction of adiabatic space, and by adopting the low multilayer heat insulation interlayer of surface reflectivity significantly to weaken radiant heat flux, is the best adiabatic pattern of present heat-insulating property.
The main difficulty of high vacuum multiple layer heat insulation is how to obtain in insulation chambers and the desired vacuum of long-term maintenance.Cause the reason that the low temperature insulation container made vacuum life-span reduces to mainly contain: the one, the venting of metal and thermal insulating layer material, the 2nd, the gas leakage by weld seam from atmospheric environment to the low-temperature (low temperature) vessel cylindrical shell and the not thorough residual portion gas of finding time, due to active carbon and molecular sieve adsorption a certain amount of foreign gas, its adsorption capacity under low pressure is very weak, the activated measure such as need to replace by heating, finding time and improve its absorption property under low pressure, make it satisfy the demand that Cryo Heat Insulation chamber condition of high vacuum degree is kept.
Summary of the invention
The object of the present invention is to provide a kind of adiabatic absorption property with adsorbent that significantly improves, greatly extended the high vacuum multiple layer heat insulation of pot life of high-vacuum insulation container with the apparatus and method of adsorbent activation.
Relate to a kind of high vacuum multiple layer heat insulation that can greatly improve vacuum suction agent performance apparatus and method of the activation of adsorbent.
Above-mentioned high vacuum multiple layer heat insulation comprises cold-trap with the adsorbent activating apparatus, the vacuum reset valve, and the first ionization gauge, the first thermocouple rule are demarcated container, the first shut-off valve, the second shut-off valve, the second ionization gauge, the second thermocouple rule, activation box, the 3rd shut-off valve, vavuum pump, the 4th shut-off valve, safety valve; The cold-trap air inlet is connected with the high pure nitrogen source of the gas, the cold-trap outlet is connected with the first end of vacuum reset valve, the second end of vacuum reset valve with demarcate container air inlet and be connected, demarcating container outlet is connected with the first end of the first shut-off valve, the second end of the first shut-off valve is connected with the second shut-off valve first end, and the second end of the second shut-off valve is connected with the activation box; The 4th shut-off valve first end is connected on pipeline between vacuum reset valve and cold-trap by one section pipeline, safety valve is connected with pipeline by the relief hole on this section pipeline, the first end of the 3rd shut-off valve is connected with vavuum pump, the second end of the 3rd shut-off valve is divided into two branch roads, article one, branch road is connected with the second end of the 4th shut-off valve, and the second branch road is connected on pipeline between the first shut-off valve and the second shut-off valve; Leave two measurement port on above-mentioned demarcation container, connect respectively the first ionization gauge and the first thermocouple rule; Leave two measurement port on connecting line between above-mentioned the second shut-off valve and activation box, connect respectively the second ionization gauge and the second thermocouple rule.
Utilize described high vacuum multiple layer heat insulation with the adsorbent activation method of the device of adsorbent activation, it is characterized in that comprising following process:
One, activation process:
Step 1, the adsorbent that will activate are packed in the activation box;
Step 2, will activate box and put into heating furnace, the first shut-off valve, the 3rd shut-off valve and vacuum reset valve are closed, the second shut-off valve, the 4th shut-off valve are opened, the heating furnace temperature is set, being used for the activated molecular sieve temperature is 550 ℃, and being used for the active carbon temperature is 250 ℃, continuous heating 24 hours;
Step 3, after 24 hours, stopped heating is opened burner hearth, in the burner hearth air blast cooling, until in stove, temperature turns off the blast after 100 ℃, naturally cooling;
Step 4, the 4th shut-off valve, vacuum reset valve are closed, the first shut-off valve, the second shut-off valve, the 3rd shut-off valve are opened, then open vavuum pump, be evacuated down to 5Pa, then close vavuum pump, the 3rd shut-off valve;
Step 5, cold-trap entrance UNICOM high pure nitrogen source of the gas is opened the first shut-off valve, the second shut-off valve, and the 3rd shut-off valve, the 4th shut-off valve are closed, by regulating the vacuum reset valve to activation box inflated with nitrogen, stop inflation after reaching an atmospheric pressure, close the second shut-off valve, kept one hour;
Step 6, open the second shut-off valve, the 3rd shut-off valve, vacuum reset valve, the first shut-off valve, the 3rd shut-off valve are closed, open vavuum pump, be evacuated to 10
-2Stop vavuum pump after Pa, close the second shut-off valve, kept 1 hour;
Step 7, repeating step (5)-(6) two to three times.
Two, seasoned strengthening process:
Step 1, will activate box and take out and to put into liquid nitrogen environment;
Step 2, close the 3rd shut-off valve, the 4th shut-off valve, the unlatching that keeps the first shut-off valve, the second shut-off valve, fill nitrogen by the vacuum reset valve to the activation box, keeping the box internal pressure is an atmospheric pressure left and right, until box internal pressure half an hour is closed vacuum reset valve and the second shut-off valve after without significant change;
Step 3, taking-up activation box are placed in air, open the second shut-off valve, the 4th shut-off valve, know that the activation box returns to room temperature, then close the first shut-off valve, open the 3rd shut-off valve, open vavuum pump, are evacuated to 10
-2Pa, then close the second shut-off valve, kept 1 hour;
Step 4, repeating step (1)-(3) three to five times.
With respect in the heat-activated technology of industrial circle extensive use, the high vacuum multiple layer heat insulation that relates to by this patent is with adsorbent activating apparatus and method, can effectively remove the residual gas in the adsorbent hole, improve effective adsorption area of adsorbent, thereby significantly improve adiabatic activity and absorption property with adsorbent, greatly extended the pot life of high-vacuum insulation container, significant to the technological progress in LNG field.
Description of drawings
Fig. 1 is high vacuum multiple layer heat insulation adsorbent activation equipment schematic diagram;
Numbering name in Fig. 1 is called: 1, cold-trap, 2, the vacuum reset valve, the 3, first ionization gauge, 4, the first thermocouple rule, 5, demarcate container, the 6, first shut-off valve, 7, the second shut-off valve, 8, the second ionization gauge, the 9, second thermocouple rule, 10, the activation box, 11, the 3rd shut-off valve, 12, vavuum pump, the 13, the 4th shut-off valve, 14, safety valve.
The specific embodiment
According to shown in Figure 1, high vacuum multiple layer heat insulation with the activating apparatus of adsorbent comprise 1, cold-trap, 2, the vacuum reset valve, 3, the first ionization gauge, the 4, first thermocouple rule, 5, demarcate container, 6, the first shut-off valve, the 7, second shut-off valve, the 8, second ionization gauge, 9, the second thermocouple rule, 10, activation box, the 11, the 3rd shut-off valve, 12, vavuum pump, 13, the 4th shut-off valve, 14, safety valve.
Activation process is as follows:
Step 1, the adsorbent that will activate are packed in activation box 10;
Step 2, will activate box 10 and put into heating furnace, the first shut-off valve 6, the 3rd shut-off valve 11 and vacuum reset valve 2 are closed, the second shut-off valve 7, the 4th shut-off valve 13 are opened, the heating furnace temperature is set, it is 550 ℃ as being used for the activated molecular sieve temperature, the active carbon temperature is 250 ℃, continuous heating 24 hours;
Step 3, after 24 hours, stopped heating is opened burner hearth, in the burner hearth air blast cooling, until in stove, temperature turns off the blast after 100 ℃, naturally cooling;
Step 4, the 4th shut-off valve 13, vacuum reset valve 2 are closed, the first shut-off valve 6, the second shut-off valve 7, the 3rd shut-off valve 11 are opened, then open vavuum pump 12, be evacuated down to 5Pa, then close vavuum pump 12, the three shut-off valves 11;
Step 5, cold-trap 1 entrance UNICOM high pure nitrogen source of the gas, the first shut-off valve 6, the second shut-off valve 7 are opened, the 3rd shut-off valve 11, the 4th shut-off valve 13 are closed, by regulating vacuum reset valve 2 to activation box 10 inflated with nitrogen, stop inflation after reaching an atmospheric pressure, close the second shut-off valve 7, kept one hour;
Step 6, after 1 hour, open the second shut-off valve 7, the 3rd shut-off valve 11, vacuum reset valve 2, the first shut-off valve 6, the 3rd shut-off valve 11 are closed, open vavuum pump 12, be evacuated to 10
-2Stop vavuum pump 12 after Pa, close the second shut-off valve 7, kept 1 hour;
Twice of step 7, repeating step (5)-(6).
Seasoned strengthening process is as follows:
Step 1, will activate box 10 and take out and put into liquid nitrogen environment;
Step 2, close the 3rd shut-off valve 11, the 4th shut-off valve 13, the unlatching that keeps the first shut-off valve 6, the second shut-off valve 7, fill nitrogen by vacuum reset valve 2 to activation box 10, keeping the box internal pressure is an atmospheric pressure left and right, until box internal pressure half an hour is closed vacuum reset valve 2 and the second shut-off valve 7 after without significant change;
Step 3, taking-up activation box 10 are placed in air, open the second shut-off valve 7, the 4th shut-off valve 13, know that activation box 10 returns to room temperature, then close the first shut-off valve 6, open the 3rd shut-off valve 7, open vavuum pump 12, are evacuated to 10
-2Pa, then close the second shut-off valve 7, kept 1 hour;
Step 4, repeating step (1)-(3) four times.
Claims (2)
1. a high vacuum multiple layer heat insulation with the device that adsorbent activates, is characterized in that: comprise cold-trap (1), vacuum reset valve (2), the first ionization gauge (3), the first thermocouple rule (4) are demarcated container (5), the first shut-off valve (6), the second shut-off valve (7), the second ionization gauge (8), the second thermocouple rule (9), activation box (10), the 3rd shut-off valve (11), vavuum pump (12), the 4th shut-off valve (13), safety valve (14);
Cold-trap (1) air inlet is connected with the high pure nitrogen source of the gas, cold-trap (1) outlet is connected with the first end of vacuum reset valve (2), the second end of vacuum reset valve (2) with demarcate container (5) air inlet and be connected, demarcating container (5) outlet is connected with the first end of the first shut-off valve (6), the second end of the first shut-off valve (6) is connected with the second shut-off valve (7) first end, and the second end of the second shut-off valve (7) is connected with activation box (10); The 4th shut-off valve (13) first end is connected on pipeline between vacuum reset valve (2) and cold-trap (1) by one section pipeline, safety valve (14) is connected with pipeline by the relief hole on this section pipeline, the first end of the 3rd shut-off valve (11) is connected with vavuum pump (12), the second end of the 3rd shut-off valve (11) is divided into two branch roads, article one, branch road is connected with the second end of the 4th shut-off valve (13), and the second branch road is connected on pipeline between the first shut-off valve (2) and the second shut-off valve (7);
Leave two measurement port on above-mentioned demarcation container (5), connect respectively the first ionization gauge (3) and the first thermocouple rule (4);
Leave two measurement port on connecting line between above-mentioned the second shut-off valve (7) and activation box (10), connect respectively the second ionization gauge (8) and the second thermocouple rule (9).
2. utilize the described high vacuum multiple layer heat insulation of claim 1 with the adsorbent activation method of the device of adsorbent activation, it is characterized in that comprising following process:
One, activation process:
Step 1, the adsorbent that will activate are packed in activation box (10);
Step 2, will activate box (10) and put into heating furnace, the first shut-off valve (6), the 3rd shut-off valve (11) and vacuum reset valve (2) are closed, the second shut-off valve (7), the 4th shut-off valve (13) are opened, the heating furnace temperature is set, being used for the activated molecular sieve temperature is 550 ℃, being used for the active carbon temperature is 250 ℃, continuous heating 24 hours;
Step 3, after 24 hours, stopped heating is opened burner hearth, in the burner hearth air blast cooling, until in stove, temperature turns off the blast after 100 ℃, naturally cooling;
Step 4, the 4th shut-off valve (13), vacuum reset valve (2) are closed, the first shut-off valve (6), the second shut-off valve (7), the 3rd shut-off valve (11) are opened, then opened vavuum pump (12), be evacuated down to 5Pa, close again vavuum pump (12), the 3rd shut-off valve (11);
Step 5, cold-trap (1) entrance UNICOM high pure nitrogen source of the gas, the first shut-off valve (6), the second shut-off valve (7) are opened, the 3rd shut-off valve (11), the 4th shut-off valve (13) are closed, by regulating vacuum reset valve (2) to activation box (10) inflated with nitrogen, stop inflation after reaching an atmospheric pressure, close the second shut-off valve (7), kept one hour;
Step 6, open the second shut-off valve (7), the 3rd shut-off valve (11), vacuum reset valve (2), the first shut-off valve (6), the 3rd shut-off valve (11) are closed, open vavuum pump (12), be evacuated to 10
-2Stop vavuum pump (12) after Pa, close the second shut-off valve (7), kept 1 hour;
Twice of step 7, repeating step (5)-(6);
Two, seasoned strengthening process:
Step 1, will activate box (10) and take out and to put into liquid nitrogen environment;
Step 2, close the 3rd shut-off valve (11), the 4th shut-off valve (13), the unlatching that keeps the first shut-off valve (6), the second shut-off valve (7), fill nitrogen by vacuum reset valve (2) to activation box (10), keeping the box internal pressure is an atmospheric pressure left and right, until box internal pressure half an hour is closed vacuum reset valve (2) and the second shut-off valve (7) after without significant change;
Step 3, taking-up activation box (10) are placed in air, open the second shut-off valve (7), the 4th shut-off valve (13), know that activation box (10) returns to room temperature, then close the first shut-off valve (6), open the 3rd shut-off valve (7), open vavuum pump (12), be evacuated to 10
-2Pa, then close the second shut-off valve (7), kept 1 hour;
Step 4, repeating step (1)-(3) three to five times.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103316631A (en) * | 2013-06-26 | 2013-09-25 | 苏州华福低温容器有限公司 | Molecular sieve activating treatment technology |
CN104258834A (en) * | 2014-10-10 | 2015-01-07 | 宁夏宝塔石化科技实业发展有限公司 | Device and method for segmentally activating natural gas absorption material by using acid-base salt |
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CN1756945A (en) * | 2003-02-21 | 2006-04-05 | 密科理股份有限公司 | Method for analysis of contaminants in a process fluid stream |
EP2080205A2 (en) * | 2006-09-15 | 2009-07-22 | SAES GETTERS S.p.A. | Metal getter systems |
CN201686172U (en) * | 2010-05-28 | 2010-12-29 | 青岛中油通用机械有限公司 | Adsorbent box for heat insulation container interlayer |
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CN1756945A (en) * | 2003-02-21 | 2006-04-05 | 密科理股份有限公司 | Method for analysis of contaminants in a process fluid stream |
EP2080205A2 (en) * | 2006-09-15 | 2009-07-22 | SAES GETTERS S.p.A. | Metal getter systems |
CN201686172U (en) * | 2010-05-28 | 2010-12-29 | 青岛中油通用机械有限公司 | Adsorbent box for heat insulation container interlayer |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103316631A (en) * | 2013-06-26 | 2013-09-25 | 苏州华福低温容器有限公司 | Molecular sieve activating treatment technology |
CN104258834A (en) * | 2014-10-10 | 2015-01-07 | 宁夏宝塔石化科技实业发展有限公司 | Device and method for segmentally activating natural gas absorption material by using acid-base salt |
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Application publication date: 20130619 |